CN103710470A - Process for preparing sugar by two-step method and device thereof - Google Patents

Process for preparing sugar by two-step method and device thereof Download PDF

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CN103710470A
CN103710470A CN201310729069.3A CN201310729069A CN103710470A CN 103710470 A CN103710470 A CN 103710470A CN 201310729069 A CN201310729069 A CN 201310729069A CN 103710470 A CN103710470 A CN 103710470A
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exchange resin
sucrose
step method
ion exchange
penetrating fluid
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CN103710470B (en
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彭文博
凌国庆
张宇
江健
张宏
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Jiangsu Jiuwu Hi Tech Co Ltd
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Abstract

The invention discloses a process for preparing sugar by a two-step method and a device thereof. The process comprises the following steps: adding water into crude sugar for dissolving to obtain crude syrup; feeding the crude syrup into a primary filter and a micro-filtration membrane in sequence for filtering to obtain filtrate; feeding the filtrate into a first ion exchange resin tower to obtain a first penetrating fluid, wherein the first ion exchange resin refers to macroporous strong-basicity anion exchange resin; feeding the first penetrating fluid into a second ion exchange resin tower to obtain a second penetrating fluid, wherein the second ion exchange resin refers to strong-acidity cation exchange resin, weak-acidity cation exchange resin or a mixing bed of anion and cation exchange resin; feeding the second penetrating fluid into an evaporator for concentrating to obtain sucrose concentrated liquor; and crystallizing, centrifuging and drying to obtain a sucrose finished product. The process disclosed by the invention can be used for producing high-purity refined sucrose in batch, wherein a pigment removal rate reaches 99.9%, a salt removal rate reaches 98%, and sucrose component of the product reaches 99.9% which reaches the standard of national senior sugar.

Description

A kind of technique and device of two step method sugaring
 
Technical field
The technique and the device that the present invention relates to a kind of two step method sugaring, belong to sugar refining field.
 
Background technology
The sugaring of most of developed countries is the Closed Circulation in Sugar Production method that adopts " two step method " in the world.Most sugar refinery produces raw sugar, then supplies with refinery and produces refined sugar." two step method " sugaring is that sugar material first uses comparatively simple technique (lime method) to produce raw sugar (being raw sugar), back dissolving again, after purifying, white sugar is produced in crystallization again, as produced refined sugar (being the white sugar that purity is higher, colour is lower, impurity a kind of high target still less requires), aspect decolouring, desalination, need pass through again the processing of the aspects such as ion-exchange.The major advantage of " two step method " is, through post-defecation impurity elimination, secondary crystal is purified, and quality product is high, can meet the demand of top-grade consumption.Purified sugar production and sales throughout the year, produce flexibly according to market situation, do not have the impact of Metamorphic Factors, and the good price of quality is high.In " two step method " because the method for lime legal system raw sugar is easy, the process flow of sugarcane production raw sugar is the shortest, can within the shortest time, produce raw sugar, and during due to production raw sugar, methose and biose mix all as the product of raw sugar, reduce in a large number steam consumption, reduce non-physical loss, therefore under same system refining appointed condition, throughput can improve 20-30%.
But the production of existing refined sugar is to adopt original lime method precipitation to add the technique that sulphur floats.The method has following shortcoming: first, used filter press, belong to more traditional, level of automation is lower, labor-intensive equipment, the work under bad environment of this equipment, production efficiency is low, and filtering accuracy is inadequate, can not effectively remove the impurity such as colloid in syrup, tannin, bring larger production load can to operation section below; The second, used lime method precipitation technology, can produce a large amount of residues, environmental pollution is more serious, and introduces aborning new impurity---ash content, causes quality product lower; The 3rd, the decolouring of this technique is to use stove drying method, has sulphur remnants in product, harmful to HUMAN HEALTH, and the sugar bleach of sulfurous gas, understands generation color development phenomenon after being long placed in.Along with the further raising of country to food safety requirements, the method will be limited to use; The 4th, do not use ion-exchange desalination, cannot remove salinity remaining in liquid glucose, cause product ash content higher, quality is lower or defective, and the 4th, used traditional triple-effect evaporator, wasted a large amount of energy, the modern techniquies such as MVR of comparing, energy consumption is higher.The 5th, relevant processing parameter does not reach optimization, causes the waste of the energy.In view of this, still await proposing the production technique of " two step method " sugaring of a kind of optimization.
 
