CN106282422B - A method of the separation and Extraction glucose from starch saccharificating liquid - Google Patents

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

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CN106282422B
CN106282422B CN201610775617.XA CN201610775617A CN106282422B CN 106282422 B CN106282422 B CN 106282422B CN 201610775617 A CN201610775617 A CN 201610775617A CN 106282422 B CN106282422 B CN 106282422B
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mixed
filtrate
powder
glucose
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CN106282422A (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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    • CCHEMISTRY; METALLURGY
    • C13SUGAR INDUSTRY
    • C13KSACCHARIDES OBTAINED FROM NATURAL SOURCES OR BY HYDROLYSIS OF NATURALLY OCCURRING DISACCHARIDES, OLIGOSACCHARIDES OR POLYSACCHARIDES
    • C13K1/00Glucose; Glucose-containing syrups
    • C13K1/06Glucose; Glucose-containing syrups obtained by saccharification of starch or raw materials containing starch
    • C13K1/08Purifying
    • CCHEMISTRY; METALLURGY
    • C02TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02FTREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F3/00Biological treatment of water, waste water, or sewage
    • C02F3/34Biological treatment of water, waste water, or sewage characterised by the microorganisms used
    • CCHEMISTRY; METALLURGY
    • C13SUGAR INDUSTRY
    • C13KSACCHARIDES OBTAINED FROM NATURAL SOURCES OR BY HYDROLYSIS OF NATURALLY OCCURRING DISACCHARIDES, OLIGOSACCHARIDES OR POLYSACCHARIDES
    • C13K1/00Glucose; Glucose-containing syrups
    • C13K1/10Crystallisation
    • CCHEMISTRY; METALLURGY
    • C02TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02FTREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F2103/00Nature of the water, waste water, sewage or sludge to be treated
    • C02F2103/32Nature of the water, waste water, sewage or sludge to be treated from the food or foodstuff industry, e.g. brewery waste waters
    • CCHEMISTRY; METALLURGY
    • C02TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02FTREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F2103/00Nature of the water, waste water, sewage or sludge to be treated
    • C02F2103/34Nature of the water, waste water, sewage or sludge to be treated from industrial activities not provided for in groups C02F2103/12 - C02F2103/32
    • C02F2103/343Nature 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
    • CCHEMISTRY; METALLURGY
    • C02TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02FTREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F2209/00Controlling or monitoring parameters in water treatment
    • C02F2209/08Chemical Oxygen Demand [COD]; Biological Oxygen Demand [BOD]
    • CCHEMISTRY; METALLURGY
    • C02TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02FTREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F2209/00Controlling or monitoring parameters in water treatment
    • C02F2209/14NH3-N

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

Abstract

The invention belongs to glucose processing technology fields, disclose a kind of method of separation and Extraction glucose from starch saccharificating liquid comprising following steps: step 1) prepares flocculating decoloring agent, step 2 filtering, step 3) flocculation decoloration, step 4) nanofiltration, step 5) crystallization, step 6) mother liquid disposal.The present invention uses flocculation purification decolorization and multi-filtering step, yield and purity is high, and investment and land occupation are reduced, and enterprise's input cost reduces.

