CN1086189C - Ultra-fine microcrystalline cellulose compositions and process for their manufacture - Google Patents
Ultra-fine microcrystalline cellulose compositions and process for their manufacture Download PDFInfo
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- CN1086189C CN1086189C CN98806151A CN98806151A CN1086189C CN 1086189 C CN1086189 C CN 1086189C CN 98806151 A CN98806151 A CN 98806151A CN 98806151 A CN98806151 A CN 98806151A CN 1086189 C CN1086189 C CN 1086189C
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Abstract
Ultra-fine microcrystalline cellulose compositions are disclosed which produce highly stable suspensions and/or dispersions in which substantially all of the microcrystalline cellulose has a particle size not greater than about 0.7 mu m. The compositions inlcude an attriting aid which has a dual functionality, assisting in reducing the size of the cellulose microcrystals and adding a desired property or ingredient to the dispersions or other product in which the compositions are utilized.
Description
The present invention relates to ultra-fine microcrystalline cellulose, its composition; The preparation method who relates to them; And some product that comprises ultra-fine microcrystalline cellulose.More precisely, the present invention relates to specific microcrystalline cellulose compositions, described composition can disperse to form suspension, perhaps can carry out dry and the specific solid dispersed that will obtain in liquid medium to produce suspension.In suspension, all microcrystalline cellulose crude granules are the sub-micro size basically, and even still keep colloidal state when carrying out centrifugation.In addition, the invention still further relates to the suspension that makes by ultra-fine microcrystalline cellulose of the present invention.
Background of invention
Microcrystalline Cellulose is a Mierocrystalline cellulose that purify, the part depolymerization, and it is by using mineral acid, be preferably hydrochloric acid to cellulose source, and preferably the alpha-cellulose of the pulp form that is obtained by vegetable fibre shape material is handled and produced.The relatively poor ordered region of the plain polymer chain of sour optionally etched fibre makes the crystallization position exposure that forms aggregates of crystallites whereby and dissociates wherein said crystalline aggregate composition Microcrystalline Cellulose.Then, from reaction mixture, isolate these materials, and the by product of degraded is removed in washing.The resulting wet material that will comprise 40-60% moisture content in the prior art usually is called following several titles, comprising: hydrocellulose, the hydrocellulose cake that wets, stable DP Mierocrystalline cellulose, the wet cake of Microcrystalline Cellulose or abbreviate wet cake as.
When wet cake being carried out drying and make it not water content, resulting product, Microcrystalline Cellulose is: white, odorless, tasteless, free-pouring relatively powder, water insoluble, organic solvent, diluted alkaline and acid.For Microcrystalline Cellulose and preparation method thereof is described more fully, referring to US2,978,446.This patent has been described Microcrystalline Cellulose as formula of medicine, in particular as the tackiness agent of preparation slugging, disintegrating agent, flow promotor, and/or filler.Microcrystalline Cellulose is made by FMC Corp., and with trade(brand)name Avicel
The PH Mierocrystalline cellulose is sold from about 20 microns several extremely about 100 microns grades with median size.
The wet cake of Microcrystalline Cellulose and/or hydrocellulose modification is used for other purposes, jelling agent in particular as food, the thickening material of food, the fat-replacer of various food and/or the filler of empty calory, as the suspension stabilizer and/or the structure agent of food, and as emulsion stabilizer and the suspension agent of medicine with beauty treatment washing lotion and cream.By making Microcrystalline Cellulose or wet cake stand violent abrasive power and described purposes being improved, because this, microcrystallite is divided into particle in small, broken bits basically.Yet, when particle diameter diminishes, may be owing to hydrogen or other bonding force between the littler size particles, each particle tends to assemble or keratinization (hornify) when drying.For preventing to assemble or the keratinization effect, during grinding or afterwards but before drying, can add protective colloid, as carboxymethyl cellulose (CMC), all or part of neutralization of described Mierocrystalline cellulose produces the bonding force of congregation or keratinization effect.Resulting material often is referred to as ground Microcrystalline Cellulose or colloid Microcrystalline Cellulose.For the colloid Microcrystalline Cellulose is described more fully, and its production and use, referring to US3,359,365, in this patent, point out, will at least 1%, the particle diameter of preferred at least 30% Microcrystalline Cellulose is reduced to and is no more than about 1.0 microns.
The colloid Microcrystalline Cellulose is the powder of white odorless, hygroscopic.In the time of in being scattered in water, it will form white, opaque thixotropic gel.Described Mierocrystalline cellulose is by FMC Corp. preparation and with trade(brand)name Avicel particularly
RC and Avicel
The various grades of CL are sold.Described Mierocrystalline cellulose comprises: simultaneously treated Microcrystalline Cellulose and Xylo-Mucine.In FMC product report RC-16, be marked with RC-501, RC-581, the grade of RC-591 and CL-611 is known as the production dispersion, when suitable the dispersion in the dispersion about 60% particle less than 0.2 micron.
Along with the interest of in food and drug suspension cellulosic material in small, broken bits being used increases day by day; the seeker in this field is devoted to always: the slipperiness and the mouthfeel of the suspension that is made by described cellulosic material; and definite, for example particle diameter will be felt particulate or saccharoid by tongue at about cellulose grain more than 3 microns.The EP0415 193A2 of Komuro points out that for avoiding providing the sensation of material, when the particle diameter of at least 25% cumulative volume in the suspension was not more than 3 microns, the particle size range of cellulose grain 50% cumulative volume was in 0.3 micron to 6.0 microns scope.This patent has also been pointed out: cellulosic material is carried out with regard to the wet-milling as grinding medium with regard to using pottery or metallic bead, use the Ginding process and the device of high speed rotating shredder, so that realize these purposes.This patent reaches the patent corresponding to people such as Komuro, US5, and 123,962, particularly the latter has extensively discussed the effort of the success of making in the prior art for further reduction Microcrystalline Cellulose particle diameter.
Similarly, US5,415,804 point out: slick mouthfeel depends on the colloid part, and size distribution and median size, described colloid partly is can not sedimentary discrete particles part when the dispersion centrifugation.Depend on size distribution (described distribution is slightly wider than pointed distribution range in the above-mentioned Komuro patent, can up to 10 microns), the colloid part must be in 50% to 65% cumulative volume scope.Yet, in this patent, used some water-soluble gum and/or hydrophilic substance, so that remedy the size distribution of broad.
Brief summary of the invention
According to the present invention, had found that a kind of reduction Microcrystalline Cellulose particle diameter, and form the method for microcrystalline cellulose compositions, that wherein said composition contains is high (in some occasion up to 100%) per-cent, particle diameter is all the time less than 1 micron Microcrystalline Cellulose; When said composition is scattered in the liquid medium, will can from dispersion, not deposit and can not be about 15 by being lower than, the centrifugation of 000rpm is carried out physics and is removed or deposit.For the present invention, hereinafter, this notion is referred to as " colloid-stabilised ".
