CN110982861A - Method for improving filtration speed of crystalline glucose saccharification liquid - Google Patents

Method for improving filtration speed of crystalline glucose saccharification liquid Download PDF

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CN110982861A
CN110982861A CN201911344643.7A CN201911344643A CN110982861A CN 110982861 A CN110982861 A CN 110982861A CN 201911344643 A CN201911344643 A CN 201911344643A CN 110982861 A CN110982861 A CN 110982861A
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liquid
starch
saccharification
enzyme
value
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赵玉斌
王新增
李法田
吴静
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Shandong Luzhou Food Group Co ltd
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    • CCHEMISTRY; METALLURGY
    • C12BIOCHEMISTRY; BEER; SPIRITS; WINE; VINEGAR; MICROBIOLOGY; ENZYMOLOGY; MUTATION OR GENETIC ENGINEERING
    • C12PFERMENTATION OR ENZYME-USING PROCESSES TO SYNTHESISE A DESIRED CHEMICAL COMPOUND OR COMPOSITION OR TO SEPARATE OPTICAL ISOMERS FROM A RACEMIC MIXTURE
    • C12P19/00Preparation of compounds containing saccharide radicals
    • C12P19/20Preparation of compounds containing saccharide radicals produced by the action of an exo-1,4 alpha-glucosidase, e.g. dextrose
    • CCHEMISTRY; METALLURGY
    • C12BIOCHEMISTRY; BEER; SPIRITS; WINE; VINEGAR; MICROBIOLOGY; ENZYMOLOGY; MUTATION OR GENETIC ENGINEERING
    • C12PFERMENTATION OR ENZYME-USING PROCESSES TO SYNTHESISE A DESIRED CHEMICAL COMPOUND OR COMPOSITION OR TO SEPARATE OPTICAL ISOMERS FROM A RACEMIC MIXTURE
    • C12P19/00Preparation of compounds containing saccharide radicals
    • C12P19/02Monosaccharides
    • CCHEMISTRY; METALLURGY
    • C12BIOCHEMISTRY; BEER; SPIRITS; WINE; VINEGAR; MICROBIOLOGY; ENZYMOLOGY; MUTATION OR GENETIC ENGINEERING
    • C12PFERMENTATION OR ENZYME-USING PROCESSES TO SYNTHESISE A DESIRED CHEMICAL COMPOUND OR COMPOSITION OR TO SEPARATE OPTICAL ISOMERS FROM A RACEMIC MIXTURE
    • C12P19/00Preparation of compounds containing saccharide radicals
    • C12P19/14Preparation of compounds containing saccharide radicals produced by the action of a carbohydrase (EC 3.2.x), e.g. by alpha-amylase, e.g. by cellulase, hemicellulase
    • CCHEMISTRY; METALLURGY
    • C12BIOCHEMISTRY; BEER; SPIRITS; WINE; VINEGAR; MICROBIOLOGY; ENZYMOLOGY; MUTATION OR GENETIC ENGINEERING
    • C12PFERMENTATION OR ENZYME-USING PROCESSES TO SYNTHESISE A DESIRED CHEMICAL COMPOUND OR COMPOSITION OR TO SEPARATE OPTICAL ISOMERS FROM A RACEMIC MIXTURE
    • C12P19/00Preparation of compounds containing saccharide radicals
    • C12P19/16Preparation of compounds containing saccharide radicals produced by the action of an alpha-1, 6-glucosidase, e.g. amylose, debranched amylopectin
    • 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

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Abstract

The invention relates to a method for improving the filtration rate of a crystalline dextrose saccharification liquid, which is characterized in that the DE value of the liquefaction liquid is reasonably controlled, single saccharifying enzyme and pullulanase are selected during saccharification, the saccharifying enzyme is added for reaction for a period of time, and then the pullulanase is added, so that the generation of linear chain macromolecular dextrin is greatly reduced, the recombination of the macromolecular dextrin is prevented, the precipitate formed by recombination is greatly reduced, the subsequent filtration rate is greatly improved, the production requirement can be met without adding a filter aid, the problem of difficult filtration of the saccharification liquid is fundamentally solved, the feeding value of sugar residues is improved, and the yield of dextrose is improved.

