CN106282422A - A kind of method of separation and Extraction glucose from starch saccharificating liquid - Google Patents

A kind of method of separation and Extraction glucose from starch saccharificating liquid Download PDF

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Publication number
CN106282422A
CN106282422A CN201610775617.XA CN201610775617A CN106282422A CN 106282422 A CN106282422 A CN 106282422A CN 201610775617 A CN201610775617 A CN 201610775617A CN 106282422 A CN106282422 A CN 106282422A
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liquid
mixed
filtrate
powder
glucose
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CN106282422B (en
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赵凤良
董力青
杜学忠
孙志宇
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Hulunbuir Northeast Fufeng Biotechnology Co Ltd
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    • C—CHEMISTRY; METALLURGY
    • C13—SUGAR INDUSTRY
    • C13K—SACCHARIDES OBTAINED FROM NATURAL SOURCES OR BY HYDROLYSIS OF NATURALLY OCCURRING DISACCHARIDES, OLIGOSACCHARIDES OR POLYSACCHARIDES
    • C13K1/00—Glucose; Glucose-containing syrups
    • C13K1/06—Glucose; Glucose-containing syrups obtained by saccharification of starch or raw materials containing starch
    • C13K1/08—Purifying
    • C—CHEMISTRY; METALLURGY
    • C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F3/00—Biological treatment of water, waste water, or sewage
    • C02F3/34—Biological treatment of water, waste water, or sewage characterised by the microorganisms used
    • C—CHEMISTRY; METALLURGY
    • C13—SUGAR INDUSTRY
    • C13K—SACCHARIDES OBTAINED FROM NATURAL SOURCES OR BY HYDROLYSIS OF NATURALLY OCCURRING DISACCHARIDES, OLIGOSACCHARIDES OR POLYSACCHARIDES
    • C13K1/00—Glucose; Glucose-containing syrups
    • C13K1/10—Crystallisation
    • C—CHEMISTRY; METALLURGY
    • C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F2103/00—Nature of the water, waste water, sewage or sludge to be treated
    • C02F2103/32—Nature of the water, waste water, sewage or sludge to be treated from the food or foodstuff industry, e.g. brewery waste waters
    • C—CHEMISTRY; METALLURGY
    • C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F2103/00—Nature of the water, waste water, sewage or sludge to be treated
    • C02F2103/34—Nature of the water, waste water, sewage or sludge to be treated from industrial activities not provided for in groups C02F2103/12 - C02F2103/32
    • C02F2103/343—Nature of the water, waste water, sewage or sludge to be treated from industrial activities not provided for in groups C02F2103/12 - C02F2103/32 from the pharmaceutical industry, e.g. containing antibiotics
    • C—CHEMISTRY; METALLURGY
    • C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F2209/00—Controlling or monitoring parameters in water treatment
    • C02F2209/08—Chemical Oxygen Demand [COD]; Biological Oxygen Demand [BOD]
    • C—CHEMISTRY; METALLURGY
    • C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F2209/00—Controlling or monitoring parameters in water treatment
    • C02F2209/14—NH3-N

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  • Chemical & Material Sciences (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Organic Chemistry (AREA)
  • Health & Medical Sciences (AREA)
  • Emergency Medicine (AREA)
  • General Health & Medical Sciences (AREA)
  • Biochemistry (AREA)
  • Microbiology (AREA)
  • Biodiversity & Conservation Biology (AREA)
  • Hydrology & Water Resources (AREA)
  • Engineering & Computer Science (AREA)
  • Environmental & Geological Engineering (AREA)
  • Water Supply & Treatment (AREA)
  • Crystallography & Structural Chemistry (AREA)
  • Pharmaceuticals Containing Other Organic And Inorganic Compounds (AREA)
  • Separation Of Suspended Particles By Flocculating Agents (AREA)

Abstract

The invention belongs to glucose processing technique field, disclose a kind of method of separation and Extraction glucose from starch saccharificating liquid, it comprises the steps: that step 1) prepares flocculating decoloring agent, step 2) filter, step 3) flocculation decoloration, step 4) nanofiltration, step 5) crystallizes, step 6) mother liquid disposal.The present invention uses flocculation purification desolventing technology and multi-filtering step, yield and purity high, invests and take up an area minimizing, and enterprise's input cost reduces.