In the method for the invention, the wet cake of hydrocellulose is under high shear force high solid mixing condition, utilizes grinding aid and utilization or does not utilize the protective colloid wet-milling, so that form microcrystalline cellulose compositions of the present invention.
Promote the grinding aid of Microcrystalline Cellulose wet-milling to be retained in the product, and preferably the finished product that wherein use Microcrystalline Cellulose are provided the performance or the component of hope.As the example of this dual-use function, lime carbonate or other suitable calcium salt can be used for preparing the grinding aid of the microcrystalline cellulose compositions that adds the calcium milk-product.In addition, what it is also contemplated that is that grinding aid itself or its major part will be suspended in the colloid microcrystalline cellulose dispersion of wherein using the present composition.
In addition, method of the present invention can also be used the protective colloid that prevents the Microcrystalline Cellulose keratinization and promote exsiccant microcrystalline cellulose compositions redispersion.Yet in some microcrystalline cellulose compositions as filler or bulk auxiliary agent, for helping forming Microcrystalline Cellulose fine and close, the low absorpting form in few hole, it will be desirable saving protective colloid.
Composition of the present invention can be the microcrystalline solids that is reclaimed the wet-milling that obtains by Ginding process; Perhaps can be by from wet solid, removing the exsiccant resistates that moisture content makes, the latter for store, transportation and for the use subsequently of preparation microcrystalline cellulose dispersion, be preferred.
Wherein use the dispersion of microcrystalline cellulose compositions of the present invention to have excellent suspension and stability, and need less Microcrystalline Cellulose (by weight) so that realize stable and/or suspension property, described performance is equal to or greater than the performance of having only the existing Microcrystalline Cellulose product of the greater amount utilized to obtain.The dispersion that is made by composition of the present invention comprises the microcrystalline cellulose crude granule of superfine, sub-micro size, and as mentioned above, all microcrystalline cellulose crude granules all are colloid-stabilised basically, therefore, can provide the suspension effect/stabilization of improvement.
Detailed Description Of The Invention
The present invention is used as raw material with the wet cake of above-mentioned hydrocellulose, when with mineral acid to cellulose source, be preferably the paper pulp shape alpha-cellulose that obtains by fibrous vegetable material and handle, when washing removes disacidify and by product then, the hydrocellulose of being produced is last exsiccant material, and the wet cake of being produced comprises the moisture content of about 40-60% usually.According to the present invention, grinding aid is mixed with wet cake.Particularly, if wish composition is carried out drying, and store or transport, and disperse to obtain colloid-stabilised dispersion, also can add protective colloid with dried forms.Mode with routine is mixed these raw materials then.In the wet mixing preparation, moisture content can be regulated as required, grinds desirable denseness to produce mixture, and can regulate during grinding as required, to keep desirable denseness.In preferred embodiments, the moisture content that is present in the wet cake is normally competent.Because excessive moisture content tends to reduce particle and intergranular frictional force, it is necessary that described frictional force is that the microcrystalline cellulose crude granule is decreased to the subparticle size, therefore, should avoid using excessive water.
Then, preferably under the mixing condition of high-shear, high solids content, wet mixture to high solids content is ground, wherein grinding aid is worn into ultra-fine sub-micro size particles with Microcrystalline Cellulose, or promoting Microcrystalline Cellulose to wear into ultra-fine sub-micro size particles, described ultra-fine sub-micro size particles is colloid-stabilised when disperseing.In preferred embodiments, by comprising that protective colloid will further promote colloidal stability.
Preferably aforesaid grinding aid is elected to be the multi-functional component of blend.That is to say that grinding aid plays a part to grind Microcrystalline Cellulose, and also plays a part to give the other of desirable performance of product or component, use microcrystalline cellulose compositions of the present invention in the described product.Therefore, when selecting grinding aid, preferably, consider these two purposes simultaneously and select.
With regard to the effect that Microcrystalline Cellulose is ground to form the ultra-fine grain size, grinding aid must be water-insoluble relatively; That is, when mixing with the wet cake of hydrocellulose, it can not dissolve in a large number.More precisely, being used for grinding aid of the present invention can be moisture K
SpBe equal to or less than 1 * 10
-7Ionic species, or the solubleness in water is equal to or less than the powder or the particulate matter of 40% (100 ℃).Described grinding aid should be quite thin material, and therefore, it grinds closely with wet cake particle and contacts during grinding, but need not the size resemble the colloid.Therefore, for example, its particle diameter can be from about 0.1 micron to about 100 microns, advantageously can be from about 0.1 micron to about 20 microns, preferably less than about 10 microns.The preparation that had proved suitable ionic species already comprises: Wingdale (lime carbonate), Lin Suanergai, tricalcium phosphate, zinc carbonate, zinc hydroxide, trimagnesium phosphate, barium carbonate, barium sulfate, iron protocarbonate, aluminium hydroxide, magnesium hydroxide, and Ripon.Comprise as other material of grinding aid: nonionic, as silica, various clays, silicate, silicon-dioxide, talcum, titanium dioxide and some plastic resin, and partly soluble organism, for example lactose etc.In fact, many materials it is believed that and can be used for this purpose, and can be contemplated that these grinding aids can use separately or be used in combination, so that obtain desirable performance.
Except that its effect in the milled fibre element, grinding aid of the present invention preferably can be as a component of the dispersion that is formed by microcrystalline cellulose compositions of the present invention, and can give described final product with desirable batching, component or performance.As mentioned above, can advantageously use lime carbonate, increase the calcium value in milky product or the milk-product, and in paper-making process, be coated with paper and the effect of finishing other; Magnesium hydroxide and/or aluminium hydroxide can be pharmaceutical preparation such as the useful additive of antacid; And the composition that comprises titanium dioxide can be in coating and pigment, finds purposes at coffee in non-dairy cream and many other products.Advantageously, abrasive of the present invention can be at medicine, Personal hygiene and cosmetic products and product such as washing lotion, ointment, gelinite, and the abrasive that uses in the paste, promptly insoluble relatively component, described articles for use and product for example comprise toothpaste and other dental care products.For toothpaste, preferred grinding aid comprises: be the lime carbonate of known abrasive in toothpaste, Lin Suanergai and silica.
With regard to the overwhelming majority used, preferably described mixture comprised protective colloid.When having protective colloid, these colloids can play some active one or more effects.What it is contemplated that is; by protective colloid being connected on the microcrystalline cellulose crude granule or substituting the hydrogen bonding force between them; therefore and between described particle, form a blocking layer and stop them to carry out keratinization, protective colloid will be as between the microcrystalline cellulose crude granule and/or blocking agent on every side.Secondly, when making the exsiccant solids composition redispersion of Microcrystalline Cellulose, protective colloid will play dispersing auxiliary, so that promote the Microcrystalline Cellulose particulate to disperse and the rehydration effect.In addition, they also will help the reservation and/or the change of suspension flow sex change.Can be contemplated that many preparations will play similar effect, for example, derivatived cellulose such as carboxymethyl cellulose, hydroxypropylcellulose, Vltra tears and Natvosol.Various natural gum such as guar gum, Viscogum BE, gum arabic, tragacanth and sterculia, and seaweed extract thing such as carrageenin and alginate, and Star Dri 5, the cereal solid of hydrolysis also can use pectin in addition.Being used for preferred preparation of the present invention is Xylo-Mucine (CMC).
