CN109136413A - A method of high purity glucose is prepared using cornstarch - Google Patents
A method of high purity glucose is prepared using cornstarch Download PDFInfo
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- CN109136413A CN109136413A CN201710464119.8A CN201710464119A CN109136413A CN 109136413 A CN109136413 A CN 109136413A CN 201710464119 A CN201710464119 A CN 201710464119A CN 109136413 A CN109136413 A CN 109136413A
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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
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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
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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
- C13K1/10—Crystallisation
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- Treatment Of Liquids With Adsorbents In General (AREA)
Abstract
The invention belongs to sugars from purification art, disclose a kind of method using cornstarch preparation high purity glucose comprising following steps: step 1) prepares liquefier, step 2 prepares saccharified liquid, step 3) micro-filtration, the processing of step 4) adsorbent, step 5) nanofiltration, step 6) condensing crystallizing.Glucose purity prepared by the present invention and high income, indices meet national standard.
Description
Technical field
The invention belongs to sugars from purification art, and in particular to a kind of separation purifying technique of glucose.
Background technique
Glucose is a kind of polyhydroxy aldehyde, is to be distributed a kind of monosaccharide the most extensive and important in the world.Pure grape
Sugar is colourless or white crystal, high not as good as sweetness of cane sugar, it is soluble easily in water in.Glucose has extremely important in field of biology
Status, the metabolic intermediate of living cells can all generate glucose, and biology mainly obtains energy by the metabolism of glucose.This
Outside, in food service industry, biochemical, papermaking, weaving and field of medicaments, glucose suffers from extensive use.Children are normal
The nutrient of growth and development is most important with sugar, protein and fatty three big elements.Carbohydrate (carbohydrate) is in supplying
The main source of heat.Glucose is a kind of monosaccharide, into can be used directly in vivo.1~6 month baby, in food
Carbohydrate is mainly lactose and a little starch.Starch-containing food gradually increases after 4 months, and pipe intestinal digesting starch is each when by 1 years old
Kind enzyme system is gradually perfect, can be hydrolyzed to glucose rapidly, and be absorbed into blood in small intestine.It can be directly fed after absorption
Energy, or stored in the form of glycogen, it is excessive to become fat.Injection, tablet and the grape of known calcium gluconate
Saccharic acid zinc oral solution all has the function of important physiological function, treatment.
Cornstarch is the important source material for extracting glucose, and corn starch molecules are connected by thousands of a glucose units
It connects, and hydrolytic process is that the starch molecule in starch milk is hydrolyzed into single glucose molecule.If hydrolytic process is done
Bad, not only subsequent handling filtration difficulty, or even crystallization and centrifuge separation can be allowed to become non-due to the presence of macromolecular amylin
It is often difficult even to crystallize, finally it is unable to get the glucose of purity is high.Currently, the industrialized production of glucose is to form sediment
Powder is raw material, is prepared using two enzymes method, and starch is by liquefaction, saccharification, active carbon decoloring, ion exchange, vacuum concentration, knot
The processes such as brilliant, centrifugation, dry.The above-mentioned a large amount of resin of process requirement, the waste water that resin regeneration generates is more, and invests and account for
The defects such as ground is big, and needs a large amount of operator, and process recovery ratio low there are working efficiency is low.
Summary of the invention
In order to overcome the shortcomings of the prior art, the present invention provides a kind of separation purifying techniques of glucose.
To achieve the goals above, the present invention is achieved by the following technical solution:
A method of high purity glucose is prepared using cornstarch comprising following steps: step 1) prepares liquefier, step
It is rapid 2) to prepare saccharified liquid, step 3) micro-filtration, the processing of step 4) adsorbent, step 5) nanofiltration, step 6) condensing crystallizing.
Further, the step 1) prepares liquefier, includes the following steps: to mix cornstarch and water, be configured to
Then the corn starch milk that Baume degrees is 20 adds fire resistant alpha-diastase according to the amount of every ml corn starch milk addition 10U, is adding
Enzyme is heated during adding, and is heated up to 105 DEG C and is maintained 1min；Then 130 DEG C are heated to rapidly to maintain 20 seconds, then are cooled down
To 90 DEG C, fire resistant alpha-diastase is added according to the amount of every ml corn starch milk addition 15U simultaneously during cooling, maintains 90 DEG C
Temperature 90min, obtain cornstarch liquefier.