Summary of the invention
The object of the invention is to overcome the deficiencies in the prior art, " two step method " sugar industry technique of a kind of comparatively energy-conserving and environment-protective, less investment is provided, it has pollution-free, and quality product is high, and technical process is short, and energy consumption is low, invest little, the feature such as floor space is little.Technical scheme is as follows:
A technique for two step method sugaring, comprises the steps:
The 1st step, obtain raw sugar slurry after raw sugar is dissolved in water, by raw sugar slurry send into coarse filter successively, microfiltration membrane is filtered, and obtains filtrate;
The 2nd step, filtrate is sent into the first exchange resin tower, obtain the first penetrating fluid, the first described ion exchange resin refers to macroporous strong basic anionite-exchange resin;
The 3rd step, the first penetrating fluid is sent into the second exchange resin tower, obtain the second penetrating fluid, the second described ion exchange resin refers to the mixed bed of storng-acid cation exchange resin, weakly acidic cation-exchange resin or anion-cation exchange resin;
The 4th step, that the second penetrating fluid is sent into vaporizer is concentrated, obtains sucrose concentrated solution, then through crystallization, centrifugal, dry, obtains sucrose finished product.
In the 1st step, the mass concentration of raw sugar slurry preferably 40%~80%, can guarantee that raw sugar syrup has suitable viscosity, also can guarantee explained hereafter efficiency, if can make the viscosity of syrup too high when concentration is excessive, it is required that in coarse filter and microfiltration membrane, flux is not suitable for engineering, if concentration is too low, can cause feed liquid rarer, follow-up evaporative process energy consumption is bigger than normal, and crystallization yields is low.Preferred, mass concentration is 60%, under this concentration range, the solubleness that can guarantee macromole in raw sugar, colloidal impurity is low, can be held back by microfiltration membrane, guarantees the quality product of follow-up sucrose finished product, also can guarantee that the viscosity of syrup is less simultaneously, the flux of later stage membrane filtration is larger, and the steam output of postorder is also less, can guarantee higher production efficiency.Coarse filter in this step includes but are not limited to: deep bed filter or screen cloth (aperture of screen cloth is preferably 0.1 μ m-5 μ m) etc., fully to remove oarse-grained impurity.Microfiltration membrane preferably adopts ceramic microfiltration membrane, and it has advantages of, and physical strength is high, acid-alkali-corrosive-resisting, filtering accuracy are high.The effect of microfiltration membrane is to remove some granule foreigns in raw sugar syrup, colloid etc., can improve purity and the quality of product.In order to make filter effect more excellent, need to select the size of the mean pore size of microfiltration membrane.If mean pore size is too little, can cause filtration flux too little, can cause filtration flux too low, and the sucrose of a part of larger particles can be trapped, have influence on yield, if mean pore size is too large, can cause a part of impurity to see through rete and enter to per-meate side, have influence on the quality of product.The mean pore size scope of preferred microfiltration membrane is 50~500 nm.The temperature of microfiltration process is relevant with sucrose and impurity, the solubleness of colloid and the viscosity of system, if excess Temperature, can cause impurity, colloid to be also dissolved in material, cannot obtain separated removal, if temperature is too low, can cause a part of sucrose not dissolve, separated film is held back, and whole yield is reduced, preferably temperature is 50~90 ℃, at this temperature, can also guarantee preferably that flux is large and suppression ratio is slower, energy consumption is relatively low simultaneously.When if filter pressure is less than normal, can cause flux low, do not conform to and be suitable for engineering actual demand, when if pressure is excessive, can cause a part of most of impurity to be pressed, see through rete, cause product quality bad, and can produce more serious Pore Blocking, and make it be difficult for being cleaned, preferred filter pressure is 0.1~0.5MPa.
In the 2nd step, macroporous strong basic anionite-exchange resin has the effect of desalination and decolouring, and can remove some negatively charged ion in sucrose liquid, and has the effect of decolouring.Preferred, the blade diameter length ratio of the first exchange resin tower is 1/3~1/10, and flow velocity is 2~10BV/h, and temperature is 40~80 ℃.Contriver finds, at adsorption tower blade diameter length ratio, is 1/8, and flow velocity is 4 BV/h, when temperature is 60 ℃, the viscosity of liquid glucose is less, and the best results of absorption can guarantee decolorizing effect, can guarantee higher production efficiency again, energy consumption is relatively low simultaneously, and the yield of sucrose is higher.
In the 3rd step, ion exchange resin is strongly-acid or weakly acidic cation-exchange resin, can be also the mixed bed of anion-cation exchange resin, and it can play the cationic effect that removes, and also can play the effect of decolouring.Described the second exchange resin tower blade diameter length ratio is 1/3~1/10, and flow velocity is 2~10BV/h, and temperature is 30~70 ℃.In addition, contriver finds, at adsorption tower blade diameter length ratio, is 1/5, and flow velocity is 4BV/h, and when temperature is 50 ℃, the best results of desalination, can slough 95% salinity, and the yield of sucrose is higher simultaneously.
In the 4th step, vaporizer preferably adopts MVR vaporizer (Mechanical Vapor Recompression), and thickening temperature is 30~80 ℃, treats that it is 1.05 left and right that liquid glucose is concentrated to supersaturation degree, decrease temperature crystalline; Wherein rearing crystal time is 1.5h, and cooling rate is 0.2~1 ℃/min, is preferably 0.4 ℃/min, cools the temperature to 5 ℃.During centrifugation, centrifugal rotational speed is 5000~8000rpm; Preferably forced air drying, drying temperature is 90~100 ℃.
In an optimum embodiment of the present invention, the mean pore size of microfiltration membrane is 200 nm, the filtration temperature of micro-filtration is 70 ℃, the transmembrane pressure of micro-filtration is 0.4 MPa, under this parameter area, the microfiltration membrane of 200 nm is held back some fat, the protein of getting rid of in sucrose, and this can guarantee the life of ion exchange resin, and can prevent that resin from, by macromole impurity absorption, having influence on the decreasing ratio for salt and pigment.
Method based on above-mentioned, another object of the present invention has been to provide a kind of device of two step method sugaring, includes the coarse filter, microfiltration membrane, the first ion exchange resin column, the second ion exchange resin column, vaporizer, crystallizer, whizzer, the moisture eliminator that connect successively.
Further, the mean pore size of described microfiltration membrane is 50~500 nm.
What further, in the first described ion exchange resin column, fill is macroporous strong basic anionite-exchange resin.
What further, in the second described ion exchange resin column, fill is storng-acid cation exchange resin or weakly acidic cation-exchange resin.
 