Description

A kind of method of separation and Extraction glucose from starch saccharificating liquid
Technical field
The invention belongs to glucose processing technique field, be specifically related to a kind of separation and Extraction glucose from starch saccharificating liquid Method.
Background technology
Glucose (Glucose) (chemical formula C6H12O6) it is also called glucose, corn sugar, referred to as glucose.English Another name: Dextrose, Cornsugar, Grapesugar, Bloodsugar, is that distributed in nature is the widest and of paramount importance one Planting monosaccharide, it is a kind of polyhydroxy aldehyde.Pure glucose is clear crystal, pleasantly sweet but sweet taste not as sucrose (common people without Method tastes sweet taste), soluble in water, it is slightly soluble in ethanol, insoluble in ether.Aqueous solution optically-active to the right, therefore belongs to " dextrose ".Fructus Vitis viniferae Sugar has critical role in field of biology, is energy source and the metabolism intermediate product of living cells, and i.e. biological is main Energy supply material.Plant can produce glucose by photosynthesis.In candy making industry and field of medicaments extensive application.
Corn starch is the important source material extracting glucose, and corn starch molecules is by thousands of glucose units even Connecing and form, the technique extracting glucose from starch saccharificating liquid is then to extract the final step work of glucose from corn starch milk Skill, equally, this step process is also related to the quality of glucose finished product.In order to reduce the by-product of glucose, people are at glucose In processing technique step, proposing a various solution, relatively common technique is: the life of existing production glucose Production. art is as follows: with starch as raw material, by liquefying under the effect of enzyme re-liquefied after sizing mixing, the most again through saccharifying enzyme effect sugar Changing, eventually form the glucose syrup of about DX95%, the mode then using kieselguhr to filter enters sheet frame or rotary drum was carried out Filter, with remove residual starch and float, then use fixed-bed ion exchange technique, mainly by substantial amounts of negative and positive from Salinity in sub-exchange resin removing sugar liquid, finally obtains pharmaceutical grade glucose by the technique of recrystallization；But this technique waste water Yield is more, and invests and take up an area big and it needs to substantial amounts of operator, there is inefficiency and process recovery ratio is low etc. lacks Fall into.
Summary of the invention
For the defect overcoming prior art to exist, the present invention proposes a kind of side of separation and Extraction glucose from starch saccharificating liquid Method.
To achieve these goals, the present invention is achieved by the following technical solution:
A kind of method of separation and Extraction glucose from starch saccharificating liquid, it comprises the steps: that step 1) prepares flocculation decoloration Agent, step 2) filter, step 3) flocculation decoloration, step 4) nanofiltration, step 5) crystallizes, step 6) mother liquid disposal.
Specifically, described method comprises the steps:
Step 1) prepares flocculating decoloring agent: (1) takes chitosan, sodium humate and pectin according to the mass ratio of 10:2:1, mixing Stir, then add the sodium hydrate aqueous solution of 2M accounting for chitosan twice quality, the ultrasonic 10min of 30KHz, finally 500 turns/min stirs 3min, obtains modification of chitosan；(2) corn straw, meerschaum are pulverized respectively obtain corn stalk powder and Sepiolite powder, then by corn stalk powder, sepiolite powder and kieselguhr according to the quality of 3:2:1 than mixing and stirring, add Being added to account in the sodium hydroxide solution that concentration is 1M of 5 times of weight of kieselguhr, 200 turns/min stirs 120min, then filters, dry Dry, obtain mixed-powder；(3) by modification of chitosan and mixed-powder according to the quality of 3:2 than mixing and stirring, put into Comminutor, pelletize and get final product；
Step 2) filter: starch saccharificating liquid first passes through 1mm screen filtration, filters after 40 eye mesh screens, then through micro-filtrate membrane filtration, Collect filtrate A；
Step 3) flocculation decoloration: in filtrate A add account for filtrate A 0.3%(w/w) flocculating decoloring agent, 300 turns/min stir 5min, then stands 60min, and 100 eye mesh screens filter, and collect liquor B；
Step 4) nanofiltration: by liquor B by NF membrane, nanofiltration temperature is 35-40 DEG C, and interception is 200-300MW, collects filtrate C；
Step 5) crystallizes: 1/2nd of liquor C concentration and evaporation to original volume, enters crystallizer, crystallization, and centrifugation obtains crystalline substance Body and mother solution；
Step 6) mother liquid disposal: mother solution is drained into sedimentation tank, it is thus achieved that precipitum and supernatant, enters microorganism by supernatant anti- Ying Chi, adds microbial bacterial agent 10 grams by every cubic metre of supernatant every time, adds every day 1 time, adds continuously three days, finally stands Four days, liquid is discharged.
Described micro-filtration membrane is inorganic ceramic film, and molecular cut off is 3000MW, and microfiltration temperature is 30-40 DEG C.
Described microbial bacterial agent is prepared according to following technique: first by bacillus amyloliquefaciens be ATCC 23843, Rhodococcus fascians ATCC 15906 and Bacillus pumilus ATCC 27142 cultivates respectively to concentration 2 × 108Individual/gram bacterium solution, so After be mixed to get mixed bacteria liquid according to the volume ratio of 3:2:2, stand 3 hours, then by mixed bacteria liquid and kieselguhr according to the matter of 1:2 Amount, than mixing, is dried, to obtain final product.
Note, above-mentioned bacterial strains all can be bought from ATCC and other commercial channel and obtain.
Compared with prior art, advantages of the present invention and having the active effect that