Use for other, for example, when hope was used as filler or raising agent with composition, the product with densification, relative atresia was desirable, and described product has low suction and oil absorbency.With regard to these application, can use Microcrystalline Cellulose and abrasive, and not comprise protective colloid.When product is carried out drying, described product will be gathered into such material, and it is compared more fine and close and still less hole is arranged with the material that utilizes previous bigger, more uneven microcrystalline cellulose crude granule to obtain.These fillers or raising agent are to hang down absorbefacient (water or oil) and can be used for low humidity to use for example low wet provision such as sandwich cake, chocolate, peanut butter etc.
Preferably, by to Microcrystalline Cellulose, abrasive, and the mixture of preferred protective colloid carries out high solids content, high shear force wet lapping, and make the particle diameter of Microcrystalline Cellulose reduce to the size of colloidal solid.For the particle diameter that reduces Microcrystalline Cellulose, it is preferred using the standard extruder that preferably has multiscrew.For the high shear force wet grinding operation, also can use other standard equipment, as the planet mixing machine, Hobart mixing machine for example, ball mill, shredder, and roller mill particularly have the roller mill of three rollers or multiple roll.Importantly, by forcing the cross section of mixture by being found in limited cross section such as extruding machine and various other the porous plate of mixing equipment, or as between the roller of roller mill other passage of limited tolerance, employed equipment provides high shear forces between Microcrystalline Cellulose and abrasive, and violent friction, grinding is provided.With regard to its ease for operation of handling at high solids content, high throughput and with regard to it with regard to the efficient that obtains very trickle crystal fiber crude granule, preferably extrusion molding is handled.
In the method for the invention, first step comprises: the Microcrystalline Cellulose that will not grind, abrasive and dispensable protective colloid are blended together.The solid content of being represented by Microcrystalline Cellulose and abrasive is suitable is about 30% to about 80% scope in blend weight, preferably from about 40% to about 60%.The weight ratio of Microcrystalline Cellulose and abrasive is suitable be about 85: 15 to about 30: 70 scope, advantageously at about 70: 30 to about 40: 60 scope.When using protective colloid, its suitable consumption is 5% to 30% of a Microcrystalline Cellulose weight, preferably from 5% to 15%; That is to say that the weight ratio of Microcrystalline Cellulose and protective colloid was from about 95: 5 to about 70: 30.Carry out blending continuously, till obtaining wet uniformly blend.
Then, make wet blend under certain shearing force, the high-shear wet lapping regular hour; Wherein said shearing force is enough to make the particle diameter of Microcrystalline Cellulose to be reduced to: wherein about 80% to 100%, and advantageously about Microcrystalline Cellulose of 90% to 100%, its particle diameter is not more than 1 micron, and is colloid-stabilised in being scattered in water-bearing media the time.However, the particle diameter of larger particles will be at about 3-4 micron, and therefore, resulting blend is substantially free of: the grittiness of being felt by mouth or tongue or the particle of granular mouthfeel.Yet preferably, almost the particle diameter of 100% Microcrystalline Cellulose is all less than 1 micron, and at least 90% to 95% particle diameter is less than 0.75 micron.As illustrating in an embodiment, in microcrystalline cellulose dispersion produced according to the invention, the size distribution of Microcrystalline Cellulose about 0.1 to about 0.7 micron scope.
When the blend of extruding comprises: its particle is during than the harder grinding aid of microcrystalline cellulose crude granule, and its particle diameter can not reduce usually significantly.For example, comprise median size and be several microns lime carbonate extrude blend, the dispersion of the calcium carbonate granule of the Microcrystalline Cellulose of subparticle and several microns sizes can be provided.Therefore, can provide: Microcrystalline Cellulose is sub-micro size and the much bigger dispersion of grinding aid particle diameter.
Can reclaim by the wet-milling microcrystalline cellulose compositions of extruding or other appropriate method obtains, stablizer/suspension agent of using as suspension and dispersion disperses then, and/or for described purposes, can further handle, drying is disperseed then.If you are using, further treatment step can comprise: the preparation raw dispersion, make resulting dispersion homogenizing, for example make it dry by spraying drying or other suitable method, all these are all in the scope of prior art and be described in the following examples.
Depend on initial batching and wherein employed ratio, composition of the present invention comprises: the microcrystalline cellulose compositions of extra-fine grinding, described microcrystalline cellulose compositions comprises: have the microcrystalline cellulose crude granule of particle diameter as mentioned above, dispensable aforesaid grinding aid, and dispensable protective colloid; Wherein the weight ratio of Microcrystalline Cellulose and grinding aid at about 85: 15 to about 30: 70 scope; advantageously from about 70: 30 to about 40: 60; and when using protective colloid, the weight ratio of Microcrystalline Cellulose and protective colloid at about 95: 5 to about 70: 30 scope.
The Microcrystalline Cellulose that superfine of the present invention is colloid-stabilised, or the product of Microcrystalline Cellulose of the present invention, grinding aid and dispensable protective colloid can be used for dispersion, emulsion, in the suspension etc., its consumption is in the finished product, from about 0.05-15% weight, advantageously from 0.05-5% weight, preferably from 0.05-3% weight; And can be used as filler or raising agent, its consumption is from about 1-25% weight.With regard to food uses, its suitable consumption is a 0.05-15% weight.
Owing to no matter when, anywhere all need more effective suspension stabilizer or smooth creamy filler or dispersing auxiliary, therefore, what those of ordinary skills should know is, composition of the present invention will have many different purposes in following product: food, medicine and personal care product, as cosmetic cream and washing lotion, dental care products, as formulation of tooth-paste, and a lot of medicine and industrial use.Therefore, the present invention is specially adapted to: milk-product add calcium, structure and stable, nutritious VITAMIN and mineral supplement suspend; Be applicable to the insoluble organic molecule of water in suspension; And be applicable to different purposes as, stablize various other food, medicine, dentistry, and cosmetic prescription, paint, and many industrial uses are as the opacifying agent that suspends in paper-making process and White Board calciferous.Therefore, following embodiment just illustrates some potential purposes of the present composition, and the scope to the useful purposes of the present invention that do not mean that limits.Except as otherwise noted, per-cent is all by weight in an embodiment.