beneficial effect
Technique tool of the present invention has the following advantages:
1, adopt above-mentioned technique, can the highly purified refined sucrose of Mass production, in embodiment preferably, the pigment removal of product reaches 99.9%, the clearance of salinity reaches 98%, the Sucrose of product reaches 99.9%, and electricity is led ash content lower than 0.01%, and content of sulfur dioxide does not detect, reach the standard of national top grade sugar, simultaneously the rate of recovery of sucrose is more than 99%, and this sucrose finished product, after placing half a year, has no and returns look phenomenon in traditional technology.
2, this technique has been done a large amount of Optimization Works to the parameter of new installation and traditional technology, obtains optimum processing parameter, has guaranteed the energy-efficient operation of producing, and the quality of product is higher simultaneously.This production technique relative energy-saving, the traditional processing technology of comparing, level of automation is high, can save 70% labour cost, has reduced more than 25% production cost, remarkable in economical benefits.
3, with ceramic membrane, substitute traditional filter press and lime precipitation, saved filter press and lime method settling step, greatly shortened technical process, reduced human input on the one hand, improved production efficiency; Ceramic membrane compare traditional polymeric amide or polyether sulfone material organic membrane, can withstand high temperatures, high pressure, chemical corrosion, and work-ing life is longer; Also avoided on the other hand the pollution of solid waste to environment.
4, with ion exchange method decoloration process, substitute traditional stove drying technique, solved on the one hand the problem of sulphur remnants in finished product sucrose; Also the operation section of having saved on the other hand stove drying, reduces production cost;
5, use ion exchange method desalination, more effectively except the ash content in sugarcane juice, improve the quality of products.
6, concentrated with MVR equipment, greatly reduced energy consumption, and vaporization temperature is lower, can because temperature is high, not make sugared coking, produce new pigment.
7, production technique is comparatively simple, and flow process is shorter, and control process is simple, and personnel labor intensity and usage quantity greatly reduce, and production quality control is stable.
8, adopt membrane separation plant and ion-exchange unit, reduced the floor space of equipment, reduced capital construction cost.
 