The present invention uses flocculation purification desolventing technology, uses multi-filtering step, including microfiltration, nanofiltration etc., produces waste water few, throws Money and occupation of land are also greatly reduced, and cost of material consumptive material is less expensive, easily operate for technical staff and yield and purity height；This A kind of novel flocculation decolorising agent of bright offer, possesses large aperture structure, adsorption capacity and specific surface area and improves, it is possible to effectively inhale Attached protein, starch and organic molecule pigment etc., and low raw-material cost；Microorganism formulation of the present invention is specifically designed for carrying Take the mother liquor waste water of preparation process, by the various strains that can form dominant microflora, be configured to high-efficiency microorganism preparation, Reasonable 5, symbiosis is coordinated, the most not antagonism, and activity is high, and Biomass is big, and breeding is fast, can improve the process water yield and water quality treatment, reduces and runs Expense, promotes qualified discharge；The flocculating decoloring agent garbage that the present invention relates to and the precipitate being collected by filtration may be used on fertilizer In material preparation.
Detailed description of the invention
For the technical scheme making those skilled in the art be more fully understood that in the application, specifically real below in conjunction with the application Execute example, the present invention is more clearly and completely described, it is clear that described embodiment is only that the application part is real Execute example rather than whole embodiments.Based on the embodiment in the application, those of ordinary skill in the art are not making creation The every other embodiment obtained under property work premise, all should belong to the scope of protection of the invention.
Embodiment 1
A kind of method of separation and Extraction glucose from starch saccharificating liquid, it comprises the steps:
Preparing flocculating decoloring agent: (1) takes chitosan, sodium humate and pectin according to the mass ratio of 10:2:1, mix and blend is equal Even, then add the sodium hydrate aqueous solution of 2M accounting for chitosan twice quality, the ultrasonic 10min of 30KHz, last 500 turns/ Min stirs 3min, obtains modification of chitosan；(2) corn straw, meerschaum are pulverized respectively obtain corn stalk powder and meerschaum Powder, then corn stalk powder, sepiolite powder and kieselguhr according to the quality of 3:2:1 than mixing and stirring, add to and account for diatom In the sodium hydroxide solution that concentration is 1M of 5 times of weight of soil, 200 turns/min stirs 120min, then filters, and is dried, is mixed Close powder；(3) by modification of chitosan and mixed-powder according to the quality of 3:2 than mixing and stirring, put into comminutor, make Grain and get final product；Grain diameter controls at 300-600um；
Filter: utilizing corn starch enzyme process to prepare starch saccharificating liquid (pol is 12%), starch saccharificating liquid first passes through 1mm screen cloth mistake After filter, after 40 eye mesh screens, then through micro-filtrate membrane filtration, collect filtrate A；Described micro-filtration membrane is inorganic ceramic film, retains molecule Amount is 3000MW, and microfiltration temperature is 30-40 DEG C；
Flocculation decoloration: in filtrate A add account for filtrate A 0.3%(w/w) flocculating decoloring agent, 300 turns/min stirs 5min, so Rear standing 60min, 100 eye mesh screens filter, and collect liquor B；
Nanofiltration: by liquor B by NF membrane, nanofiltration temperature is 35-40 DEG C, and nanofiltration pressure is 15-20bar, and interception is 200- 300MW, collects liquor C；
Crystallization: 1/2nd of liquor C concentration and evaporation to original volume, enters crystallizer, crystallization, and centrifugation obtains crystal and mother Liquid；Crystal is dried prepared finished product；
Mother liquid disposal: mother solution is drained into sedimentation tank, is the kieselguhr of 50cm thickness bottom sedimentation tank, and natural subsidence solid-liquid divides From, it is thus achieved that precipitum and supernatant, supernatant is entered microbial reaction pond, adds microorganism by every cubic metre of supernatant every time Microbial inoculum 10 grams, adds 1 every day, adds continuously three days, finally stands four days, is discharged by liquid.After testing: mother solution before process Middle COD, the concentration of ammonia nitrogen are respectively 1967mg/L and 179 mg/L, and after process, in liquid, COD, the concentration of ammonia nitrogen are respectively 103mg/L and 12 mg/L, clearance reaches more than 90%.
Described microbial bacterial agent is prepared according to following technique:
First by bacillus amyloliquefaciens be ATCC 23843, Rhodococcus fascians ATCC 15906 and Bacillus pumilus ATCC 27142 cultivate respectively to concentration 2 × 108Individual/gram bacterium solution, then according to the volume ratio of 3:2:2 is mixed to get mixed bacteria liquid, quiet Putting 3 hours, then mixed bacteria liquid and kieselguhr are mixed according to the mass ratio of 1:2, be dried, holding moisture is 20- 30wt%, packaging, to obtain final product.
Embodiment 2
The glucose parametric measurement of embodiment 1 preparation, is specifically shown in Table 1:
Table 1
Index Embodiment 1 National standard
Purity % 99.7 ------
Yield % 83.2 ------
Acidity ml 0.09 Meet
Chloride % Less than 0.003 Meet
Specific optical rotation 25 DEG C 7.6 Meet
Heavy metal % Less than 0.00002 Meet
Conclusion: product purity and yield prepared by separation and Extraction of the present invention are good, energy-saving and emission-reduction are environment friendly and pollution-free, its product prepared Product meet state-promulgated pharmacopoeia standard.
Listed above is only the optimal specific embodiment of the present invention.It is clear that the invention is not restricted to above example, it is also possible to have Many deformation.All deformation that those of ordinary skill in the art can directly derive from present disclosure or associate, All it is considered as protection scope of the present invention.