Yet these embodiment have also illustrated the purposes of product of the present invention in finished product, must consider many different formula factors, and these factors will influence and/or determine to be produced the character and the quality of product.For every kind of described product, composition of the present invention must use with an amount of or suitable concentration.The characteristic of every kind of product or prescription are influenced by other factors may, as for special formulation, are included in the selected particular abrasive such as other additive in the prescription.Example as described design and prescription, embodiment 9 has illustrated: although for food and medicine, calcium value as calcium complement agent is special hope, but when using highly soluble calcium salt such as calcium sulfate, but can not produce finely disseminated microcrystalline cellulose compositions in water-bearing media, and the flocculation that tends to produce Microcrystalline Cellulose, the reason of flocculation is still not fully aware of at present.Use similar method, embodiment 17 has illustrated the preparation of pourable suspension, comprises sucrose in this prescription, forms a kind of mashed prod, and it can not resuspending when adding water.Similarly, embodiment 18 has illustrated: prepare the ability of the pharmaceutical preparation of stable available spoon taking-up, described preparation has denseness and the outward appearance of beating emulsifiable paste or other whipping food, medicine or makeup.
Embodiment 1
With 237.5 gram ground Wingdale (K
Sp=3.36 * 10
-9), wet cake of 552.3 gram hydrocelluloses and the moderately viscous carboxymethyl cellulose of 26.9 grams place the Hobart mixing tank.The solids ratios of forming this mixture is: 47.5 parts of Mierocrystalline celluloses, 47.5 parts of lime carbonate and 5 parts of carboxymethyl celluloses.Open mixing tank, till composition evenly.Then with delivery of composition to twin screw extruder with 150rpm running, the outlet fence gate that passes through for the first time is set at 6.35 millimeters, and the outlet fence gate that passes through for second to the 4th time is set at 19.05 millimeters.Preparation contains the dispersion that 1% and 2% solid is somebody's turn to do wet product in water then.1% dispersion will become stable gel.When utilizing microscope to check, cellulosic particle seem superfine and size very even.2% dispersion will form strong gel.Be scattered in water with 5% solid content remaining product and 17, carry out homogenizing under the 236.9kPa (2500psi) and handle.The viscosity of this dispersion is 8700cps after homogenizing is handled.Then, the temperature out with 190-200 ℃ temperature in and 100 ℃ makes this dispersion carry out spraying drying.The dispersion of the resulting powder of preparation 8 grams in 392 gram water in Waring blending machine.At first, the measured viscosity of measurement of using the Brookfield RVT viscometer with 10 rev/mins spindle #1 to carry out 1 minute is 615cps.The dispersion of this powder has and the identical stability of dispersion of grinding wet composition afterwards.Solid content with 1%, 0.75% and 0.5% prepares the dispersion of other spray-dried powders.1% dispersion does not have precipitation and this system with gelling.0.75% dispersion has only precipitation seldom.This system will form weak gel and be assessed as stable.0.5% dispersion has a little precipitation and this system will produce slight gelling.
Embodiment 2
Obviously changing under the situation of solid constituent ratio, prepare other composition.Fully according to embodiment 1 described step.In table 1, listed the composition that grinds, comprise solids ratios.
Table 1
| Embodiment | Composition | Solids ratios | ||
| Wet cake a(gram) | Lime carbonate (gram) | CMC b(gram) | ||
| 2A | 576.9 | 225.0 | 53.8 c | 45/45/10 |
| 2B | 865.4 | 125.0 | 40.3 d | 67.5/25/7.5 |
| 2C | 718.0 | 488.0 | 34.4 d | 35/61/4 |
| 2D | 980.8 | 75.0 | 45.7 d | 76.5/15/8.5 |
aThe hydrocellulose cake that wets
bCarboxymethyl cellulose
cEach 26.9 gram of low viscosity and moderately viscous carboxymethyl cellulose
dModerately viscous carboxymethyl cellulose
When being scattered in the water with 1% solid content, the product of these embodiment will obtain stable dispersion, and wherein embodiment 2A and 2C will produce very slight deposition, and the latter is because high lime carbonate: due to the Microcrystalline Cellulose ratio.In addition, also disperse embodiment 2B and 2D, and form stable dispersion with this solid content with 0.5% solid content.
Present embodiment shows that the scope of the consumption of each component and ratio can be very big in the composition.
Embodiment 3
By with 8250 rev/mins centrifugal 15 minutes, then anhydrous upper strata product is carried out gravimetric analysis and measures the colloidal content of embodiment 2 abrasive compositions.Colloid thing content is measured as 49.4% in embodiment 1 product, but because lime carbonate is 50% of composition, therefore, Mierocrystalline cellulose adds that the colloidal content of carboxymethyl cellulose is 98.8%.For the product of embodiment 2A to 2D, similarly measure.These measurements are listed in the table 2.
Table 2
| Colloid % | ||
| Embodiment | Composition | Mierocrystalline cellulose a |
| 2A | 52.9 | 96.1 |
| 2B | 74.0 | 98.7 |
| 2C | 39.0 | 100.0 |
| 2D | 80.0 | 94.1 |
aIn Mierocrystalline cellulose and carboxymethyl cellulose total amount
Embodiment 4
With the about 0.8 micron ground Wingdale in 250 gram particles footpath, wet cake of 576.9 gram hydrocelluloses and the moderately viscous carboxymethyl cellulose of 26.9 grams place the Hobart mixing tank.The solids ratios that comprises this mixture is: 45 parts of Mierocrystalline celluloses, 50 parts of lime carbonate and 5 parts of carboxymethyl celluloses.Opened mixing tank 5 minutes, till composition evenly.Then with delivery of composition to twin screw extruder with 150rpm running, the outlet fence gate that passes through for twice is set at 25.4 millimeters.Be scattered in water with 8% solid content product and, carry out homogenizing under the 236.9kPa (2500psi) and handle 17.Then, the temperature out with 200 ℃ temperature ins and 100 ℃ makes this dispersion carry out spraying drying.In Waring blending machine, make comprise 0.5% and the dispersion of 1% powder of being produced be stable, but each all has slight deposition to produce.The colloidal content of the composition that records by embodiment 3 is 49.4%, and this shows: Mierocrystalline cellulose and carboxymethyl cellulose bonded colloidal content are 98.8%.Said composition is labeled as embodiment 4A.In an identical manner, utilize the lime carbonate of different median sizes to prepare other composition.These compositions are labeled as embodiment 4B to 4E respectively in table 3.