Further, the step 2 prepares saccharified liquid, includes the following steps: cornstarch liquefier being transported to saccharification
In tank, while glucoamylase is added by the amount of every ml cornstarch liquefier addition 50U, and maintain temperature at 62 DEG C,
Under pH4.3 state, it is stirred to react 30h, finally obtains saccharified liquid.
Further, the step 3) micro-filtration includes the following steps: to stand saccharified liquid into 8h, collects upper liquid, then will
Upper liquid collects filtrate A through micro-filtrate membrane filtration；The microfiltration membranes are inorganic ceramic membrane, molecular cut off 3000Da, micro-filtration temperature
Degree is 35 DEG C.
Further, the step 4) adsorbent processing includes the following steps: that addition accounts for filtrate A 0.15% into filtrate A
(w/w) adsorbent, 300rpm stir 5min, are then allowed to stand 90min, and 200 mesh net filtrations collect liquor B.
Further, the step 5) nanofiltration includes the following steps: liquor B passing through nanofiltration membrane, nanofiltration temperature 35
DEG C, interception 300Da collects liquor C.
Further, the step 6) condensing crystallizing includes the following steps: liquor C concentration and evaporation to three points of original volume
One of, into crystallizer, crystallization, centrifuge separation obtains crystal, by the dry obtained glucose finished product of crystal.
Further, the adsorbent is prepared according to following technique: by nano silicon oxide, glass fibre and go from
Sub- water is mixed according to the mass ratio of 7:2:20, and 300rpm stirs 5min, then adds the vinyl for accounting for 10% mass parts of nano silicon oxide
Triethoxysilane, is warming up to 60 DEG C, and ultrasonication 30min obtains mixed liquor；The ultrasonic frequency is 20KHz, function
Rate is 1000W；Mixed liquor is mixed with acrylic sphere according to the mass ratio of 1:2, is then added in pelletizer, is added and account for
The concentration of acrylic sphere quality 10% is the polyvinyl alcohol water solution of 7wt%, and the sphere that partial size is 500um is made；By sphere
It is placed in 80 DEG C of baking oven dry 60min, then puts into sintering furnace and is sintered, 700 DEG C of sintering temperature, 30min is kept the temperature, takes
Out, cooled to room temperature to get.
Compared with prior art, the advantages and positive effects of the present invention mainly include but is not limited to following side
Face:
The present invention saves the process of original enzyme deactivation, to reduce production cost, simultaneously by changing traditional hydrolysis process
The ratio DX value that glucose accounts for total reducing sugar is improved, the DX value of saccharified liquid reaches 96% or more；
Present invention employs multiple film filtration treatment and adsorption treatment, ion exchange is eliminated, investment and land occupation be all big
To reduce, system automation degree is high, and required operator is few, and work efficiency is high and process recovery ratio is high；
Adsorbent of the present invention can effectively adsorpting pigment, metal ion and protein component, any chemistry does not occur with liquid glucose
Reaction, does not influence physics or chemical property, and can reuse by calcination and regeneration, save entreprise cost；
In adsorbent preparation process of the present invention, when nano silicon oxide is through vinyltriethoxysilane coupling agent treatment, coupling agent
One end combined with nano silicon oxide with chemical bond, it is anti-that with acrylic sphere chemistry can occur for other end of amido functional group
It answers, enhances the combination of phase interface, improve compatibility, reduce interface void and defect, and increase specific surface area；
The present invention is prepared into large aperture granular absorption particle using pore creating material acrylic sphere, firm in structure, will not rupture, be easier to
It is removed from solution, ensure that noresidue in solution.