Description

A method of the separation and Extraction glucose from starch saccharificating liquid
Technical field
The invention belongs to glucose processing technology fields, and in particular to one kind separation and Extraction glucose from starch saccharificating liquid Method.
Background technique
Glucose (Glucose) (chemical formula C6H12O6) it is also known as corn sugar, corn sugar, referred to as glucose.English Another name: Dextrose, Cornsugar, Grapesugar, Bloodsugar, be distributed in nature it is most wide and mostly important one Kind monosaccharide, it is a kind of polyhydroxy aldehyde.Pure glucose be clear crystal, pleasantly sweet but sweet taste not as good as sucrose (common people without Method tastes sweet taste), it is soluble easily in water, it is slightly soluble in ethyl alcohol, does not dissolve in ether.Aqueous solution optically-active to the right, therefore belongs to " dextrose ".Grape Sugar has critical role in field of biology, is energy source and the metabolism intermediate product of living cells, i.e., biological is main Energy supply material.Plant can generate glucose by photosynthesis.In candy making industry and field of medicaments extensive application.
Cornstarch is the important source material for extracting glucose, and corn starch molecules are connected by thousands of a glucose units It connects, the technique that glucose is extracted from starch saccharificating liquid is then that the final step work of glucose is extracted from corn starch milk Skill, equally, this step process are also related to the quality of glucose finished product.In order to reduce the by-product of glucose, people are in glucose In processing technology step, a various solutions, relatively common technique are proposed are as follows: the life of existing production glucose Production. art is as follows: being made from starch, by liquefying under the action of enzyme re-liquefied after sizing mixing, then again through saccharification enzyme effect sugar Change, eventually form the glucose syrup of DX95% or so, then enters sheet frame by the way of diatomite filtering or rotary drum carried out Filter, to remove remaining starch and suspended matter, then use fixed bed ion-exchange process, mainly using a large amount of yin-yang from Sub-exchange resin removes the salinity in liquid glucose, finally obtains pharmaceutical grade glucose with the technique of recrystallization;But the technique waste water Yield is more, and invests and land occupation is big, and needs a large amount of operator, and it is equal scarce that and process recovery ratio low there are working efficiency is low It falls into.
Summary of the invention
In order to overcome the shortcomings of the prior art, the present invention proposes one kind separation and Extraction glucose from starch saccharificating liquid Method.
To achieve the goals above, the present invention is achieved by the following technical solution:
A method of the separation and Extraction glucose from starch saccharificating liquid comprising following steps: step 1) preparation flocculation Decolorising agent, step 2 filtering, step 3) flocculation decoloration, step 4) nanofiltration, step 5) crystallization, step 6) mother liquid disposal.
Specifically, described method includes following steps:
Step 1) prepares flocculating decoloring agent: (1) according to the mass ratio of 10:2:1 take chitosan, sodium humate and pectin, Be mixed evenly, then addition account for twice of mass of chitosan 2M sodium hydrate aqueous solution, the ultrasonic 10min of 30KHz, most 500 turns/min stirs 3min afterwards, obtains modification of chitosan;(2) corn stover, sepiolite are crushed respectively and obtains corn stalk powder And sepiolite powder, then corn stalk powder, sepiolite powder and diatomite are mixed evenly according to the mass ratio of 3:2:1, It is added to the concentration for accounting for 5 times of weight of diatomite as in the sodium hydroxide solution of 1M, 200 turns/min stirs 120min, then filters, It is dry, obtain mixed-powder;(3) modification of chitosan and mixed-powder are mixed evenly according to the mass ratio of 3:2, are put into To pelletizer, it is granulated to obtain the final product;
Step 2 filtering: starch saccharificating liquid first passes through 1mm the screen to filtrate, after 40 mesh net filtrations, then through microfiltration membranes Filtrate A is collected in filtering;
Step 3) flocculation decoloration: into filtrate A, addition accounts for filtrate A 0.3%(w/w) flocculating decoloring agent, 300 turns/min stirs 5min is mixed, 60min is then allowed to stand, 100 mesh net filtrations collect liquor B;
Step 4) nanofiltration: by liquor B by nanofiltration membrane, nanofiltration temperature is 35-40 DEG C, interception 200-300MW, is collected Liquor C;
Step 5) crystallization: the half of liquor C concentration and evaporation to original volume, into crystallizer, crystallization, centrifuge separation is obtained Obtain crystal and mother liquor;
Step 6) mother liquid disposal: mother liquor is drained into sedimentation basin, sediment and supernatant is obtained, supernatant is discharged into micro- life Object reaction tank adds 10 grams of microbial bacterial agent by every cubic metre of supernatant every time, adds daily 1 time, continuously adds three days, finally Four days are stood, liquid is discharged.
The microfiltration membranes are inorganic ceramic membrane, and molecular cut off 3000MW, micro-filtration temperature is 30-40 DEG C.
The microbial bacterial agent is prepared according to following technique: be first ATCC 23843 by bacillus amyloliquefaciens, Rhodococcus sp ATCC 15906 and bacillus pumilus ATCC 27142 is cultivated respectively to concentration 2 × 108It is a/gram bacterium solution, so Mixed bacteria liquid is mixed to get according to the volume ratio of 3:2:2 afterwards, stands 3 hours, then by mixed bacteria liquid and diatomite according to the matter of 1:2 Amount than mixing, it is dry to get.
Note, above-mentioned bacterial strains can be obtained from ATCC and the purchase of other commercial channel.
