CN100507008C - Method of discoloring glucose saccharifying liquid by ion exchange resin - Google Patents
Method of discoloring glucose saccharifying liquid by ion exchange resin Download PDFInfo
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- CN100507008C CN100507008C CNB2006100688708A CN200610068870A CN100507008C CN 100507008 C CN100507008 C CN 100507008C CN B2006100688708 A CNB2006100688708 A CN B2006100688708A CN 200610068870 A CN200610068870 A CN 200610068870A CN 100507008 C CN100507008 C CN 100507008C
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Abstract
The invention discloses the method for decolouring dextroglucose liquid with ion exchange resin. The method comprises the following steps: confirming the temperature, concentration and flow velocity, putting the 35-45% liquid glucose into ion-exchange device at 40-50Deg.C and 2.5-4.0BV/h; or using activated charcoal to decolour liquid glucose, and then putting it into ion-exchange device. The light transmittance ratio of the decolour liquid is up to 100%, and the conductance is reduced to below 10 mus/cm.
Description
Technical field
The present invention relates to a kind of production method of crystalline dextrose, relate in particular to a kind of method that adopts ion exchange resin that glucose saccharifying liquid is decoloured.
Background technology
Glucose is a kind of monose, is the significant energy source of humans and animals, in food service industry and medicine trade purposes is very widely arranged.The color of glucose is very important Oranoleptic indicator of glucose product, selects a kind of not only economy but also very effective that decoloring method be the problem that numerous manufacturers extremely pay close attention to always.The production of glucose will can produce some pigments through high-temperature injection liquefaction in this process.Its pigment is the product of sugar and coloring matter precursors reaction.For example, class melanochrome then is (Maillard reaction) that sugar and amino acid effect generate, and another kind of pigment then is (as the caramel) that sugared degradation produces.Some coloring matter produces under alkaline condition, as the hexose degraded product.These organic compound generally are negatively charged ion in alkaline medium, have amphipathic characteristic, and existing wetting ability has hydrophobicity again.If not with colour removal, will have a strong impact on the Oranoleptic indicator of finished product, and the economic benefit of restriction manufacturer.
The widely used discoloring agent of glucose industry is a wood activated charcoal at present.Wood activated charcoal divides Powdered Activated Carbon and granulated active carbon, though the granulated active carbon decolorizing effect is fine and can regenerate, price is expensive (200,000 yuan per ton) too.Powdered Activated Carbon is the most commonly used, but in use there are a lot of drawbacks in it:
1. the powder activity carbon activity lost efficacy soon, and general general is 3-6 month;
2. Powdered Activated Carbon is non-renewable, can not reuse the cost height;
3. produce a large amount of dust in the Powdered Activated Carbon use, pollute environment;
4. saccharification liquid can cause that specific conductivity raises, and influences the liquid glucose quality after by gac;
5. Powdered Activated Carbon also has certain absorption to liquid glucose, and the sugar that contains in the breeze reaches more than 13%, influences product yield.
Summary of the invention
The objective of the invention is to overcome traditional deficiency, provide that a kind of to have method simple, good decolorizing effect, the method that the employing ion exchange resin of low cost and other advantages decolours to glucose saccharifying liquid with absorbent charcoal fine purification saccharification liquid.
For achieving the above object, the present invention has adopted following technical scheme:
A kind of method that adopts ion exchange resin that glucose saccharifying liquid is decoloured, its technological process be,
A. glucose saccharifying liquid is handled, obtained dry-matter and be 35～45% glucose saccharifying liquid, be beneficial to ion exchange unit and reach the maximum adsorption effect;
B. with the gained glucose saccharifying liquid under 40 ℃～50 ℃ temperature, send into ion exchange unit with the 2.5-4.0BV/h flow and decolour, resin absorption amount maximum, best results under this flow; This temperature then helps resin performance adsorption effect, reduces the destruction to resin;
C. make finished product at purifying or after making with extra care.
Before glucose saccharifying liquid enters ion exchange unit, carry out activated carbon decolorizing among the described step b earlier, promptly use gac to decolour earlier with respect to saccharification liquid butt amount 0.5-1.5%.