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 high purity glucose is prepared using cornstarch comprising following steps:
Step 1) prepares liquefier: cornstarch and water are mixed, the corn starch milk that Baume degrees is 20 is configured to, then according to
The amount of every ml corn starch milk addition 10U adds fire resistant alpha-diastase, and enzyme is heated in adding procedure, is heated up to 105 DEG C simultaneously
Maintain 1min；Then 130 DEG C are heated to rapidly to maintain 20 seconds, then is cooled to 90 DEG C, simultaneously according to every during cooling
The amount that ml corn starch milk adds 15U adds fire resistant alpha-diastase, maintains 90 DEG C of temperature 90min, obtains cornstarch liquefaction
Liquid；
Step 2 prepares saccharified liquid: cornstarch liquefier being transported in saccharifying tank, while pressing every ml cornstarch liquefier
Glucoamylase is added in the amount for adding 50U, and maintains temperature under 62 DEG C, pH4.3 state, is stirred to react 30h, finally obtains
Saccharified liquid；
Step 3) micro-filtration: standing 8h for saccharified liquid, collect upper liquid, and upper liquid is then collected filtrate A through micro-filtrate membrane filtration；
The microfiltration membranes are inorganic ceramic membrane, and molecular cut off 3000Da, micro-filtration temperature is 35 DEG C；
Step 4) adsorbent processing: into filtrate A addition account for filtrate A 0.15%(w/w) adsorbent, 300rpm stirring 5min,
It is then allowed to stand 90min, 200 mesh net filtrations collect liquor B；
Step 5) nanofiltration: by liquor B by nanofiltration membrane, nanofiltration temperature is 35 DEG C, interception 300Da, collects liquor C；
Step 6) condensing crystallizing: the one third of liquor C concentration and evaporation to original volume, into crystallizer, crystallization, centrifuge separation is obtained
Crystal is obtained, by the dry obtained glucose finished product of crystal.
The adsorbent is prepared according to following technique: by nano silicon oxide, glass fibre and deionized water according to
The mass ratio of 7:2:20 mixes, and 300rpm stirs 5min, then adds the vinyl triethoxyl for accounting for 10% mass parts of nano silicon oxide
Silane, is warming up to 60 DEG C, and ultrasonication 30min obtains mixed liquor；The ultrasonic frequency is 20KHz, and power is
1000W；Mixed liquor is mixed with acrylic sphere according to the mass ratio of 1:2, is then added in pelletizer, is added and account for poly- third
The concentration of alkene ball quality 10% is the polyvinyl alcohol water solution of 7wt%, and the sphere that partial size is 500um is made；Sphere is placed in
Dry 60min in 80 DEG C of baking oven, then put into sintering furnace and be sintered, 700 DEG C of sintering temperature, 30min is kept the temperature, is taken out,
Cooled to room temperature obtains adsorbent；Through detecting, the specific surface area of adsorbent can reach 500m2/ g or more.
Embodiment 2
Adsorbent after using is put into 50-60 DEG C of water and impregnates 30min, taken out, be placed in 400-500 DEG C of calcining 3min,
Adsorbate is removed, natural cooling can reuse, and realize the regeneration of adsorbent, adsorption effect does not have significant change.
Embodiment 3
The glucose performance test of present invention process preparation:
Test group: glucose prepared by embodiment 1；Control group: referring to " a kind of separation and Extraction glucose from starch saccharificating liquid
The adsorbent that embodiment 1 uses in method ", remaining step is the same as the embodiment of the present invention 1.Specifically it is shown in Table 1:
Table 1
| Index | Test group | Control group | National standard |
| Purity % | 99.5 | 98.9 | ------ |
| Yield % | 88.1 | 84.5 | ------ |
| Chloride % | Less than 0.003 | Less than 0.003 | Meet |
| 25 DEG C of specific rotation | 7.6 | 7.6 | Meet |
| Heavy metal % | Less than 0.00002 | Less than 0.00002 | Meet |
Conclusion: compared with the control group, yield of the present invention is higher, and indices meet national standard.
Embodiment 4
The performance test of adsorbent of the present invention:
Sample selection: the glucose solution of 50g/L, wherein the concentration of iron ion is 0.189g/L, protein concentration 1.86g/
L；The residual quantity % of glucose: glucose amount accounts for the weight ratio of the adsorbent before use in adsorbent.
Group: test group: adsorbent prepared by the embodiment of the present invention 1；Control group 1: referring to " one kind is from starch saccharificating liquid
Adsorbent in the method for separation and Extraction glucose "；Control group 2: active carbon；Control group 3: diatomite.
Operating process: 0.15%(w/w is added into sample) adsorbent, 300rpm stir 5min, be then allowed to stand 90min,
200 mesh net filtrations collect filtrate and adsorbent trapped substance.Concrete outcome is shown in Table 2:
Table 2
| Index | Test group | Control group 1 | Control group 2 | Control group 3 |
| Iron g/L | 0.002 | 0.013 | 0.033 | 0.046 |
| Albumen g/L | 0.003 | 0.012 | 0.16 | 0.13 |
| The residual quantity % of glucose | 0.13 | 3.08 | 7.26 | 5.34 |
Conclusion: compared with the control group, adsorbent of the present invention can be effectively removed protein impurities and metal ion, Portugal in adsorbent
Grape sugar residual quantity is low, and adsorbent can regenerate recycling, save entreprise cost.