Accompanying drawing explanation
Fig. 1 is sugar refining technology schema provided by the invention;
Fig. 2 is sugaring device schematic diagram provided by the invention.
 
Embodiment
Embodiment 1
A novel process for sugar industry, it comprises the following steps:
A, change sugar: raw sugar is heated to 80 ℃ of dissolvings by adding water, make syrup, sucrose content is about respectively 40%, 50%, 60%, 70%, 80% left and right;
B, pre-treatment: syrup is carried out to pre-treatment by sheet frame, remove colloid or larger particulate contamination; The precision of sheet frame filter cloth used is 0.1 μ m;
C, ceramic membrane filter: by the pretreated syrup of collecting, by microfiltration of ceramic membrane, mean pore size is 50 nm, and the temperature of filtration is 50 ℃, and filter pressure is 0.5Mpa, obtains syrup clear liquid;
D, one-level ion-exchange desalination: syrup clear liquid is carried out to ion-exchange desalination with macroporous strong basic anionite-exchange resin, also can play the effect of decolouring, the flow velocity in resin column is 2BV/h simultaneously, and temperature is 70 ℃, blade diameter length ratio is 1/3, and the hammer degree of the sucrose syrup obtaining is 55;
E, secondary ion-exchange desalination: the syrup obtaining in step D is carried out to desalination with anionite-exchange resin, also can play the effect of decolouring, the flow velocity in resin column is 10 BV/h simultaneously, and temperature is 30 ℃, blade diameter length ratio is 1/10, and the hammer degree of the sucrose syrup obtaining is 55;
F, concentrated: the syrup obtaining in step e is sent into MVR vaporizer, and thickening temperature is 65 ℃, and it is 1.05 that liquid glucose is concentrated to degree of supersaturation, obtains sucrose concentrated solution;
G, crystallization: add crystal seed, growing the grain 1.5h, then be slow cooling to 60 ℃ with the speed of 0.2 ℃/min, separate out crystallization of sucrose;
H, centrifugation: crystallization of sucrose is centrifugal with whizzer, rotating speed 8000rpm, time 25min;
I, dry: be dried about 4 hours at 90 ℃, obtain finished product, measure the indexs such as colour, percent of decolourization, ratio of desalinization, Sucrose and the rate of recovery.
Figure 2013107290693100002DEST_PATH_IMAGE001
As can be seen from the table, with the increase of sucrose content, there is downward trend in the rate of recovery of sucrose, and this is mainly due to after syrup concentration change greatly, cause having more sucrose to be trapped, and cannot reach certain cycles of concentration, still, when sucrose concentration is controlled to 60%, macromole in raw sugar can be reduced to solubleness, these impurity are more easily trapped, thereby have prevented that the impurity effects such as these colloids, albumen are to ion exchange resin, make it keep higher desalination and percent of decolourization.This sucrose finished product, after placing half a year, has no and returns look phenomenon in traditional technology.
 