Used ion-exchange unit is the positively charged ion and the anion-exchange resin column of serial connection among the described step b, calculating after wherein the resin Intake Quantity expands by resin is the 70-90% of column volume, yin and yang resin is just being washed backwash then earlier, using acid-base pretreatment again, then saccharification liquid is being decoloured.
Described step a comprises following technology
1) size mixing, in material-compound tank starch milk is transferred to 16-20Be, add the high temperature resistant α-Dian Fenmei of 0.45%-0.55%L/T butt, Jet liquefier is squeezed into pump in the back that stirs;
2) liquefaction, powder slurry and steam meet in Jet liquefier, and drop temperature is controlled at 95-110 ℃, and the feed liquid of coming out from injector enters the laminar flow jar after cooling, carry out second spraying, this sprays feed liquid and steam directly mixes, and temperature rises to more than 110 ℃, with the thorough deactivation of α-Dian Fenmei, then, feed liquid is cooled to 80-100 ℃ of insulation through the vacuum cooling system, cools to 40-65 ℃ under the qualified situation of iodine examination, simultaneously the liquid glucose pH value is transferred between the 3.5-6.5;
3) saccharification adds saccharifying enzyme, keeps saccharification about 45-60 hour, reach the saccharification terminal point after, rise to 70-90 ℃ with injector and reach the enzyme purpose of going out;
4) filter, the pH value of liquid glucose is transferred to 4.0～5.5 temperature be controlled between 60-80 ℃, remove by filter albumen through precoating formula vacuum-type drum filter.
Described step c comprises following technology
1) evaporation concentration, the liquid glucose after the decolouring is to be concentrated to 60-80% under the 60-90 ℃ of condition with the multiple-effect falling film vaporizer at vacuum tightness 0.5-1.1mpa and temperature;
2) crystallization, with pump liquid glucose is imported the multistage crystallization jar, in the one-level crystallizer, stirred 2 hours, after under the 40-50 ℃ of temperature crystallization 5-12 hour, inject secondary jar, three grades of jars, level Four jar etc. in order successively, quicken blowing with uniform flow stream continuously then, water coolant is cooled to the one-level crystallizer from final stage jar and material adverse current simultaneously, crystallizers at different levels are controlled differing temps respectively by crystallization curve and are made the liquid glucose state that constantly reaches capacity, glucose molecule is separated out on nucleus, crystallization reaches balance fully, surveys and can realize continuous blowing after mother liquid concentration reaches requirement;
3) separate, magma is separated mother liquor by separating machine;
4) drying, the wet sugar of finished product generates crystalline dextrose through airflow drying and cooling back.
Advantage of the present invention is:
1, resin has good selective adsorption to pigment, and pigment dissociates easily, and washing gets final product;
2, resin to the absorption of sugar seldom contains sugar below 8% in the elutriant;
3, the physical strength of resin is big, can be than big flow charging;
4, the graininess resin has certain clearance each other in resin column, so saccharification liquid can reduce resistance during by resin;
When 5, liquid glucose is by resin decolorization, can also play the ionic effect of taking off (being desalination), the electricity of saccharification liquid is led, and (ash content of finished product) reduces;
6, resin can reach the purpose of using repeatedly by regeneration, saves cost;
7, the resin expiration date long, the phase of abandoning that resin is general is (to be determined on a case-by-case basis) more than 1 year.
8, spent ion exchange resin is decoloured to saccharification liquid, decolorizing effect is better than the effect with activated carbon treatment slightly, and per ton cost can reduce about 8 yuan; In addition, use resin that liquid glucose is carried out exquisiteness after activated carbon decolorizing, the purity of glucose and quality will improve greatly.