Description

Method for improving filtration speed of crystalline glucose saccharification liquid
Technical Field
The invention relates to a method for improving the filtration speed of a crystalline glucose saccharification liquid, belonging to the technical field of starch sugar production.
Background
The glucose production process mainly comprises the steps of liquefaction, saccharification, filtration, ion exchange, concentration, crystallization, drying and the like. The prior production process of glucose mainly adopts a double-enzyme method, the liquefaction process adopts secondary injection liquefaction, the temperature is reduced, the pH is adjusted, then composite saccharifying enzyme is added for saccharification, and filtration is carried out after saccharification, wherein the purpose of filtration is to remove insoluble impurities in a saccharification liquid.
The filtration in the glucose production process comprises a plate frame filter and a vacuum rotary drum filter to filter suspended or deposited water-insoluble impurities in a saccharification liquid, the plate frame filter is generally used for filtration at present, filter aids such as diatomite and the like are required to be added for both the plate frame filtration and the vacuum rotary drum filtration, and the diatomite is used as the filter aid to protect capillary pores of filter cloth from being blocked by some fine colloidal particles, so that the filtration speed is increased, the filtration period is prolonged, and the clarity of the filtrate is improved; the use of a diatomaceous earth filter aid minimizes the labor involved in the filtration operation and achieves the highest filtration rates. However, the addition of filter aids such as diatomite causes great pollution to the environment, reduces the feeding value of the sugar residues and causes great waste. Despite the maturity of existing glucose production technologies, improvements are sought through first-line investigations. The method is characterized in that the filtering process mainly adopts plate-and-frame filtration, the filtering speed is low, filter aids such as kieselguhr and the like need to be added in the filtering process, the environmental pollution is great, the filter aids cannot be used as feed raw materials, and if the filter aids are not added, the filtering speed is slower, so that the normal production cannot be realized.
Chinese patent document CN105315313A discloses a method for increasing filtration rate in glucose production, which comprises the following steps: (1) and (3) heating: adjusting the temperature of the saccharification liquid to enable protein to be flocculated after high-temperature denaturation and separated from glucose; (2) maintaining time: the maintenance time is utilized to quickly inactivate the saccharifying enzyme, thereby achieving the purpose of completely stopping the saccharifying reaction; (3) adjusting the pH value: regulating the pH value by utilizing the protein neutralization isoelectric point to further flocculate a small amount of soluble protein; (4) activated carbon decolorization: adsorbing colored substances and impurities in the saccharification liquid by using the adsorption effect of the activated carbon; (5) and (3) filtering: filtering with a filter press, and filtering the precipitated impurities such as protein, dextrin and the like to remove impurities. The method is to flocculate and separate out protein in the saccharified liquid by heating and adjusting pH to denature the protein, but the effect is still not good in the actual application process, and the filtering speed is still slow.
Through the analysis of the existing process and the reason causing the difficulty in filtration, repeated experimental analysis shows that the new combination of macromolecular dextrin in the saccharification process, particularly in the early stage of saccharification, forms viscous precipitates, the reaction is the reverse reaction of starch hydrolysis, the newly combined product amylase is difficult to decompose, the larger the dextrin molecules are, the higher the content of the amylose is, the easier the amylose is to combine, and the precipitates paste the filter cloth in the early stage of filtration, thereby causing the difficulty in filtration.
At present, crystalline glucose is produced to reach higher glucose content, the liquefied DE value is generally controlled to be 10-14%, a lower DE value means larger dextrin molecules, meanwhile, composite saccharifying enzymes are adopted in the saccharifying process, pullulanase (debranching enzyme) is compounded in the saccharifying enzymes to cut off branched chains in the macromolecular dextrin, and because the pullulanase is an endonuclease and has quick action and the saccharifying enzyme is an exonuclease and has slow action, a large amount of straight-chain dextrin is formed in a short time after the enzymes are added, so that the recombination of the macromolecular dextrin is greatly promoted, viscous precipitates are formed, the filtration difficulty is caused, and the product yield and the separation difficulty of crystalline sugar are also influenced.
Disclosure of Invention
In order to solve the defects of the prior art, the invention provides a method for improving the filtration speed of a crystalline glucose saccharification liquid.
The invention greatly eliminates the condition of recombining macromolecular dextrin by properly improving the liquefied DE value and changing the enzyme adding procedure, and greatly reduces the precipitate formed by recombining, thereby solving the problem of difficult filtration of the saccharified liquid and greatly improving the filtration speed of the saccharified liquid.