Compared with prior art, the advantages and positive effects of the present invention are:
The present invention uses flocculation purification decolorization, using multi-filtering step, including micro-filtration, nanofiltration etc., generates waste water Few, investment and land occupation are also greatly reduced, and cost of material consumptive material is less expensive, are easy as technical staff's operation and yield and purity It is high;The present invention provides a kind of novel flocculation decolorising agent, has macropore gauge structure, and adsorption capacity and specific surface area improve, can Effectively adsorbed proteins, starch and small organic molecule pigment etc., and low raw-material cost;Microorganism formulation of the present invention is special The various strains that can form dominant microflora are configured to high-efficiency microorganism preparation for the mother liquor waste water for extracting preparation process by door, Reasonable compatibility, symbiosis are coordinated, mutually not antagonism, and activity is high, and biomass is big, and breeding is fast, and processing water and water quality treatment, drop can be improved Low operating cost promotes qualified discharge;Flocculating decoloring agent waste of the present invention and the sediment being collected by filtration can answer It uses in fertilizer preparation.
Specific embodiment
In order to make those skilled in the art better understand the technical solutions in the application, having below in conjunction with the application Body embodiment more clearly and completely describes the present invention, it is clear that described embodiment is only the application one Divide embodiment, instead of all the embodiments.Based on the embodiment in the application, those of ordinary skill in the art are not making Every other embodiment obtained, should fall within the scope of the present invention under the premise of creative work.
Embodiment 1
A method of the separation and Extraction glucose from starch saccharificating liquid comprising following steps:
It prepares flocculating decoloring agent: (1) taking chitosan, sodium humate and pectin according to the mass ratio of 10:2:1, mixing is stirred Mix uniformly, then addition account for twice of mass of chitosan 2M sodium hydrate aqueous solution, the ultrasonic 10min of 30KHz, last 500 Turn/min stirring 3min, obtains modification of chitosan;(2) corn stover, sepiolite are crushed respectively and obtains corn stalk powder and sea Afrodite powder, then corn stalk powder, sepiolite powder and diatomite are mixed evenly according to the mass ratio of 3:2:1, are added to and account for The concentration of 5 times of weight of diatomite is in the sodium hydroxide solution of 1M, and 200 turns/min stirs 120min, is then filtered, dry, is obtained To mixed-powder;(3) modification of chitosan and mixed-powder are mixed evenly according to the mass ratio of 3:2, put into granulation Machine is granulated to obtain the final product;Grain diameter is controlled in 300-600um;
Filtering: being prepared starch saccharificating liquid (pol 12%) using cornstarch enzyme process, and starch saccharificating liquid first passes through 1mm sieve After net filtration, after 40 mesh screens, then through micro-filtrate membrane filtration, filtrate A is collected;The microfiltration membranes are inorganic ceramic membrane, retention Molecular weight is 3000MW, and micro-filtration temperature is 30-40 DEG C;
Flocculation decoloration: into filtrate A addition account for filtrate A 0.3%(w/w) flocculating decoloring agent, 300 turns/min stirring 5min, is then allowed to stand 60min, and 100 mesh net filtrations collect liquor B;
Nanofiltration: by liquor B by nanofiltration membrane, nanofiltration temperature is 35-40 DEG C, nanofiltration pressure 15-20bar, and interception is 200-300MW collects liquor C;
Crystallization: the half of liquor C concentration and evaporation to original volume, into crystallizer, crystallization, centrifuge separation obtains crystal And mother liquor;By the dry finished product of crystal;
Mother liquid disposal: mother liquor is drained into sedimentation basin, precipitating bottom of pond portion is the diatomite of 50cm thickness, natural subsidence solid-liquid Separation obtains sediment and supernatant, supernatant is discharged into microbial reaction pond, adds micro- life every time by every cubic metre of supernatant It 10 grams of object microbial inoculum, adds daily 1 time, continuously adds three days, finally stand four days, liquid is discharged.Through detecting: female before processing COD in liquid, ammonia nitrogen concentration be respectively 1967mg/L and 179 mg/L, COD in liquid after processing, ammonia nitrogen concentration be respectively 103mg/L and 12 mg/L, removal rate reach 90% or more.
The microbial bacterial agent is prepared according to following technique:
It is first ATCC 23843, Rhodococcus sp ATCC 15906 and bacillus pumilus by bacillus amyloliquefaciens ATCC 27142 is cultivated respectively to concentration 2 × 108It is a/gram bacterium solution, be then mixed to get Mixed Microbes according to the volume ratio of 3:2:2 Liquid stands 3 hours, then mixes mixed bacteria liquid and diatomite according to the mass ratio of 1:2, dry, holding moisture content is 20- 30wt%, packaging to get.
Embodiment 2
Glucose parametric measurement prepared by embodiment 1, 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
25 DEG C of specific rotation 7.6 Meet
Heavy metal % Less than 0.00002 Meet
Conclusion: the product purity and yield of separation and Extraction preparation of the present invention are good, and energy-saving and emission-reduction are environment friendly and pollution-free, preparation Product meet National Pharmacopeia standard.
Listed above is only best specific embodiment of the invention.It is clear that the invention is not restricted to which above embodiments, may be used also With there are many deformations.All changes that those skilled in the art directly can export or associate from present disclosure Shape is considered as protection scope of the present invention.