Embodiment
The invention will be further described below in conjunction with embodiment.
Embodiment 1:
Employing ion-exchange resin decolorization glucose saccharifying liquid technology of the present invention is as follows:
1. size mixing, in material-compound tank starch milk is transferred to 16Be, add a certain amount of high temperature resistant α-Dian Fenmei, Jet liquefier is squeezed into pump in the back that stirs;
2. liquefaction, powder slurry and steam meet in Jet liquefier, and drop temperature is controlled at 95 ℃, and the feed liquid of coming out from injector enters the laminar flow jar after cooling, carry out second spraying.This sprays feed liquid and steam directly mixes, and temperature rises to more than 110 ℃, and with the thorough deactivation of α-Dian Fenmei, then, feed liquid is cooled to 80 ℃ of insulations through the vacuum cooling system.Under the qualified situation of iodine examination, cool to 40 ℃, simultaneously the liquid glucose pH value is transferred between 3.5;
3. saccharification adds saccharifying enzyme, keeps saccharification about 45-60 hour, reach the saccharification terminal point after, rise to 70 ℃ with injector and reach the enzyme purpose of going out;
4. filter, the pH value of liquid glucose is transferred to 4.0 temperature be controlled between 60 ℃, remove by filter albumen through precoating formula vacuum-type drum filter.
5. resin decolorization, at 40 ℃, concentration is 35% with the liquid glucose after filtering, flow velocity be 2.5BV/h down successively by polyphone positively charged ion and anion-exchange resin column, decolour, and the transmittance, the electricity that regularly detect effluent liquid are led;
6. evaporation concentration, the liquid glucose after the decolouring is concentrated to 60% with the multiple-effect falling film vaporizer under vacuum tightness 0.5mpa and 60 ℃ of conditions;
7. crystallization, with pump input multistage crystallization jar, in the one-level crystallizer, stirred about 2 hours, crystallization is after 5 hours under 40 ℃ of temperature, inject secondary jar, three grades of jars, level Four jar etc. in order successively, quicken blowing with uniform flow stream continuously then, water coolant is cooled to the one-level crystallizer from final stage jar and material adverse current simultaneously, crystallizers at different levels are controlled differing temps respectively by crystallization curve and are made the liquid glucose state that constantly reaches capacity, glucose molecule is separated out on nucleus, crystallization reaches balance fully, surveys and can realize continuous blowing after mother liquid concentration reaches requirement;
8. separate, magma is separated mother liquor by separating machine;
9. dry, the wet sugar of finished product generates crystalline dextrose through airflow drying and cooling back.
In the present embodiment, the resin Intake Quantity is the 70-90% (resin calculates after expanding) of column volume, and yin and yang resin is just being washed backwash then earlier, again with pre-treatment such as soda acids, then saccharification liquid is decoloured.Water content: 50-60%, wet volume density: 0.65-0.75g/ml, wet true density: 1.03-1.07g/ml, granularity: 〉=95 (0.315-1.250) %, mill back rate of small round spheres: 〉=97% (exquisiteness reaches more than 95% with resin).Decolouring back liquid glucose can reach transmittance 〉=98%, and electricity is led≤10 μ s/cm.
Embodiment 2:
Employing ion-exchange resin decolorization glucose saccharifying liquid technology of the present invention is as follows:
1. size mixing, in material-compound tank starch milk is transferred to 20Be, add a certain amount of high temperature resistant α-Dian Fenmei, Jet liquefier is squeezed into pump in the back that stirs;
2. liquefaction, powder slurry and steam meet in Jet liquefier, and drop temperature is controlled at 110 ℃, and the feed liquid of coming out from injector enters the laminar flow jar after cooling, carry out second spraying.This sprays feed liquid and steam directly mixes, and temperature rises to more than 110 ℃, and with the thorough deactivation of α-Dian Fenmei, then, feed liquid is cooled to 100 ℃ of insulations through the vacuum cooling system.Under the qualified situation of iodine examination, cool to 65 ℃, simultaneously the liquid glucose pH value is transferred between 6.5;
3. saccharification adds saccharifying enzyme, keeps saccharification about 45-60 hour, reach the saccharification terminal point after, rise to 90 ℃ with injector and reach the enzyme purpose of going out;
4. filter, the pH value of liquid glucose is transferred to 5.5 temperature be controlled between 80 ℃, remove by filter albumen through precoating formula vacuum-type drum filter.
