CN113527533A - Pullulan film concentration process - Google Patents
Pullulan film concentration process Download PDFInfo
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- CN113527533A CN113527533A CN202110607784.4A CN202110607784A CN113527533A CN 113527533 A CN113527533 A CN 113527533A CN 202110607784 A CN202110607784 A CN 202110607784A CN 113527533 A CN113527533 A CN 113527533A
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08B—POLYSACCHARIDES; DERIVATIVES THEREOF
- C08B37/00—Preparation of polysaccharides not provided for in groups C08B1/00 - C08B35/00; Derivatives thereof
- C08B37/0003—General processes for their isolation or fractionation, e.g. purification or extraction from biomass
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08B—POLYSACCHARIDES; DERIVATIVES THEREOF
- C08B37/00—Preparation of polysaccharides not provided for in groups C08B1/00 - C08B35/00; Derivatives thereof
- C08B37/0006—Homoglycans, i.e. polysaccharides having a main chain consisting of one single sugar, e.g. colominic acid
- C08B37/0009—Homoglycans, i.e. polysaccharides having a main chain consisting of one single sugar, e.g. colominic acid alpha-D-Glucans, e.g. polydextrose, alternan, glycogen; (alpha-1,4)(alpha-1,6)-D-Glucans; (alpha-1,3)(alpha-1,4)-D-Glucans, e.g. isolichenan or nigeran; (alpha-1,4)-D-Glucans; (alpha-1,3)-D-Glucans, e.g. pseudonigeran; Derivatives thereof
- C08B37/0018—Pullulan, i.e. (alpha-1,4)(alpha-1,6)-D-glucan; Derivatives thereof
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- Separation Using Semi-Permeable Membranes (AREA)
- Preparation Of Compounds By Using Micro-Organisms (AREA)
Abstract
The invention belongs to the technical field of pullulan production, and particularly discloses a pullulan film concentration process which specifically comprises the following steps: s1, preprocessing: introducing fermentation liquor containing pullulan polysaccharide and more impurities into a pretreatment tank, and carrying out high-temperature enzyme deactivation treatment; s2, clarification: adding a proper amount of filter aid into the fermentation liquor, and introducing the fermentation liquor into a plate-and-frame filter press for filter pressing to obtain clear liquor; s3, decoloring: introducing the clarified liquid into a decoloring tank for decoloring; s4, protein removal: introducing the decolorized clear solution into a treatment tank, and removing impurity proteins by using a resin adsorption method to obtain a treatment solution; s5, ultrafiltration treatment: introducing the treatment solution into an ultrafiltration membrane system, and performing circulating filtration; s6, drying: collecting the ultrafiltration membrane concentrated solution obtained by the step S5, and performing spray drying to obtain a powdery finished product; the method can fully remove impurities in the fermentation liquor, and has the advantages of high product purity, simple process flow, lower energy consumption and low production cost.
Description
Technical Field
The invention relates to the technical field of pullulan production, in particular to a pullulan film concentration process.
Background
Pullulan is an extracellular water-soluble mucopolysaccharide prepared by fermenting corn, also known as Aureobasidium pullulans and pullulan, and has the English name of Pullulan. Due to the unique structure and properties of the polysaccharide, the polysaccharide has wide application prospect in the industries of medicine, food, petroleum, chemical industry and the like. Because the biodegradable plastic can be degraded and utilized by microorganisms in nature, and cannot cause environmental pollution, the plastic is praised as nuisanceless plastic. No. 8 announcement is issued by the national ministry of health in 2006, and pullulan is one of four new food additive products and can be used as a coating agent and a thickening agent in candies, chocolate coatings, films, compound seasoning families and fruit and vegetable juice beverages. The pullulan is industrially prepared by a microbial fermentation method, but the fermentation liquor has more impurities besides the pullulan, and the pullulan solution with higher purity can be obtained by further filtering. In the traditional process, impurities are removed by adopting a plate-frame filtration or activated carbon filtration mode, or the concentration of the solution is improved by adopting a thermal concentration method, but the removal of the impurities such as protein, ash, monosaccharide, disaccharide and the like by adopting the plate-frame filtration and activated carbon filtration methods is insufficient, the product quality is difficult to ensure, and the loss of pullulan components is large; the heat concentration has high energy consumption, and the high temperature can denature protein and reduce the product quality.
Disclosure of Invention
The invention aims to provide a pullulan film concentration process to solve the problems in the background technology.