Claims (2)

1. a kind of method of the separation and Extraction glucose from starch saccharificating liquid, which is characterized in that described method includes following steps:
Step 1) prepares flocculating decoloring agent: (1) taking chitosan, sodium humate and pectin according to the mass ratio of 10:2:1, mix Stir evenly, then addition account for twice of mass of chitosan 2M sodium hydrate aqueous solution, the ultrasonic 10min of 30KHz, finally 500 turns/min stirs 3min, obtains modification of chitosan;(2) corn stover, sepiolite are crushed respectively obtain corn stalk powder and Then corn stalk powder, sepiolite powder and diatomite are mixed evenly according to the mass ratio of 3:2:1, add by sepiolite powder Being added to and accounting for the concentration of 5 times of weight of diatomite is in the sodium hydroxide solution of 1M, and 200 turns/min stirs 120min, then filters, and does It is dry, obtain mixed-powder;(3) modification of chitosan and mixed-powder are mixed evenly according to the mass ratio of 3:2, are put into Pelletizer is granulated to obtain the final product;
Step 2 filtering: starch saccharificating liquid first passes through 1mm the screen to filtrate, after 40 mesh net filtrations, then through micro-filtrate membrane filtration, Collect filtrate A;
Step 3) flocculation decoloration: into filtrate A, addition accounts for the flocculating decoloring agent of filtrate A 0.3%w/w, 300 turns/min stirring 5min, is then allowed to stand 60min, and 100 mesh net filtrations collect liquor B;
Step 4) nanofiltration: by liquor B by nanofiltration membrane, nanofiltration temperature is 35-40 DEG C, interception 200-300MW, collects filtrate C;
Step 5) crystallization: the half of liquor C concentration and evaporation to original volume, into crystallizer, crystallization, centrifuge separation obtains brilliant Body and mother liquor;
Step 6) mother liquid disposal: mother liquor is drained into sedimentation basin, sediment and supernatant is obtained, it is anti-that supernatant is discharged into microorganism Ying Chi adds 10 grams of microbial bacterial agent by every cubic metre of supernatant every time, adds daily 1 time, continuously adds three days, finally stand Four days, liquid is discharged;
The microbial bacterial agent is prepared according to following technique: being first ATCC 23843, red ball by bacillus amyloliquefaciens Bacterium ATCC 15906 and bacillus pumilus ATCC 27142 is cultivated respectively to concentration 2 × 108It is a/gram bacterium solution, then press Mixed bacteria liquid is mixed to get according to the volume ratio of 3:2:2, stands 3 hours, then by mixed bacteria liquid and diatomite according to the mass ratio of 1:2 Mixing, it is dry.
2. molecular cut off is the method according to claim 1, wherein the microfiltration membranes are inorganic ceramic membrane 3000MW, micro-filtration temperature are 30-40 DEG C.
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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
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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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

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