5. resin decolorization, at 50 ℃, concentration is 45% with the liquid glucose after filtering, flow velocity be 4.0BV/h down successively by polyphone positively charged ion and anion-exchange resin column, decolour, and the transmittance, the electricity that regularly detect effluent liquid are led;
6. evaporation concentration, the liquid glucose after the decolouring is concentrated to 80% with the multiple-effect falling film vaporizer under vacuum tightness 1.1mpa and 90 ℃ of conditions of temperature;
7. crystallization, with pump input multistage crystallization jar, in the one-level crystallizer, stirred about 2 hours, 50 ℃ of following crystallizations of temperature are after 12 hours, inject secondary jar, three grades of jars, level Four jar etc. in order successively, quicken blowing with uniform flow stream continuously then, water coolant is cooled to the one-level crystallizer from final stage jar and material adverse current simultaneously, crystallizers at different levels are controlled differing temps respectively by crystallization curve and are made the liquid glucose state that constantly reaches capacity, glucose molecule is separated out on nucleus, crystallization reaches balance fully, surveys and can realize continuous blowing after mother liquid concentration reaches requirement;
8. separate, magma is separated mother liquor by separating machine;
9. dry, the wet sugar of finished product generates crystalline dextrose through airflow drying and cooling back.
In the present embodiment, the resin Intake Quantity is the 70-90% (resin calculates after expanding) of column volume, and yin and yang resin is just being washed backwash then earlier, again with pre-treatment such as soda acids, then saccharification liquid is decoloured.Water content: 50-60%, wet volume density: 0.65-0.75g/ml, wet true density: 1.03-1.07g/ml, granularity: 〉=95 (0.315-1.250) %, mill back rate of small round spheres: 〉=97% (exquisiteness reaches more than 95% with resin).Decolouring back liquid glucose can reach transmittance 〉=98%, and electricity is led≤10 μ s/cm.
Embodiment 3:
Employing ion-exchange resin decolorization glucose saccharifying liquid technology of the present invention is as follows:
1. size mixing, in material-compound tank starch milk is transferred to 18Be, add a certain amount of high temperature resistant α-Dian Fenmei, Jet liquefier is squeezed into pump in the back that stirs;
2. liquefaction, powder slurry and steam meet in Jet liquefier, and drop temperature is controlled at 107 ℃, and the feed liquid of coming out from injector enters the laminar flow jar after cooling, carry out second spraying.This sprays feed liquid and steam directly mixes, and temperature rises to more than 110 ℃, and with the thorough deactivation of α-Dian Fenmei, then, feed liquid is cooled to 90 ℃ of insulations through the vacuum cooling system.Under the qualified situation of iodine examination, cool to 60 ℃, simultaneously the liquid glucose pH value is transferred between 4.5;
3. saccharification adds saccharifying enzyme, keeps saccharification about 45-60 hour, reach the saccharification terminal point after, rise to 80 ℃ with injector and reach the enzyme purpose of going out;
4. filter, the pH value of liquid glucose is transferred to 5.0 temperature be controlled between 70 ℃, remove by filter albumen through precoating formula vacuum-type drum filter.
5. glucose saccharifying liquid carries out activated carbon decolorizing earlier before entering ion exchange unit, promptly uses the gac with respect to saccharification liquid butt amount 0.5% to carry out the decolorizing resin decolouring earlier.