Embodiment 2
A novel process for sugar industry, it comprises the following steps:
A, change sugar: raw sugar is heated to 80 ℃ of dissolvings by adding water, make syrup, sucrose content is respectively 60% left and right;
B, pre-treatment: syrup is carried out to pre-treatment by sheet frame, remove colloid or larger particulate contamination; The precision of sheet frame filter cloth used is 5 μ m;
C, ceramic membrane filter: by the pretreated syrup of collecting, by microfiltration of ceramic membrane, mean pore size is respectively 50 nm, 200 nm and 500 nm, and the temperature of filtration is 90 ℃, and filter pressure is 0.1Mpa, obtains syrup clear liquid;
D, one-level ion-exchange desalination: syrup clear liquid is carried out to ion-exchange desalination and decolouring with macroporous strong basic anionite-exchange resin, and the flow velocity in resin column is 10 BV/h, and temperature is 40 ℃, and blade diameter length ratio is 1/10, and the hammer degree of the sucrose syrup obtaining is 55;
E, secondary ion-exchange desalination: the syrup obtaining in step D is carried out to desalination and decolouring with anionite-exchange resin, and the flow velocity in resin column is 2 BV/h, and temperature is 70 ℃, and blade diameter length ratio is 1/3, and the hammer degree of the sucrose syrup obtaining is 55;
F, concentrated: the syrup obtaining in step e is sent into MVR vaporizer, and thickening temperature is 65 ℃, and it is 1.05 that liquid glucose is concentrated to degree of supersaturation, obtains sucrose concentrated solution;
G, crystallization: add crystal seed, growing the grain 1.5h, then be slow cooling to 60 ℃ with the speed of 0.2 ℃/min, separate out crystallization of sucrose;
H, centrifugation: crystallization of sucrose is centrifugal with whizzer, rotating speed 8000rpm, time 25min;
I, dry: be dried about 4 hours at 90 ℃, obtain finished product, measure the indexs such as colour, percent of decolourization, ratio of desalinization, Sucrose and the rate of recovery.
Figure 2013107290693100002DEST_PATH_IMAGE003
As can be seen from the table, when using the microfiltration membrane of 500 nm, there is more impurity can see through rete and enter into per-meate side, these impurity not only can have influence on the purity of product, also can have influence on the operating performance of ion exchange resin, the decrease in efficiency that causes desalination and decolouring, if while adopting the less microfiltration membrane in aperture, be affected the yield of product.
 
Embodiment 3
A novel process for sugar industry, it comprises the following steps:
A, change sugar: raw sugar is heated to 80 ℃ of dissolvings by adding water, make syrup, sucrose content is respectively 60% left and right;
B, pre-treatment: syrup is carried out to pre-treatment by sheet frame, remove colloid or larger particulate contamination; The precision of sheet frame filter cloth used is 4 μ m;
C, ceramic membrane filter: by the pretreated syrup of collecting, by microfiltration of ceramic membrane, mean pore size is 200 nm, and the temperature of filtration is respectively 50 ℃, 70 ℃, 90 ℃, and filter pressure is 0.4Mpa, obtains syrup clear liquid;
D, one-level ion-exchange desalination: syrup clear liquid is carried out to ion-exchange desalination and decolouring with macroporous strong basic anionite-exchange resin, and the flow velocity in resin column is 4 BV/h, and temperature is 60 ℃, and blade diameter length ratio is 1/8, and the hammer degree of the sucrose syrup obtaining is 55;
E, secondary ion-exchange desalination: the syrup obtaining in step D is carried out to desalination and decolouring with anionite-exchange resin, and the flow velocity in resin column is 4 BV/h, and temperature is 50 ℃, and blade diameter length ratio is 1/5, and the hammer degree of the sucrose syrup obtaining is 55;
F, concentrated: the syrup obtaining in step e is sent into MVR vaporizer, and thickening temperature is 65 ℃, and it is 1.05 that liquid glucose is concentrated to degree of supersaturation, obtains sucrose concentrated solution;
G, crystallization: add crystal seed, growing the grain 1.5h, then be slow cooling to 60 ℃ with the speed of 0.2 ℃/min, separate out crystallization of sucrose;
H, centrifugation: crystallization of sucrose is centrifugal with whizzer, rotating speed 8000rpm, time 25min;
I, dry: be dried about 4 hours at 90 ℃, obtain finished product, measure the indexs such as colour, percent of decolourization, ratio of desalinization, Sucrose and the rate of recovery.
Figure 2013107290693100002DEST_PATH_IMAGE005
As can be seen from the table, when higher micro-filtration temperature, can cause the solubleness of a part of impurity in material to raise, in the process of filtering, see through rete and enter to per-meate side, these impurity can have influence on life-span and percent of decolourization and the ratio of desalinization of resin, if filtration temperature is low, can cause cycles of concentration to promote, cause the rate of recovery of sucrose on the low side, under preferred condition, can reach 99% the rate of recovery and 99% Sucrose.