Table 3
| Colloidal content | |||
| Embodiment | Lime carbonate particle diameter (micron) | Composition (%) | Mierocrystalline cellulose a |
| 4A | 0.8 | 49.40 | 98.8 |
| 4B | 3.5 | 48.80 | 97.8 |
| 4C | 5.5 | 57.8 | 115.6 |
| 4D | 8.0 | 50.00 | 100.0 |
| 4E | 12-13 | 51.25 | 102.5 |
aMierocrystalline cellulose adds carboxymethyl cellulose
Embodiment 5
With the about 8.0 microns Wingdale of 400 gram ground particle diameters, wet cake of 974.4 gram hydrocelluloses and 21.5 gram high viscosity carboxymethyl celluloses place the Hobart mixing tank.The solids ratios that comprises this mixture is: 47.5 parts of Mierocrystalline celluloses, 50 parts of lime carbonate and 2.5 parts of carboxymethyl celluloses.Open mixing tank, till composition evenly.Then with delivery of composition to twin screw extruder with 150rpm running, will export fence gate at the beginning and be set at 1.59 millimeters, first by the time increase to 6.35 millimeters, and the second time by the time increase to 25.4 millimeters.Be scattered in water with 8% solid content product and, carry out homogenizing under the 236.9kPa (2500psi) and handle 17.Then, the temperature out with 200 ℃ temperature ins and 100 ℃ makes this dispersion carry out spraying drying.Utilize Waring blending machine that the dry powder of gained is scattered in the water, produce solid content and be 1% and 1.5% stabilising dispersions.The colloid percentage composition that records in composition is 41.9%, and this shows: Mierocrystalline cellulose (Microcrystalline Cellulose adds MCC) colloidal content is 83.8%.Compare with other composition that comprises the medium-viscosity carboxymethyl cellulose, the shearing force that said composition need increase is disperseed so that make it.Said composition is embodiment 5A.
Prepare the wet cake of 872 gram hydrocelluloses in identical mode, 400 gram ground particle diameters are 8.0 microns Wingdale, with second composition of 64.5 gram low viscosity carboxymethyl celluloses, different is: in entire method, twin screw is exported fence gate remain on 25.4 millimeters.The solids ratios that comprises this mixture is: 42.5 parts of Mierocrystalline celluloses, 50 parts of lime carbonate and 7.5 parts of carboxymethyl celluloses.Utilize the Lightnin mixing tank, the solid content with 0.5%, 1.0% and 1.5% is scattered in the dry powder of being produced in the water fully, keeps 5 minutes.Only the dispersion of 1.5% solid content is stable, very slight deposition wherein occurs.Colloidalmaterial in said composition is measured as 52.0%, and this shows: Mierocrystalline cellulose (Microcrystalline Cellulose adds CMC) colloidal content is 104%.Said composition is embodiment 5B.
Embodiment 6
With the wet cake of 1153.85 gram hydrocelluloses, 500 gram lime carbonate and 53.82 gram low viscosity methoxypectins place the Hobart mixing tank of 9.46 liters (10 quarts).The solids ratios that comprises this mixture is: 45 parts of Mierocrystalline celluloses, 50 parts of lime carbonate and 5 parts of low viscosity methoxypectins.Said composition is mixed, till composition evenly.Make this mixture pass through twin screw extruder three times then.The mixture (447.95 gram) that a part is ground places 5 liters Waring mixing machine, and adds 1302.5 deionized waters.Disperse this mixture with low speed then, obtain comprising the dispersion of 15% solid content.Repeat once this dispersion steps.Dispersion is mixed, and before spraying drying,, carry out homogenizing under the 236.9kPa (2500psi) and handle 17.It is 110 ℃ with temperature out that the temperature in of spray-dryer is 210 ℃.After drying step, be recovered to 384 gram dried powders altogether.
Embodiment 7
By the method for embodiment 1, with the wet cake of 576.9 gram hydrocelluloses, 250 gram tricalcium phosphate (K
Sp=2.07 * 10
-33), the moderately viscous carboxymethyl cellulose of 26.9 grams, and 45 ml waters mix together, and pass through twin screw extruder.Utilize microscope that the dispersion of this product in water detected.The result shows: be not only Mierocrystalline cellulose and be that the tricalcium phosphate particle is the sub-micro size.
Embodiment 8
By the method for embodiment 4, with the wet cake of 1730.8 gram hydrocelluloses, 750 gram Lin Suanergai (K
Sp=1.55 * 10
-7) and the moderately viscous carboxymethyl cellulose of 80.64 grams mix and grind.The solids ratios that comprises this mixture is: 45 parts of Mierocrystalline celluloses, 50 parts of Lin Suanergais and 5 parts of carboxymethyl celluloses.The microscopic analysis of this material 2% dispersion shows: Microcrystalline Cellulose is 100% colloid on substantially.Under the condition of embodiment 1, the dispersion of this material 8% is carried out spraying drying.Spray-dried powders dispersion of 1% in water is stable, but some depositions will appear in 0.5% dispersion.These results come to the same thing with the product that utilizes embodiment 4 is resulting basically.Solid content is half of the viscosity of 1%, 2%, 3% and 4% the dispersion corresponding dispersion that is about the material that embodiment 4 makes.
Embodiment 9
By the method for embodiment 4, with the wet cake of 576.9 gram hydrocelluloses, 250 gram calcium sulfate (K
Sp=4.93 * 10
-5) and the moderately viscous carboxymethyl cellulose of 26.9 grams mix and grind.The solids ratios that comprises this mixture is: 45 parts of Mierocrystalline celluloses, 50 parts of calcium sulfate and 5 parts of carboxymethyl celluloses.After grinding was finished, because Microcrystalline Cellulose flocculates, this may be owing to due to the high dissolution constant of calcium sulfate, therefore, attempt to make the wet cake of last exsiccant to be scattered in not success in the water.
Embodiment 10
With the wet cake of 1153.85 gram hydrocelluloses, 500 gram titanium dioxide and the moderately viscous carboxymethyl cellulose of 53.76 grams place the Hobart mixing tank of 9.46 liters (10 quarts).The solids ratios that comprises this mixture is: 45 parts of Mierocrystalline celluloses, 50 parts of titanium dioxide and 5 parts of moderately viscous carboxymethyl celluloses.Said composition is mixed, till composition evenly.Make this mixture pass through twin screw extruder three times then.The mixture (1144.78 gram) that a part is ground places the colloidal mill that utilizes the Lighnin mixing tank to stir for the circulation that improves sample, and adds 7355.22 gram deionized waters.Be set at 60 pairs of these mixtures with varistor then and ground 10 minutes, obtain comprising the dispersion of 8% solid content.After finishing grinding, before spraying drying,, under the 236.9kPa (2500psi) sample is carried out homogenizing and handle 17.It is 110 ℃ with temperature out that the temperature in of spray-dryer is 210 ℃.After drying step, be recovered to 100 gram dried powders altogether.This powder dispersion of 0.5% in water is completely stable.
Embodiment 11
By the method for embodiment 4, with the wet cake of 417.23 gram hydrocelluloses, 180.8 gram talcum powder and the moderately viscous carboxymethyl cellulose of 19.4 grams mix and grind.The solids ratios that comprises this mixture is: 45 parts of Mierocrystalline celluloses, 50 parts of talcum powder and 5 parts of carboxymethyl celluloses.After carrying out spraying drying by the method for embodiment 1, spray-dried powders water dispersion of 1% in water is stable, but 0.5% dispersion is unsettled.
