CN103981749A - Method used for preparing microcrystalline cellulose from reed pulp - Google Patents
Method used for preparing microcrystalline cellulose from reed pulp Download PDFInfo
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- CN103981749A CN103981749A CN201410000319.4A CN201410000319A CN103981749A CN 103981749 A CN103981749 A CN 103981749A CN 201410000319 A CN201410000319 A CN 201410000319A CN 103981749 A CN103981749 A CN 103981749A
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Abstract
The invention discloses a preparation method of microcrystalline cellulose. According to the preparation method, reed vegetable fiber is taken as a raw material, an organic acid or an inorganic acid is taken as a solvent; the reed vegetable fiber is mixed with the acid, an obtained mixture is delivered into a reactor; reaction is carried out for 20 to 150min at a temperature of 30 to 110 DEG C, with an acid solution concentration of 0.1 to 10%, and at a feed-to-liquid ratio of 1:2-1:30; an obtained undissolved material is collected, and is subjected to washing, drying, and smashing so as to obtain microcrystalline cellulose. The method is capable of solving problems that microcrystalline cellulose production is short of raw materials, and production cost is high; the novel raw material and the preparation method capable of realizing industrialized production of microcrystalline cellulose are provided; raw material source is wide; the method is simple,and is high in efficiency; and additional value is high.
Description
Technical field
The present invention relates to biorefinery technology, particularly relate to the technology that reduces production costs and save the energy simultaneously and increase added value in biorefinery process, specifically from plant cellulose reed pulp, extract the method for microcrystalline cellulose.
Background technology
Making full use of renewable green resource, is the important content of Green Chemistry research.Cellulose is as the natural macromolecular material of occurring in nature output maximum, and it is reasonably used is the effective method that solves the environment of advanced facing mankind and resource problem.From protection and the biodegradable feature of sustainable development, environment, people, for utilizing native cellulose, produce various cellulose derivatives and have expressed very large expectation, have good industrial prospect.Carry out the research of reed pulp, exploitation cellulose derivative, makes reed pulp high-valued, contributes to the application reed pulp of maximum profit, and this will produce good social benefit, environmental benefit and economic benefit.
Microcrystalline cellulose (MCC) be native cellulose through dilute acid hydrolysis the solid product to levelling off degree of polymerization (LODP).MCC has many good characteristics, such as purity is high, chemical stability is high, pollution-free, wear intensity is low, have good compressibility, disintegration rapidly, good fluidity etc., can be used as anticaking agent, filler, disintegrant, free-flow agent, lubricant, sugar-coat additive etc., be widely used in the industry such as pharmacy, food chemistry.Due to more and more wider purposes, its market prospects are good especially.The U.S. is microcrystalline cellulose largest production state of the world, is secondly Brazil and Japanese.Along with economic globalization, the production of various countries' microcrystalline cellulose is also tending towards synchronized development.Current China microcrystalline cellulose industry development is rapid, and continuous expansion trend appears in production, adds national industrial policies encouragement, and the concern of investor to enterprise of China newly-increased investment project, all further promotes the development of China's microcrystalline cellulose industry.
Summary of the invention
The present invention bases oneself upon China's biorefinery present situation, processes pulp with certain acid solution, ensureing to extract under the prerequisite of quality, extracts the microcrystalline cellulose in pulp, and being intended to provides production method for the development and utilization of reed raw material extraction microcrystalline cellulose.Process of the present invention is shown in shown in accompanying drawing 1.
Object is achieved through the following technical solutions:
In order to improve the solubility property of raw material, can be made into fine hair shape, then do dry processing, dry run can adopt the whole bag of tricks, in order not change the characteristic of string, preferably adopts low-temperature vacuum drying.The pulp of dried fine hair is dissolved in the acid solution in reactor, and the solvent here should be inorganic acid or organic acid or the two mixed solution.The concentration of the preferred described acid solution of preparation method of the present invention is 0.1% ~ 10%, and solid-liquid ratio is 1:2 ~ 1:30, and reaction temperature is 30 DEG C ~ 110 DEG C, and the reaction time is 20min ~ 150min.
When course of dissolution finishes, can adopt the method such as centrifugal sedimentation or filtration, isolate not dissolved matter wherein, and be washed with water to neutrality, be dried, pulverize and make microcrystalline cellulose.