A method for increasing the filtration rate of a crystallized glucose saccharification liquid comprises the following steps:
(1) when starch is liquefied, adjusting the concentration of starch milk to 16-20 Be, adjusting the pH value to 5.5-6.0, adding high temperature resistant α -amylase, stirring the feed liquid uniformly, pumping the slurry into a jet liquefier for liquefaction to enable the DE value of the liquefied liquid to reach 14-16%, then heating to 135 ℃ and 145 ℃ for 3-5 minutes, and inactivating the enzyme;
(2) cooling the liquefied liquid after enzyme deactivation to 58-62 ℃, preserving heat, adjusting the pH value to 4.0-4.4, firstly adding saccharifying enzyme for saccharification for 16-28 hours, wherein the adding amount of the saccharifying enzyme is 500 mL/ton based on the dry starch basis, then adding pullulanase for continuous saccharification till the end, and the adding amount of the pullulanase is 100 mL/ton based on the dry starch basis and 200 mL/ton; heating the feed liquid to 70-75 ℃ to inactivate enzyme to obtain saccharified liquid;
(3) filtering the saccharified liquid by a plate and frame filter.
Preferably, according to the invention, in step (1), the high temperature resistant α -amylase is added in an amount of 400-600 mL/ton based on the dry weight of starch.
According to the invention, in the step (1), the discharge temperature is controlled at 104-110 ℃ during liquefaction, and the feed liquid discharged from the ejector enters the laminar flow tank and is subjected to heat preservation for 60-90min, so that the temperature is kept at 95-98 ℃.
Preferably, according to the invention, the adding amount of the saccharifying enzyme in the step (2) is 380-440 mL/ton based on the dry basis of starch.
Preferably, in step (2), the saccharification time is 20 to 27 hours after the addition of the saccharifying enzyme.
Preferably, in step (2), the addition amount of pullulanase is 140-180 mL/ton based on the dry weight of starch.
The invention improves the DE value of the liquefied liquid by adjusting liquefaction, so that the DE value of the liquefied liquid reaches 14-16%, the hydrolysis degree of the liquefied liquid is increased, the molecular weight of macromolecular dextrin is reduced, single saccharifying enzyme and pullulanase are adopted and are added separately in different saccharification periods, saccharifying enzyme is added firstly, the liquefied liquid is hydrolyzed to a certain degree after being saccharified for a period of time, the molecular weight of dextrin and the content of straight-chain dextrin are both greatly reduced, pullulanase is added to debranch branched-chain starch, so that the saccharifying enzyme is further hydrolyzed, the condition of recombining the macromolecular dextrin is greatly eliminated, and precipitates formed by recombining the dextrin are greatly reduced, thereby solving the problem of difficult filtration of the saccharified liquid and greatly improving the filtration speed of the saccharified liquid.
The invention has the beneficial effects that:
according to the invention, by reasonably controlling the DE value of the liquefied liquid, single saccharifying enzyme and pullulanase are selected during saccharification, and the pullulanase is added after the saccharifying enzyme is added for reaction for a period of time, so that the generation of linear macromolecular dextrin is greatly reduced, the recombination of the macromolecular dextrin is prevented, the precipitate formed by recombination is greatly reduced, the subsequent filtering speed is greatly increased, the production requirement can be met without adding a filter aid, the problem of difficult filtering of the saccharified liquid is fundamentally solved, the feeding value of sugar residues is improved, and the yield of glucose can be improved.
Detailed Description
The following detailed description of the embodiments of the present invention will make it easier for those skilled in the art to understand the present invention, and thus, the scope of the present invention will be more clearly defined.
The jet liquefier, the laminar flow tank, the saccharification tank, the vacuum flash evaporation cooling system and the plate-and-frame filter in the embodiment are all the existing commercial equipment.
Example 1
A method for improving the filtration speed of a crystalline glucose saccharification liquid comprises the following steps:
(1) in a material mixing tank, regulating the concentration of starch milk to 18 Be, regulating the pH value to 5.6, adding 400 mL/ton (calculated on a dry basis of starch) of high-temperature resistant α -amylase, uniformly stirring the material liquid, pumping the powder slurry into a jet liquefier, controlling the discharging temperature to be 104 ℃, keeping the temperature of the material liquid at 95 ℃ after the material liquid is discharged from the jet liquefier and is flashed, keeping the temperature of the material liquid in a laminar flow tank for 90min to ensure that the DE value of the liquefied liquid reaches 14.2%, heating the temperature to 135 ℃, keeping the high temperature for 5 min, and inactivating the enzyme;
(2) and (3) cooling the liquefied liquid after enzyme deactivation to 62 ℃ in a vacuum flash evaporation cooling system, preserving heat, simultaneously reducing the pH value to 4.4, adding 300 mL/ton of saccharifying enzyme (calculated by dry starch basis), adding 100 mL/ton of pullulanase (calculated by dry starch basis) after saccharifying for 27 hours, adding pullulanase after saccharifying for 27 hours, enabling the DE value to reach 96.3% after 48 hours, and spraying and heating the feed liquid to 75 ℃ for enzyme deactivation.