Embodiment 12
By the method for embodiment 4, with the wet cake of 1153.8 gram hydrocelluloses, 515.5 gram lactose (solubleness in the water=27% (100 ℃)) and the moderately viscous carboxymethyl cellulose of 53.8 grams mix and grind.The solids ratios that comprises this mixture is: 45 parts of Mierocrystalline celluloses, 50 parts of lactose and 5 parts of carboxymethyl celluloses.Before carrying out spraying drying, prepare the dispersion of 7% solid content, and with 17,236.9kPa (2500psi) carries out homogenizing to be handled by the method for embodiment 1.During the water dispersion of 1% solid content, spray-dired powder is easy to disperse in being prepared in water.
Embodiment 13
The commercially available skimming milk of 547.25 grams is placed the stainless steel beaker of 1200ml.Stir down, in this skimming milk, add powder 2.75 grams of embodiment 1 preparation.After mixing is finished, in water-bath with this mixture heating up to 79.4 ℃ (175 °F).Utilize two steps to make this mixture homogenization then; The first step is carried out under the 236.9kPa (2500psi) 17, and second step carried out under the 447.4kPa (500psi) 3.After homogenizing is handled, in cooling bath, make skimming milk be cooled to 4 ℃ (40 °F).When finishing cooling, this skimming milk is observed, so that determine to occur sedimentary degree, after a week, observe then, so that determine when storing, to form sedimentary degree.The results are shown in Table 4 for embodiment 13A to 13G.
Table 4
| Embodiment | MCC/CaCO 3The source | Observe at the beginning | Observe after seven days |
| 13A | Embodiment 1 | Stable, there is not precipitation | A large amount of precipitations |
| 13B | Embodiment 4B | Stable, there is not precipitation | Slight precipitation |
| 13C | Embodiment 4C | Stable, there is not precipitation a | Slight precipitation |
| 13D | Embodiment 4D | Stable, there is not precipitation | Very slight precipitation |
| 13E | Embodiment 4E | Stable, there is not precipitation | Very slight precipitation |
| 13F | Embodiment 6A | A large amount of precipitations | Fairly obvious precipitation |
| 13G | Embodiment 6B | Very tiny precipitation | Very slight precipitation |
aWhen this enhanced skimming milk is tasted, tongue will be felt very slight drying.
Except 13F may except, all above-mentioned prescriptions all are acceptable, and obtain than initial skimming milk calcium content have more 40% increase the calcium skimming milk, prescription 13F scrapes through.
By composition and 0.016% weight Seakem with 0.25% weight embodiment 4A
The CM611 carrageenin is added into the lower fat Ruzhong that comprises 96.46% weight skimming milk and 3.28% weight heavy cream (38%) fat, utilizes similar production method, and preparation adds the lower fat dairy products of calcium.Except that heavy cream, all wt per-cent is all to add the lower fat dairy products of calcium.These lower fat dairy products, per 240 milliliters will provide 120 milligrams of other calcium.
Embodiment 14
With the wet cake (45 parts) of 2.25 gram hydrocelluloses of preparation among the embodiment 1, lime carbonate (50 parts) and moderately viscous carboxymethyl cellulose (5 parts) add as in the gram of 375.96 in the steel beaker that very much not the becomes rusty water.Utilize the Lihgtnin mixing tank that Microcrystalline Cellulose was disperseed 10 minutes.When disperseing to finish, with 0.515 gram VITAMIN and mineral substance (premix)
, 3.55 gram soy protein isolates and 0.075 gram carrageenin (Viscarin
GP 209) the thing that do to mix be added in this dispersion, and then mixed 30 minutes.At last, with 12.5 gram Semen Maydis oils, 43 gram corn-syrup solids (24DE), 33 gram particle shape sucrose, 16.5 gram skimming milk powder, each 3 gram of the red cocoa of alkaline purification and natural cocoa, 1.5 gram Tripotassium Citrates, 1.4 gram soybean lecithin, 1.25 gram Vanilla condiment, 1.15 gram Repone K, 1 gram Rhodiaphos DKP, be added in this mixture with 0.35 gram sodium-chlor, and then stirred 5 minutes.In the high temperature short time pasteurization device, make this mixture carry out the pasteurization in 3 seconds then in 79.4 ℃ (175 °F).After pasteurization, in two steps this mixture is carried out homogenizing and handle: the first step is 20,684kPa (3000psi), and second step is 3,447.4kPa (500psi).After cooling,, and before with the naked eye checking, make it to leave standstill at least 16 hours with the mixture bottling.The Brookfield LVF viscometer with the spindle #1 of 60rpm running is equipped with in utilization, in 5 ℃ (41 °F) viscosity is measured.After interference-free is shelved more than 72 hours, shake sample, and observe, measure second viscosity then.Listed the prescription of three products in table 5, they are respectively embodiment 14A, 14B and 14C.
Table 5
| Embodiment | |||
| Batching | 14A(％) | 14B(％) | 14C(％) |
| Water | 75.192 | 74.792 | 75.092 |
| Corn-syrup solids, 24DE | 8.600 | 8.600 | 8.600 |
| Sucrose, particle | 6.600 | 6.600 | 6.600 |
| The skimming milk powder | 3.300 | 3.300 | 3.300 |
| Semen Maydis oil | 2.500 | 2.500 | 2.500 |
| Soy protein isolate | 0.710 | 0.710 | 0.710 |
| MCC/CaCO 3/CMC a | 0.450 | 0.850 | - |
| Microcrystalline Cellulose b | - | - | 0.450 |
| The red cocoa of alkaline purification | 0.600 | 0.600 | 0.600 |
| Natural cocoa | 0.600 | 0.600 | 0.600 |
| Tripotassium Citrate | 0.300 | 0.300 | 0.300 |
| Soybean lecithin | 0.280 | 0.280 | 0.280 |
| Vanilla condiment | 0.250 | 0.250 | 0.250 |
| Repone K | 0.230 | 0.230 | 0.230 |
| Rhodiaphos DKP | 0.200 | 0.200 | 0.200 |
| The vitamin/mineral pre-composition | 0.103 | 0.103 | 0.103 |
| Sodium-chlor | 0.070 | 0.070 | 0.070 |
| Carrageenin c | 0.015 | 0.015 | 0.015 |
| Lime carbonate | - | - | 0.100 |
aThe product of embodiment 1
bAvicel
CL-611, FMC Corp., Philadephia, PA 19103
cViscarin
GP 209, FMC Corp., and Philadephia, PA 19103
Table 6 has been listed embodiment 14A, the performance of 14B and 14C.