Claims (4)

1. a method for separation and Extraction glucose from starch saccharificating liquid, it comprises the steps: that step 1) preparation flocculation is de- Toner, step 2) filter, step 3) flocculation decoloration, step 4) nanofiltration, step 5) crystallizes, step 6) mother liquid disposal.
Method the most according to claim 1, it is characterised in that described method comprises the steps:
Step 1) prepares flocculating decoloring agent: (1) takes chitosan, sodium humate and pectin according to the mass ratio of 10:2:1, mixing Stir, then add the sodium hydrate aqueous solution of 2M accounting for chitosan twice quality, the ultrasonic 10min of 30KHz, finally 500 turns/min stirs 3min, obtains modification of chitosan；(2) corn straw, meerschaum are pulverized respectively obtain corn stalk powder and Sepiolite powder, then by corn stalk powder, sepiolite powder and kieselguhr according to the quality of 3:2:1 than mixing and stirring, add Being added to account in the sodium hydroxide solution that concentration is 1M of 5 times of weight of kieselguhr, 200 turns/min stirs 120min, then filters, dry Dry, obtain mixed-powder；3) by modification of chitosan and mixed-powder according to the quality of 3:2 than mixing and stirring, put into Comminutor, pelletize and get final product；
Step 2) filter: starch saccharificating liquid first passes through 1mm screen filtration, filters after 40 eye mesh screens, then through micro-filtrate membrane filtration, Collect filtrate A；
Step 3) flocculation decoloration: in filtrate A add account for filtrate A 0.3%(w/w) flocculating decoloring agent, 300 turns/min stir 5min, then stands 60min, and 100 eye mesh screens filter, and collect liquor B；
Step 4) nanofiltration: by liquor B by NF membrane, nanofiltration temperature is 35-40 DEG C, and interception is 200-300MW, collects filtrate C；
Step 5) crystallizes: 1/2nd of liquor C concentration and evaporation to original volume, enters crystallizer, crystallization, and centrifugation obtains crystalline substance Body and mother solution；
Step 6) mother liquid disposal: mother solution is drained into sedimentation tank, it is thus achieved that precipitum and supernatant, enters microorganism by supernatant anti- Ying Chi, adds microbial bacterial agent 10 grams by every cubic metre of supernatant every time, adds every day 1 time, adds continuously three days, finally stands Four days, liquid is discharged.
Method the most according to claim 2, it is characterised in that described micro-filtration membrane is inorganic ceramic film, molecular cut off is 3000MW, microfiltration temperature is 30-40 DEG C.
Method the most according to claim 2, it is characterised in that described microbial bacterial agent is prepared according to following technique: First by bacillus amyloliquefaciens be ATCC 23843, Rhodococcus fascians ATCC 15906 and Bacillus pumilus ATCC 27142 Cultivate respectively to concentration 2 × 108Individual/gram bacterium solution, then according to the volume ratio of 3:2:2 is mixed to get mixed bacteria liquid, stand 3 little Time, then mixed bacteria liquid and kieselguhr are mixed according to the mass ratio of 1:2, it is dried, to obtain final product.
CN201610775617.XA 2016-08-31 2016-08-31 A method of the separation and Extraction glucose from starch saccharificating liquid Active CN106282422B (en)