In the description of this specification, reference term " one embodiment ", " some embodiments ", " example ", " specific example " or
The description of " some examples " etc. means that particular features, structures, materials, or characteristics described in conjunction with this embodiment or example include
In at least one embodiment of the present invention or example.In the present specification, schematic expression of the above terms necessarily needle
Pair be identical embodiment or example.Although the embodiments of the present invention has been shown and described above, it is to be understood that
Above-described embodiment is exemplary, and is not considered as limiting the invention, and those skilled in the art are of the invention
It can make changes, modifications, alterations, and variations to the above described embodiments in range.
Claims (8)
1. a kind of method using cornstarch preparation high purity glucose comprising following steps: step 1) prepares liquefier,
Step 2 prepares saccharified liquid, step 3) micro-filtration, the processing of step 4) adsorbent, step 5) nanofiltration, step 6) condensing crystallizing.
2. the method according to claim 1, wherein the step 1) prepares liquefier, include the following steps: by
Cornstarch and water mixing, are configured to the corn starch milk that Baume degrees is 20, then according to every ml corn starch milk addition 10U's
Amount addition fire resistant alpha-diastase, enzyme is heated in adding procedure, 105 DEG C is heated up to and maintains 1min；Then heating rises rapidly
Temperature maintains 20 seconds to 130 DEG C, then is cooled to 90 DEG C, simultaneously according to the amount of every ml corn starch milk addition 15U during cooling
Fire resistant alpha-diastase is added, 90 DEG C of temperature 90min is maintained, obtains cornstarch liquefier.
3. according to the method described in claim 2, it is characterized in that, the step 2 prepares saccharified liquid, include the following steps: by
Cornstarch liquefier is transported in saccharifying tank, while glucose is added by the amount of every ml cornstarch liquefier addition 50U and forms sediment
Powder enzyme, and maintain temperature under 62 DEG C, pH4.3 state, it is stirred to react 30h, finally obtains saccharified liquid.
4. according to the method described in claim 3, it is characterized in that, the step 3) micro-filtration, includes the following steps: saccharified liquid
8h is stood, upper liquid is collected, upper liquid is then collected into filtrate A through micro-filtrate membrane filtration；The microfiltration membranes are inorganic ceramic membrane,
Molecular cut off is 3000Da, and micro-filtration temperature is 35 DEG C.
5. according to the method described in claim 4, it is characterized in that, step 4) adsorbent processing, includes the following steps: past
In filtrate A addition account for filtrate A 0.15%(w/w) adsorbent, 300rpm stir 5min, be then allowed to stand 90min, 200 mesh screens
Liquor B is collected in filtering.
6. according to the method described in claim 5, it is characterized in that, the step 5) nanofiltration, includes the following steps: liquor B
By nanofiltration membrane, nanofiltration temperature is 35 DEG C, interception 300Da, collects liquor C.
7. according to the method described in claim 6, it is characterized in that, the step 6) condensing crystallizing, includes the following steps: filtrate
C concentration and evaporation is to the one third of original volume, and into crystallizer, crystallization, centrifuge separation obtains crystal, by the dry obtained Portugal of crystal
Grape sugar finished product.
8. according to method described in claim 5-7, which is characterized in that the adsorbent is prepared according to following technique: will
Nano silicon oxide, glass fibre and deionized water are mixed according to the mass ratio of 7:2:20, and 300rpm stirs 5min, then adds and account for
The vinyltriethoxysilane of 10% mass parts of nano silicon oxide, is warming up to 60 DEG C, and ultrasonication 30min obtains mixture
Liquid；The ultrasonic frequency is 20KHz, power 1000W；Mixed liquor is mixed with acrylic sphere according to the mass ratio of 1:2,
It is then added in pelletizer, adds the polyvinyl alcohol water solution for accounting for that the concentration of acrylic sphere quality 10% is 7wt%, grain is made
Diameter is the sphere of 500um；Sphere is placed in in 80 DEG C of baking oven dry 60min, then puts into sintering furnace and is sintered,
700 DEG C of sintering temperature, keep the temperature 30min, take out, cooled to room temperature to get.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
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| 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 |
| JP7454103B2 (en) | 2021-05-25 | 2024-03-21 | 浙江▲華▼康葯▲業▼股▲フン▼有限公司 | System and method for simultaneous production of erythritol and liquid sorbitol using corn starch |
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