Table 6
| Embodiment | The range estimation appraisal | Viscosity (cps) |
| 14A | ||
| 16 hours | The thin precipitation of calcium carbonate of band speckle | 41.5 |
| 72 hours | Coarse particles, some thin precipitation of calcium carbonate, no speckle or spot | 47 |
| 14B | ||
| 16 hours | Slight atomizing mouthfeel, band speckle, and precipitation of calcium carbonate | 113 a |
| 72 hours | There is not precipitation, speckle, or spot | 97.5 a |
| 14C | ||
| 16 hours | Cocoa, lime carbonate and/or VITAMIN and mineral substance seriously precipitate | 38.5 |
| 72 hours | Lime carbonate and some thick cocoa solids precipitations | 48 |
aThe spindle #2 that utilization is turned round with 60rpm measures
Embodiment 14A has produced well accepted product, and it has desirable viscosity and minimum throw out, redispersion easily when shaking.Because use more MCC, therefore, embodiment 14B is thickness too.Embodiment 14C is far from satisfactory, and when 16 hours and 72 hours, it has demonstrated serious precipitation.Present embodiment shows: composition of the present invention can be used for nutritious alcoholic beverage effectively.In addition, present embodiment has also illustrated: be better than by Avicel
The improvement of the dispersion that the CL-611 Mierocrystalline cellulose makes.
Embodiment 15
2692.4 gram skimming milks and 400 gram heavy creams are placed the container that utilizes the Lightnin mixing tank to stir.Adding 266.8 gram skimming milk powder, 400 gram sugar, 210 gram corn-syrup solids (42DE), the wet cake/lime carbonate of the hydrocellulose that 16 grams grind/carboxymethyl cellulose powder (embodiment 1), the 0.8 gram carrageenin (Lactarin that FMC Corp. sells
IC 1222), 4 gram Walocel MT 20.000PVs are (by the Aqualon of Hercules Incorporated sale
7HF) and 10 gram emulsifying agents (Tandem 100K, single, doing 2-glycidyl ester: 80: 20 mixtures of Spheron MD 30/70, sold by Witco company) mixes before the thing, and this mixture was mixed about 5 minutes, be added in the vortex of mixing tank then and mix 30 minutes, so that the abundant aquation of glue.When mixing is finished,, utilize Cherry-Burrel ultrahigh-temperature device 76.7 ℃ (170) operation two minutes, and this mixture is carried out pasteurization by the high temperature, short time method.After pasteurization, utilize APV Gaulin homogenizer to make mixture homogenization, the first step is 13,789.5kPa (2000psi) carries out, and second step was 3,447.4kPa (500psi) carries out.When homogenizing is finished, but and age overnight in the refrigerator and cooled of 1.7-4.4 ℃ (35-40).The separation phenomenon that mixture do not occur.Next day, under gentle agitation, add 37.9 gram Vanilla condiment by wooden spoon, thereby prevent from the continuous refrigerator of Taylor, to carry out freezing before with in this mixture of inclusion of air.In addition, carry out freezing before, utilize Brookfield LVF viscometer, the viscosity that records 400 ml mixtures is 310cps.Utilizing the measured second viscosity of #2 Zahn cap is 43 seconds.The rate of expansion of frozen confection is 65%, and the melting behaviour of standard will produce 68 milliliters melts.About ice-cream taste test provides: with the at present industrial Avicel that in low-fat ice cream, uses used as stabilizers
The performance that RC-581 is suitable, but present embodiment has the calcium amount of increase.
Embodiment 16
Gravity method by embodiment 3 shows that the colloid amount in the present composition is relevant with the total amount of existing Mierocrystalline cellulose and carboxymethyl cellulose.The size that is present in the cellulose grain in the composition is utilized Horiba LA-910 size distribution analyser, measures by laser scattering method.Pure lime carbonate is carried out the size distribution analysis, the size distribution of a standard is provided.Analysis to the wet cake/lime carbonate of hydrocellulose/carboxymethyl cellulose has obtained and independent lime carbonate result much at one, and this shows: big relatively calcium carbonate granule has been arranged analysis, and has almost hidden all smaller particles.For overcoming this effect, the dispersion of the powder that embodiment 1 is made with the rotating speed of 8000rpm was carried out centrifugation 15 minutes.Remove supernatant liquor and analyze by scattering of light.Analytical results shows: wherein its particle diameter of 100% particle is less than 0.7 micron, and its particle diameter of about 90% particle is less than 0.3 micron.Particle size range is at 0.1 to 0.7 micron, and mean particle size is lower than 0.2 micron slightly.By gravity method and light scattering method,, two kinds of commercially available prod are analyzed in conjunction with identical centrifugation.Result's contrast of these three analyses is listed in the table 7.
Table 7
| Sample | Embodiment | RC-581 a | CL-611 b |
| Colloid % weight c | 98.8 | 61.2 d | 67.4 d |
| Size distribution | |||
| Bulk sample | Inapplicable c | 0.5-275 micron | 0.4-50 micron |
| Median size | Inapplicable | 17.03 micron | 8.29 micron |
| The sample of centrifugation | 0.1-0.7 micron | 0.2-0.9 micron | 0.1-0.7 micron |
| Median size | ＜0.2 micron | 0.31 micron | About 0.25 micron |
aAvicel
RC-581, FMC Corp., Philadelphia, PA 19103
bAvicel
CL-611, FMC Corp., Philadelphia, PA 19103
cThe colloidal per-cent of measuring according to the method for embodiment 3
dAdd the bulk sample amount of carboxymethyl cellulose in Mierocrystalline cellulose
eInapplicable owing to the lime carbonate of existence 50%.
Avicel
The CL-611 Mierocrystalline cellulose is one of most colloid microcrystalline cellulose cellulosic material of present industrial use, but in this material only about 67-68% in the particle size range that 100% material of the present invention is found.In addition, Avicel
The cellulosic median size of CL-611 is obviously greater than the cellulosic median size of the present invention.Avicel
The RC-581 Mierocrystalline cellulose has even bigger median size, and its colloidal content compares Avicel
The CL-611 Mierocrystalline cellulose is low.
Embodiment 17
The small beaker that will comprise 30 gram propylene glycol is heated to 50 ℃, and utilizes the Lightnin mixing tank to stir, to dissolve 1 gram methyl p-hydroxybenzoate and 0.1 gram propylparaben.When mixing is finished, this solution is added in the gram of 400 in the 2 liters of mixing tanks deionized water.After finishing mixing, 200 gram 70% Sorbitol Solution USPs (USP) and 1.6 gram soluble saccharins (USP) are added in this aqueous solution, and mix, till dissolving fully.Then, adding 100 grams mixed ten minutes with the Scott Turbon mixing tank that 2000rpm moves according to the embodiment 4 described simultaneously treated Microcrystalline Cellulose/lime carbonate that makes/carboxymethyl cellulose powder and utilization.This graceful suspension is pourable, and its viscosity number is measured as 120cps according to the Carrimed rheometer with the 6rpm operation.At the beginning, this suspension is seemingly stable, and at 4 ℃, 25 ℃, 30 ℃ and 40 ℃ store three months and still can keep stable afterwards.In this antacid suspension energy of 10 milliliters and 11.5 millinormal acid.