Brief description of the drawings
Fig. 1 is process flow sheet of the present invention.
beneficial effect
Compared with prior art, tool has the following advantages in the present invention:
1. from raw material aspect, current production both domestic and external is mainly taking cotton, wood pulps as raw material, and cost is higher, prepares MCC also do not form large-scale industrial production taking cotton linter, straw, bagasse as raw material.Because reed raw material sources are extensive, cost is lower, less on the impact of environment, can create higher economic benefit, is the direction developing.Carry out the research of reed pulp, exploitation cellulose derivative, makes reed pulp high-valued, contributes to the application reed pulp of maximum profit, and this will produce good social benefit, environmental benefit and economic benefit.
2. in the present invention, adopt acid solution to process pulp and extract microcrystalline cellulose, can in existing biorefinery flow process, apply very easily, by the optimization to extraction process condition, obtained extracting the optimum process condition of microcrystalline cellulose.
Detailed description of the invention
Below in conjunction with the extraction conditions of microcrystalline cellulose in the present invention and the degree of polymerization and the degree of crystallinity etc. of microcrystalline cellulose, the invention will be further described, following non-limiting example can make the present invention of those of ordinary skill in the art's comprehend, but does not limit the present invention in any way.
embodiment 1
1. reed pulp is broken into fine hair shape, equilibrium water conten, gets pulp after treatment (separately materials and measure moisture) and packs in conical flask simultaneously, taking solid-liquid ratio as 1:7, adding concentration is 8% acid solution, after sealing, keeping reaction temperature is 100 DEG C, and the reaction time is 75min, then cooling, dilute, leave standstill after solid-liquid layering, separate solid content, be washed till neutrality (centrifugation solid content), dry, pulverize to obtain microcrystalline cellulose.
2. gained microcrystalline cellulose: degree of polymerization 201Lg-1, degree of crystallinity 74%, yield 84%, ash content 0.10%.
embodiment 2
1. reed pulp is broken into fine hair shape, equilibrium water conten, gets pulp after treatment (separately materials and measure moisture) and packs in conical flask simultaneously, taking solid-liquid ratio as 1:15, adding concentration is 10% acid solution, after sealing, keeping reaction temperature is 90 DEG C, and the reaction time is 60min, then cooling, dilute, leave standstill after solid-liquid layering, separate solid content, be washed till neutrality (centrifugation solid content), dry, pulverize to obtain microcrystalline cellulose.
2. gained microcrystalline cellulose: degree of polymerization 160Lg-1, degree of crystallinity 66%, yield 80%, ash content 0.12%.
embodiment 3
1. reed pulp is broken into fine hair shape, equilibrium water conten, gets pulp after treatment (separately materials and measure moisture) and packs in conical flask simultaneously, taking solid-liquid ratio as 1:20, adding concentration is 9% acid solution, after sealing, keeping reaction temperature is 85 DEG C, and the reaction time is 120min, then takes out cooling, dilute, leave standstill after solid-liquid layering, separate solid content, be washed till neutrality (centrifugation solid content), dry, pulverize to obtain microcrystalline cellulose.
2. gained microcrystalline cellulose: degree of polymerization 216Lg-1, degree of crystallinity 65%, yield 82%, ash content 0.05%.
embodiment 4
1. reed pulp is broken into fine hair shape, equilibrium water conten, gets pulp after treatment (separately materials and measure moisture) and packs in conical flask simultaneously, taking solid-liquid ratio as 1:10, adding concentration is 7% acid solution, after sealing, keeping reaction temperature is 60 DEG C, and the reaction time is 140min, then takes out cooling, dilute, leave standstill after solid-liquid layering, separate solid content, be washed till neutrality (centrifugation solid content), dry, pulverize to obtain microcrystalline cellulose.
2. gained microcrystalline cellulose: degree of polymerization 235Lg-1, degree of crystallinity 71%, yield 86%, ash content 0.09%.
embodiment 5
1. reed pulp is broken into fine hair shape, equilibrium water conten, gets pulp after treatment (separately materials and measure moisture) and packs in conical flask simultaneously, taking solid-liquid ratio as 1:16, adding concentration is 6% acid solution, after sealing, keeping reaction temperature is 80 DEG C, and the reaction time is 90min, then cooling, dilute, leave standstill after solid-liquid layering, separate solid content, be washed till neutrality (centrifugation solid content), dry, pulverize to obtain microcrystalline cellulose.
2. gained microcrystalline cellulose: degree of polymerization 277Lg-1, degree of crystallinity 80%, yield 88%, ash content 0.09%.
In sum, from embodiment 1,2,3,4,5 result of the tests: acid solution is the good solvent that extracts microcrystalline cellulose, it is considerable that acid solution is extracted yield to reed pulp, and the degree of polymerization of the prepared microcrystalline cellulose of acid system and degree of crystallinity, ash content are all within theory is prepared the scope that microcrystalline cellulose obtains.Datum Argument provided by the present invention reed pulp can be used as raw material produce microcrystalline cellulose.