6. the liquid glucose after will filtering is 45 ℃ in temperature, and concentration is 40%, flow velocity be 3.5BV/h down successively by polyphone positively charged ion and anion-exchange resin column, decolour, and the transmittance, the electricity that regularly detect effluent liquid are led;
7. evaporation concentration, the liquid glucose after the decolouring is concentrated to 75% with the multiple-effect falling film vaporizer under vacuum tightness 0.9mpa and 90 ℃ of conditions;
8. crystallization, with pump input multistage crystallization jar, in the one-level crystallizer, stirred about 2 hours, 44 ℃ of following crystallizations of temperature are after 12 hours, inject secondary jar, three grades of jars, level Four jar etc. in order successively, quicken blowing with uniform flow stream continuously then, water coolant is cooled to the one-level crystallizer from final stage jar and material adverse current simultaneously, crystallizers at different levels are controlled differing temps respectively by crystallization curve and are made the liquid glucose state that constantly reaches capacity, glucose molecule is separated out on nucleus, crystallization reaches balance fully, surveys and can realize continuous blowing after mother liquid concentration reaches requirement;
9. separate, magma is separated mother liquor by separating machine;
10. dry, the wet sugar of finished product generates crystalline dextrose through airflow drying and cooling back.
In the present embodiment, the resin Intake Quantity is the 70-90% (resin calculates after expanding) of column volume, and yin and yang resin is just being washed backwash then earlier, again with pre-treatment such as soda acids, then saccharification liquid is decoloured.Water content: 50-60%, wet volume density: 0.65-0.75g/ml, wet true density: 1.03-1.07g/ml, granularity: 〉=95 (0.315-1.250) %, mill back rate of small round spheres: 〉=97% (exquisiteness reaches more than 95% with resin).Decolouring back liquid glucose can reach transmittance 〉=98%, and electricity is led≤10 μ s/cm.
Embodiment 4:
In the 5th step of present embodiment, use gac to carry out the decolorizing resin decolouring earlier with respect to saccharification liquid butt amount 1.5%.All the other steps are identical with embodiment 3, repeat no more.
Embodiment 5:
In the 5th step of present embodiment, use gac to carry out the decolorizing resin decolouring earlier with respect to saccharification liquid butt amount 1%.All the other steps are identical with embodiment 3, repeat no more.
Claims (3)
1. one kind is adopted ion exchange resin to the method that glucose saccharifying liquid decolours, and it is characterized in that: its technological process is,
A. glucose saccharifying liquid is handled, obtaining dry-matter is 35～45% glucose saccharifying liquids;
B. with the gained glucose saccharifying liquid 40 ℃～50 ℃ the time, send into ion exchange unit with the 2.5-4.OBV/h flow and decolour; Before glucose saccharifying liquid enters ion exchange unit, use gac to decolour earlier with respect to saccharification liquid butt amount 0.5-1.5%; Used ion-exchange unit is the positively charged ion and the anion-exchange resin column of serial connection, calculating after wherein the resin Intake Quantity expands by resin is the 70-90% of column volume, yin and yang resin is just being washed earlier backwash then, use acid-base pretreatment again, then saccharification liquid is decoloured, wherein the water content of resin: 50-60%, wet volume density: 0.65-0.75g/ml, wet true density: 1.03-1.07g/ml, granularity: 〉=95 (0.315-1.250) %, mill back rate of small round spheres: 〉=97%; Exquisiteness reaches more than 95% with resin;