Embodiment 18
The small beaker that will comprise 15 gram propylene glycol is heated to 50 ℃, and utilizes the Lightnin mixing tank to stir, to dissolve 0.5 gram methyl p-hydroxybenzoate and 0.05 gram propylparaben.When mixing is finished, this solution is added in the gram of 200 in the 1 liter of mixing tank deionized water.After finishing mixing, 100 gram 70% Sorbitol Solution USPs (USP) and 0.8 gram soluble saccharin (USP) are added in this aqueous solution, and mix, till dissolving fully.Then, add 75 grams according to the Microcrystalline Cellulose/lime carbonate/carboxymethyl cellulose powder of the embodiment 4 described co-processing that make and utilize the Lightnin mixing tank to mix ten minutes.Add the deionized water of capacity, so that the cumulative volume of this dispersion reaches 0.5 liter, this suspension is mixed, until evenly, this suspension has the outward appearance of beating emulsifiable paste.In the suspension of this whipping, add 160 milligrams of paracetamol.Make the thorough mixing of respectively preparing burden, thereby produce the available spoon suspension that get, that beat the emulsifiable paste shape of paracetamol.
Claims (18)
1, a kind of microcrystalline cellulose compositions of extra-fine grinding comprises the protective colloid that microcrystalline cellulose crude granule, abrasive and selectivity are added; Wherein its particle diameter of microcrystalline cellulose crude granule of 80-100% weight is not more than 1 micron, and described abrasive is moisture K
SpBe equal to or less than 1 * 10
-7Ionic species, or solubleness is equal to or less than 40% powder or particulate matter in 100 ℃ water, this abrasive is selected from: lime carbonate, titanium dioxide, tricalcium phosphate, Lin Suanergai, silica, talcum and lactose; And in the described microcrystalline cellulose compositions, the weight ratio of Microcrystalline Cellulose and abrasive is in 85: 15 to 30: 70 scope, and when having protective colloid, the weight ratio of Microcrystalline Cellulose and protective colloid is 95: 5 to 70: 30.
2, the composition of claim 1 wherein uses protective colloid.
3, the composition of claim 1, wherein, the particle diameter of the Microcrystalline Cellulose of at least 90% weight is not more than 0.75 micron.
4, the composition of claim 1, wherein, the median size of Microcrystalline Cellulose is in the scope of 0.1-0.7 micron.
5, the composition of claim 1, said composition is the dried residue of the suspension of Microcrystalline Cellulose, abrasive and protective colloid, wherein abrasive is selected from: lime carbonate, titanium dioxide, tricalcium phosphate, Lin Suanergai, talcum and lactose; Protective colloid is selected from: carboxymethyl cellulose and pectin.
6, the composition of claim 1, wherein, described Microcrystalline Cellulose particle grain size is by in the presence of described abrasive, and the wet cake of Microcrystalline Cellulose is carried out wet lapping and obtains, and the solid content of being represented by Microcrystalline Cellulose and abrasive in the wet lapping is the 30-80% of blend weight.
7, the composition of claim 5, wherein, described Microcrystalline Cellulose particle grain size is by in the presence of described abrasive, and the wet cake of Microcrystalline Cellulose is carried out wet lapping and obtains, and the solid content of being represented by Microcrystalline Cellulose and abrasive in the wet lapping is the 30-80% of blend weight.
8, a kind of preparation method of ultra-fine microcrystalline cellulose compositions comprises the steps:
(a) protective colloid that Microcrystalline Cellulose, abrasive and the selectivity of not grinding are added is blended together, and wherein, employed abrasive is moisture K
SpBe equal to or less than 1 * 10
-7Ionic species, or solubleness is equal to or less than 40% powder or particulate matter in 100 ℃ water, this abrasive is selected from: lime carbonate, titanium dioxide, tricalcium phosphate, Lin Suanergai, silica, talcum and lactose; The solid content of being represented by Microcrystalline Cellulose and abrasive is in 30% to 80% scope of blend weight, the weight ratio of Microcrystalline Cellulose and abrasive is in 85: 15 to 30: 70 scope, when using protective colloid, the weight ratio of Microcrystalline Cellulose and protective colloid is 95: 5 to 70: 30;
(b) make blend stand the high-shear wet lapping of certain hour under shearing force, described shearing force is enough to make the particle diameter of Microcrystalline Cellulose to be reduced to: wherein the particle diameter of the Microcrystalline Cellulose of 80-100% weight is not more than 1 micron; With
(c) reclaim resulting ultra-fine microcrystalline cellulose compositions.
9, the method for claim 8 is wherein used protective colloid.
10, a kind of food that adds calcium, it comprises: be suspended in the nutraceutical dispersion in the composition of claim 1 of stable quantity.
11, the food of claim 10, it comprises the VITAMIN, mineral substance of therapeutic dose or magnitude of recruitment or both.
12, a kind of calcium milk-product that add, wherein, these milk-product are stablized with the composition of claim 1.
13, claim 12 add the calcium milk-product, wherein, milk-product are lipopenicillinase breasts.
14, a kind of food that comprises frozen confection, this food composition stable of claim 1.
15, a kind of liquid composition comprises the composition with the water-fast substantially medicament blended claim 1 of water and biologic effective dose.
16, the microcrystalline cellulose compositions of a kind of extra-fine grinding as claimed in claim 1, comprise the microcrystalline cellulose crude granule, described particle grain size distribution is not more than 0.7 micron and be colloid-stabilised being as the criterion with the particle diameter of the Microcrystalline Cellulose of at least 95% weight when disperseing.
17, a kind of pourable aqeous suspension comprises the composition of claim 1 and is selected from the auxilliary batchings that add of following one or more: alkyl diol, alkyl paraben, sorbyl alcohol, asccharin, and composition thereof.
18, a kind of suspension of available spoon of whipping of getting, has the outward appearance of beating emulsifiable paste, tissue and denseness, it comprises the composition of claim 1 and is selected from the auxilliary batchings that add of following one or more: alkyl diol, alkyl paraben, sorbyl alcohol, asccharin, and composition thereof.
Applications Claiming Priority (4)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| US4947997P | 1997-06-12 | 1997-06-12 | |
| US60/049,479 | 1997-06-12 | ||
| US4954497P | 1997-06-13 | 1997-06-13 | |
| US60/049,544 | 1997-06-13 |
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|---|---|
| CN1278830A CN1278830A (en) | 2001-01-03 |
| CN1086189C true CN1086189C (en) | 2002-06-12 |
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ID=26727210
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|---|---|---|---|
| CN98806151A Expired - Fee Related CN1086189C (en) | 1997-06-12 | 1998-06-12 | Ultra-fine microcrystalline cellulose compositions and process for their manufacture |
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| CN (1) | CN1086189C (en) |
| HK (1) | HK1030223A1 (en) |
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| WO1994012043A1 (en) * | 1992-11-25 | 1994-06-09 | Fmc Corporation | A low fat spread and process for making same |
| CN1138455A (en) * | 1995-05-26 | 1996-12-25 | 科尔加特·帕尔莫利弗公司 | Silica abrasive dentifrice of reduced stringiness and improved flavor |
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| Publication number | Publication date |
|---|---|
| CN1278830A (en) | 2001-01-03 |
| HK1030223A1 (en) | 2001-04-27 |
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