Claims (10)

1. a technique for two step method sugaring, is characterized in that, comprises the steps:
The 1st step, obtain raw sugar slurry after raw sugar is dissolved in water, by raw sugar slurry send into coarse filter successively, microfiltration membrane is filtered, and obtains filtrate;
The 2nd step, filtrate is sent into the first exchange resin tower, obtain the first penetrating fluid, the first described ion exchange resin refers to macroporous strong basic anionite-exchange resin;
The 3rd step, the first penetrating fluid is sent into the second exchange resin tower, obtain the second penetrating fluid, the second described ion exchange resin refers to the mixed bed of storng-acid cation exchange resin, weakly acidic cation-exchange resin or anion-cation exchange resin;
The 4th step, that the second penetrating fluid is sent into vaporizer is concentrated, obtains sucrose concentrated solution, then through crystallization, centrifugal, dry, obtains sucrose finished product.
2. the technique of two step method sugaring according to claim 1, is characterized in that: in the 1st described step, the mass concentration of raw sugar slurry is 40%~80%.
3. the technique of two step method sugaring according to claim 1, is characterized in that: in the 1st described step, the mean pore size scope of microfiltration membrane is 50~500 nm, and filtration temperature is 50~90 ℃, and micro-filtration pressure is 0.1~0.5MPa.
4. the technique of two step method sugaring according to claim 1, is characterized in that: in the 2nd described step, the blade diameter length ratio of the first exchange resin tower is 1/3~1/10, and feed velocity is 2~10BV/h, and feed temperature is 40~80 ℃.
5. the technique of two step method sugaring according to claim 1, is characterized in that: in the 3rd described step, the second exchange resin tower blade diameter length ratio is 1/3~1/10, and feed velocity is 2~10BV/h, and feed temperature is 30~70 ℃.
6. the technique of two step method sugaring according to claim 1, is characterized in that: in the 4th described step, vaporizer is to adopt MVR vaporizer, and thickening temperature is 30~80 ℃; Rearing crystal time in Crystallization Procedure is 1.5h, and cooling rate is 0.2~1 ℃/min, and during centrifugation, centrifugal rotational speed is 5000~8000rpm; Drying process is forced air drying, and drying temperature is 90~100 ℃.
7. a device for two step method sugaring, is characterized in that: include the coarse filter, microfiltration membrane, the first ion exchange resin column, the second ion exchange resin column, vaporizer, crystallizer, whizzer, the moisture eliminator that connect successively.
8. the device of two step method sugaring according to claim 7, is characterized in that: the mean pore size of described microfiltration membrane is 50~500 nm.
9. the device of two step method sugaring according to claim 7, is characterized in that: what in the first described ion exchange resin column, fill is macroporous strong basic anionite-exchange resin.
10. the device of two step method sugaring according to claim 7, is characterized in that: what in the second described ion exchange resin column, fill is storng-acid cation exchange resin or weakly acidic cation-exchange resin.
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