C. make finished product at purifying or after making with extra care.
2. employing ion exchange resin according to claim 1 is characterized in that the method that glucose saccharifying liquid decolours: described step a comprises following technology
1) size mixing, in material-compound tank starch milk is transferred to 16-20Be, add a certain amount of high temperature resistant α-Dian Fenmei, Jet liquefier is squeezed into pump in the back that stirs;
2) liquefaction, powder slurry and steam meet in Jet liquefier, drop temperature is controlled at 95-110 ℃, and the feed liquid of coming out from injector enters the laminar flow jar after cooling, carry out second spraying, this sprays feed liquid and steam directly mixes, temperature rises to more than 110 ℃, and with the thorough deactivation of α-Dian Fenmei, feed liquid is cooled to 80-100 ℃ of insulation through the vacuum cooling system then, under the qualified situation of iodine examination, cool to 40-65 ℃, simultaneously the liquid glucose pH value is transferred between the 3.5-6.5;
3) saccharification adds saccharifying enzyme, keeps saccharification about 45-60 hour, reach the saccharification terminal point after, rise to 70-90 ℃ with injector and reach the enzyme purpose of going out;
4) filter, the pH value of liquid glucose is transferred to 4.0～5.5 temperature be controlled between 60-80 ℃, remove by filter albumen through precoating formula vacuum-type drum filter.
3. employing ion exchange resin according to claim 1 is characterized in that the method that glucose saccharifying liquid decolours: described step c comprises following technology,
1) evaporation concentration, the liquid glucose after the decolouring is to be concentrated to 60-80% under the 60-90 ℃ of condition with the multiple-effect falling film vaporizer in vacuum tightness 0.5-1.1mpa, temperature;
2) crystallization, with pump liquid glucose is imported the multistage crystallization jar, in the one-level crystallizer, stirred 2 hours, at 40-50 ℃ of following crystallization 5-12 hour, inject secondary jar, three grades of jars, level Four jar etc. in order successively, quicken blowing with uniform flow stream continuously then, water coolant is cooled to the one-level crystallizer from final stage jar and material adverse current simultaneously, crystallizers at different levels are controlled differing temps respectively by crystallization curve and are made the liquid glucose state that constantly reaches capacity, glucose molecule is separated out on nucleus, crystallization reaches balance fully, surveys and can realize continuous blowing after mother liquid concentration reaches requirement;
3) separate, magma is separated mother liquor by separating machine;
4) drying, the wet sugar of finished product generates crystalline dextrose through airflow drying and cooling back.
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| CN102586492B (en) * | 2011-12-31 | 2015-04-22 | 三达膜科技（厦门）有限公司 | Method for removing impurities from saccharification solution in glucose production process |
| GB201215261D0 (en) * | 2012-08-28 | 2012-10-10 | Tongaat Hulett Ltd | Process for refining impoure crystallised sucrose |
| CN102994653A (en) * | 2012-12-10 | 2013-03-27 | 浙江海洋学院普陀科学技术学院 | Saccharification liquid decoloring method |
| CN104017910A (en) * | 2014-06-30 | 2014-09-03 | 赖禄波 | Sucrose decolorization method |
| CN106755613B (en) * | 2016-12-16 | 2020-05-19 | 广州双桥股份有限公司 | Purification method of starch sugar |
| CN108251569A (en) * | 2018-01-23 | 2018-07-06 | 山东兆光色谱分离技术有限公司 | A kind of DEXTROSE ANHYDROUS preparation process |
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| CN1220780C (en) * | 2002-04-27 | 2005-09-28 | 山东西王集团有限公司 | Crystallization process for glucose production |
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| CN1220780C (en) * | 2002-04-27 | 2005-09-28 | 山东西王集团有限公司 | Crystallization process for glucose production |
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| 酶法制取葡萄糖的工艺技术. 李成涛等.食品研究与开发，第26卷第1期. 2005 |
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Assignee: Shandong Xiwang Biochemical Technology Co., Ltd. Assignor: Shandong Xiwang Sugar Co., Ltd. Contract fulfillment period: 2007.6.1 to 2017.6.1 Contract record no.: 2010370000032 Denomination of invention: Method of decolouring glucose saccharifying liquid by ion exchange resin Granted publication date: 20090701 License type: Exclusive license Record date: 2010.1.18 |
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