Claims (7)
1. the invention is characterized in taking string reed pulp as raw material, produce microcrystalline cellulose, organic or inorganic acid equal solvent dissolves the amorphous region of plant cellulose, retains crystal region, thereby makes microcrystalline cellulose.
2. pulp according to claim 1, in order to improve its solvability, preferably by its fine hair.
3. fine hair pulp according to claim 1, in order to improve its dissolubility in solvent, can adopt various drying process methods, and preferably low-temperature vacuum drying, to remove its contained humidity as far as possible.
4. preparation method according to claim 1, the concentration that it is characterized in that described acid solution is 0.1% ~ 10%.
5. preparation method according to claim 1, is characterized in that described solid-liquid ratio is 1:2 ~ 1:30.
6. preparation method according to claim 1, is characterized in that described reaction temperature is 30 DEG C ~ 110 DEG C.
7. preparation method according to claim 1, is characterized in that the described reaction time is 20min ~ 150min.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201410000319.4A CN103981749A (en) | 2014-01-02 | 2014-01-02 | Method used for preparing microcrystalline cellulose from reed pulp |
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| Application Number | Priority Date | Filing Date | Title |
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| CN201410000319.4A CN103981749A (en) | 2014-01-02 | 2014-01-02 | Method used for preparing microcrystalline cellulose from reed pulp |
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| CN201410000319.4A Pending CN103981749A (en) | 2014-01-02 | 2014-01-02 | Method used for preparing microcrystalline cellulose from reed pulp |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104988779A (en) * | 2015-06-01 | 2015-10-21 | 苏州贝彩纳米科技有限公司 | Preparation method and application of Salix cheilophila nanocellulose |
| CN105839273A (en) * | 2016-04-29 | 2016-08-10 | 华南再生棉纱（梧州）有限公司 | Bamboo fiber flax towel manufacturing method |
| CN113336863A (en) * | 2021-05-14 | 2021-09-03 | 珠海市东辰制药有限公司 | Microcrystalline cellulose and preparation method thereof |
Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20030089465A1 (en) * | 2001-11-02 | 2003-05-15 | David Schaible | Process for producing microcrystalline cellulose |
| JP2004041119A (en) * | 2002-07-12 | 2004-02-12 | Asahi Kasei Chemicals Corp | Water-dispersible cellulose and method for producing the same |
| CN101070352A (en) * | 2007-03-27 | 2007-11-14 | 鲁东大学 | Method for preparing sheet-like microcrystal cellulose and modification processing method |
| CN101649569A (en) * | 2009-09-01 | 2010-02-17 | 陕西科技大学 | Process for preparing low-pollution wheatgrass microcrystalline cellulose |
| CN102817265A (en) * | 2012-08-20 | 2012-12-12 | 新疆光大山河化工科技有限公司 | Preparation method of arc-shaped microcrystalline cellulose |
-
2014
- 2014-01-02 CN CN201410000319.4A patent/CN103981749A/en active Pending
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20030089465A1 (en) * | 2001-11-02 | 2003-05-15 | David Schaible | Process for producing microcrystalline cellulose |
| JP2004041119A (en) * | 2002-07-12 | 2004-02-12 | Asahi Kasei Chemicals Corp | Water-dispersible cellulose and method for producing the same |
| CN101070352A (en) * | 2007-03-27 | 2007-11-14 | 鲁东大学 | Method for preparing sheet-like microcrystal cellulose and modification processing method |
| CN101649569A (en) * | 2009-09-01 | 2010-02-17 | 陕西科技大学 | Process for preparing low-pollution wheatgrass microcrystalline cellulose |
| CN102817265A (en) * | 2012-08-20 | 2012-12-12 | 新疆光大山河化工科技有限公司 | Preparation method of arc-shaped microcrystalline cellulose |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104988779A (en) * | 2015-06-01 | 2015-10-21 | 苏州贝彩纳米科技有限公司 | Preparation method and application of Salix cheilophila nanocellulose |
| CN105839273A (en) * | 2016-04-29 | 2016-08-10 | 华南再生棉纱（梧州）有限公司 | Bamboo fiber flax towel manufacturing method |
| CN113336863A (en) * | 2021-05-14 | 2021-09-03 | 珠海市东辰制药有限公司 | Microcrystalline cellulose and preparation method thereof |
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Application publication date: 20140813 |