(3) The saccharified solution was filtered with a plate and frame filter without adding a filter aid, at a filtration pressure of 0.12MPa and a filtration flow rate of 21 cubic/hr, exceeding 18 cubic/hr in the comparative example.
Example 2
A method for improving the filtration speed of a crystalline glucose saccharification liquid comprises the following steps:
(1) in a material mixing tank, regulating the concentration of starch milk to 20 Be, regulating the pH value to 6.0, adding 600 mL/ton (calculated on a dry basis of starch) of high-temperature resistant α -amylase, uniformly stirring the material liquid, pumping the powder slurry into a jet liquefier, controlling the discharging temperature to be 110 ℃, keeping the temperature of the material liquid at 97 ℃ after the material liquid is discharged from the jet liquefier for flash evaporation, keeping the temperature of the material liquid in a laminar flow tank for 70min to ensure that the DE value of the liquefied liquid reaches 15.3%, heating the temperature to 145 ℃, keeping the high temperature for 3 min, and inactivating the enzyme;
(2) and (3) cooling the liquefied liquid after enzyme deactivation to 60 ℃ in a vacuum flash evaporation cooling system, preserving heat, simultaneously reducing the pH value to 4.2, adding 500 mL/ton of saccharifying enzyme (calculated by dry starch basis), introducing into a saccharifying tank for saccharification, adding 200 mL/ton of pullulanase (calculated by dry starch basis) after 18 hours of saccharification, enabling the DE value to reach 96.4% after 44 hours, and spraying and heating the feed liquid to 70 ℃ for enzyme deactivation.
(3) The saccharified solution was filtered with a plate and frame filter without adding a filter aid, at a filtration pressure of 0.13MPa and a filtration flow rate of 20 cubic/hr, exceeding that of the comparative example of 18 cubic/hr.
Example 3
A method for improving the filtration speed of a crystalline glucose saccharification liquid comprises the following steps:
(1) in a material mixing tank, regulating the concentration of starch milk to 16 Be, regulating the pH value to 5.6, adding high-temperature resistant α -amylase 400 mL/ton (calculated on a dry basis of starch), uniformly stirring the material liquid, pumping the powder slurry into a jet liquefier, controlling the discharging temperature to be 107 ℃, keeping the temperature of the material liquid at 96 ℃ after the material liquid is discharged from the jet liquefier and is flashed, keeping the temperature of the material liquid in a laminar flow tank for 80min to ensure that the DE value of the liquefied liquid reaches 14.9%, heating the temperature to 140 ℃, keeping the high temperature for 4 min, and inactivating the enzyme;
(2) and (3) cooling the liquefied liquid after enzyme deactivation to 58 ℃ in a vacuum flash evaporation cooling system, preserving heat, simultaneously reducing the pH value to 4.0, firstly adding 400 mL/ton of saccharifying enzyme (calculated by dry starch basis), then adding 150 mL/ton of pullulanase (calculated by dry starch basis) after saccharifying for 20 hours, enabling the DE value to reach 96.6% after 46 hours, and spraying and heating the liquid to 75 ℃ for enzyme deactivation.
(3) The saccharified solution was filtered with a plate and frame filter without adding a filter aid, at a filtration pressure of 0.11MPa and a filtration flow rate of 22 cubic/hr, exceeding 18 cubic/hr in the comparative example.
Comparative example 1
A method for improving the filtration speed of a crystalline glucose saccharification liquid comprises the following steps:
(1) in a material mixing tank, regulating the concentration of starch milk to 18 Be, regulating the pH value to 5.6, adding 400mL of high-temperature resistant α -amylase, stirring the feed liquid uniformly, pumping the slurry into a jet liquefier, controlling the discharge temperature to be 105 ℃, flashing the slurry from a jet liquefier, keeping the temperature at 96 ℃, keeping the temperature of the slurry at 13 ℃ after the slurry enters a laminar flow tank, keeping the temperature for 80min, keeping the DE value at 13.2%, performing secondary jet, heating the temperature to 135 ℃, keeping the high temperature for 5 min, and deactivating the enzyme.
(2) The feed liquid enters a vacuum flash evaporation cooling system to be cooled to 60 ℃ for heat preservation, simultaneously the pH value is reduced to 4.2, 500 mL/ton (dry basis) of composite saccharifying enzyme sold in the market is added, the feed liquid enters a saccharifying tank for saccharification, the DE value reaches 96.2 percent after 46 hours of saccharification, and the feed liquid is sprayed and heated to 75 ℃ for enzyme deactivation.
(3) Filtering with a plate-and-frame filter after saccharification, adding filter aid 5kg in advance to form a filter layer on the filter cloth, wherein the filtering pressure is 0.16Mpa, and the filtering flow is 18 cubic/hour.
Experimental example:
the filtration pressure of examples 1 to 3 and comparative example were measured, and the results of the filtration flow rate test are shown in table 1 below.
TABLE 1 filtration pressure, filtration flow for different treatment methods
Filtering the flow Filtration pressure
Example 1 22 cubic/hour 0.12Mpa
Example 2 21 cubic per hour 0.13Mpa
Example 3 23 cubic/hour 0.11Mpa
Comparative example 12 cubic/hour 0.21Mpa
As can be seen from Table 1, the method improves the DE value of the liquefied liquid, adopts single saccharifying enzyme and pullulanase, separately adds the saccharifying enzyme at different saccharifying periods, adds the pullulanase after saccharifying for a period of time, improves the filtration flow, reduces the filtration pressure, solves the problem of difficult filtration of the saccharified liquid, and greatly improves the filtration speed of the saccharified liquid.