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Cited By (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN108004190A (en) * 2018-01-19 2018-05-08 何红娣 Bacillus is used for the method for increasing bead algae biomass
CN109136305A (en) * 2017-06-19 2019-01-04 卢松 A kind of separation purifying technique of glucose
CN109136413A (en) * 2017-06-19 2019-01-04 卢松 A method of high purity glucose is prepared using cornstarch
CN110846359A (en) * 2019-09-12 2020-02-28 赵兰坤 Production method of edible glucose
CN112322679A (en) * 2020-11-06 2021-02-05 齐齐哈尔龙江阜丰生物科技有限公司 Novel saccharification process without cooling pipe
CN112409423A (en) * 2020-11-02 2021-02-26 呼伦贝尔东北阜丰生物科技有限公司 Process for improving quality of glucose

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CN1675368A (en) * 2002-08-05 2005-09-28 西巴特殊化学水处理有限公司 Use of flocculating agents for separating the solid residue in hydrolysed fermentationsubstrates
CN105132593A (en) * 2015-09-18 2015-12-09 山东创利添加剂研发科技有限公司 Method for preparing crystalline fructose and crystal glucose from maize straw
CN105692823A (en) * 2016-01-19 2016-06-22 赵东星 Environment-friendly efficient biological flocculant and preparing method thereof
CN105821095A (en) * 2015-09-14 2016-08-03 呼伦贝尔东北阜丰生物科技有限公司 Optimization method for crystallization of glucose

Patent Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1675368A (en) * 2002-08-05 2005-09-28 西巴特殊化学水处理有限公司 Use of flocculating agents for separating the solid residue in hydrolysed fermentationsubstrates
CN105821095A (en) * 2015-09-14 2016-08-03 呼伦贝尔东北阜丰生物科技有限公司 Optimization method for crystallization of glucose
CN105132593A (en) * 2015-09-18 2015-12-09 山东创利添加剂研发科技有限公司 Method for preparing crystalline fructose and crystal glucose from maize straw
CN105692823A (en) * 2016-01-19 2016-06-22 赵东星 Environment-friendly efficient biological flocculant and preparing method thereof

Cited By (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN109136305A (en) * 2017-06-19 2019-01-04 卢松 A kind of separation purifying technique of glucose
CN109136413A (en) * 2017-06-19 2019-01-04 卢松 A method of high purity glucose is prepared using cornstarch
CN108004190A (en) * 2018-01-19 2018-05-08 何红娣 Bacillus is used for the method for increasing bead algae biomass
CN108004190B (en) * 2018-01-19 2019-12-06 杭州渔森农业技术开发有限公司 Method for increasing chlorella biomass by using bacillus
CN110846359A (en) * 2019-09-12 2020-02-28 赵兰坤 Production method of edible glucose
CN112409423A (en) * 2020-11-02 2021-02-26 呼伦贝尔东北阜丰生物科技有限公司 Process for improving quality of glucose
CN112322679A (en) * 2020-11-06 2021-02-05 齐齐哈尔龙江阜丰生物科技有限公司 Novel saccharification process without cooling pipe

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