Claims (6)

1. A method for increasing the filtration rate of a crystallized glucose saccharification liquid comprises the following steps:
(1) when starch is liquefied, adjusting the concentration of starch milk to 16-20 Be, adjusting the pH value to 5.5-6.0, adding high temperature resistant α -amylase, stirring the feed liquid uniformly, pumping the slurry into a jet liquefier for liquefaction to enable the DE value of the liquefied liquid to reach 14-16%, then heating to 135 ℃ and 145 ℃ for 3-5 minutes, and inactivating the enzyme;
(2) cooling the liquefied liquid after enzyme deactivation to 58-62 ℃, preserving heat, adjusting the pH value to 4.0-4.4, firstly adding saccharifying enzyme for saccharification for 16-28 hours, wherein the adding amount of the saccharifying enzyme is 500 mL/ton based on the dry starch basis, then adding pullulanase for continuous saccharification till the end, and the adding amount of the pullulanase is 100 mL/ton based on the dry starch basis and 200 mL/ton; heating the feed liquid to 70-75 ℃ to inactivate enzyme to obtain saccharified liquid;
(3) filtering the saccharified liquid by a plate and frame filter.
2. The method as set forth in claim 1, wherein the high temperature resistant α -amylase is added in an amount of 400-600 mL/ton on a dry basis of starch in step (1).
3. The method as claimed in claim 1, wherein in the step (1), the temperature of the discharged liquid is controlled to be 104-110 ℃, and the liquid discharged from the ejector enters the laminar flow tank and is kept at 95-98 ℃ for 60-90 min.
4. The method as set forth in claim 1, wherein the amount of saccharifying enzyme added in step (2) is 380-440 mL/ton on a dry basis of starch.
5. The method for increasing the filtration rate of a crystallized glucose glycated liquid according to claim 1, wherein the glycation time after the addition of the saccharifying enzyme in step (2) is 20 to 27 hours.
6. The method for increasing the filtration rate of a crystallized glucose saccharification liquid of claim 1, wherein in step (2), the pullulanase is added in an amount of 140-180 mL/ton based on the dry basis of starch.
CN201911344643.7A 2019-12-24 2019-12-24 Method for improving filtration speed of crystalline glucose saccharification liquid Pending CN110982861A (en)

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CN101831477A (en) * 2010-05-21 2010-09-15 万福生科(湖南)农业开发股份有限公司 Method for preparing rice into glucose for injection
CN104903459A (en) * 2012-12-14 2015-09-09 丹尼斯科美国公司 Method of using alpha-amylase from aspergillus fumigatus and pullulanase for saccharification
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* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US3565765A (en) * 1966-12-27 1971-02-23 Cpc International Inc Preparation of high maltose conversion products
CN101684504A (en) * 2008-09-26 2010-03-31 保龄宝生物股份有限公司 Preparation method of superhigh maltose syrup
CN101831477A (en) * 2010-05-21 2010-09-15 万福生科(湖南)农业开发股份有限公司 Method for preparing rice into glucose for injection
CN104903459A (en) * 2012-12-14 2015-09-09 丹尼斯科美国公司 Method of using alpha-amylase from aspergillus fumigatus and pullulanase for saccharification
CN105483181A (en) * 2015-12-28 2016-04-13 河南飞天农业开发股份有限公司 Preparation method of high-purity glucose

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Title
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Application publication date: 20200410