In order to achieve the purpose, the invention provides the following technical scheme: a pullulan film concentration process specifically comprises the following steps:
s1, preprocessing: introducing fermentation liquor containing pullulan polysaccharide and more impurities into a pretreatment tank, and carrying out high-temperature enzyme deactivation treatment;
s2, clarification: adding a proper amount of filter aid into the fermentation liquor, and introducing the fermentation liquor into a plate-and-frame filter press for filter pressing to obtain clear liquor;
s3, decoloring: introducing the clarified liquid into a decoloring tank for decoloring;
s4, protein removal: introducing the decolorized clear solution into a treatment tank, and removing impurity proteins by using a resin adsorption method to obtain a treatment solution;
s5, ultrafiltration treatment: introducing the treatment solution into an ultrafiltration membrane system, and performing circulating filtration;
s6, drying: and (4) collecting the ultrafiltration membrane concentrated solution obtained by the step S5, and performing spray drying to obtain a powdery finished product.
Preferably, the temperature of the high-temperature enzyme deactivation treatment in the step S1 is 70-90 ℃, and the treatment time is 1-2 h.
Preferably, the filter aid in step S2 includes any one or more of diatomite, perlite, cellulose and asbestos, and the mass of the filter aid accounts for 1-3% of the total mass of the fermentation broth.
Preferably, the decoloring in step S3 specifically includes the following steps: adding activated carbon into the clear solution, and stirring to uniformly mix the solution.
Preferably, the mass of the activated carbon accounts for 0.1-1% of the total mass of the clarified liquid, the decoloring treatment temperature is 20-80 ℃, and the stirring treatment time is 20-100 min.
Preferably, the step S3 further includes hydrogen peroxide treatment after the activated carbon is decolorized, and specifically includes the following steps: adding a hydrogen peroxide solution into the solution subjected to the activated carbon decoloration treatment, wherein the mass of the hydrogen peroxide solution accounts for 0.1-0.5% of the total mass of the solution.
Preferably, the ultrafiltration treatment in the step S5 adopts a roll-type ultrafiltration membrane, the molecular weight of the roll-type ultrafiltration membrane is 2000-10000 Dalton, the ultrafiltration treatment pressure is 3-10bar, and the temperature is 10-40 ℃.
Preferably, the circulating filtration in step S5 specifically includes the following steps: introducing the concentrated solution into a circulating tank, and adding dialysis water into the circulating tank when the solid content of the feed liquid reaches 15-30%.
Preferably, the mass ratio of the dialysis water to the feed liquid is 1: 1.
compared with the prior art, the invention has the beneficial effects that:
1) by adopting a membrane filtration and concentration mode, the contents of protein, monosaccharide, disaccharide and ash can be greatly reduced, and the product quality is improved;
2) the temperature, pressure, flow and the like of a system are adjusted by a certain technical means, corresponding ultrafiltration membrane filtration technical parameters are set according to the quality requirement of a product, a high-concentration pullulan solution is produced, the energy consumption of a subsequent drying section is reduced, the energy consumption of membrane concentration is only 1/5-1/3 of that of the traditional heat concentration process, and the product quality is better than that of a heat concentration process;
3) clear liquid separated in the ultrafiltration membrane concentration process is clear and transparent in color, almost has no effective components, can be recycled, saves resources and reduces cost;
4) the traditional processes such as plate-frame filtration and the like are low in filtration precision, so that the loss of pullulan is easily caused compared with membrane filtration, the defects of the traditional processes can be basically avoided by ultrafiltration membrane filtration, and the product yield is greatly improved;
5) the ultrafiltration membrane system is simple to operate, the production cost can be reduced, the working environment is improved compared with that of the traditional process, and the working strength of workers is lower.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
In the description of the present invention, it should also be noted that, unless otherwise explicitly specified or limited, the terms "disposed," "mounted," "connected," and "connected" are to be construed broadly and may, for example, be fixedly connected, detachably connected, or integrally connected; can be mechanically or electrically connected; they may be connected directly or indirectly through intervening media, or they may be interconnected between two elements. The specific meanings of the above terms in the present invention can be understood by those skilled in the art according to specific situations.
Example one
The invention provides a technical scheme that: a pullulan film concentration process specifically comprises the following steps:
s1, preprocessing: introducing fermentation liquor containing pullulan polysaccharide and more impurities into a pretreatment tank, and carrying out high-temperature enzyme deactivation treatment;
s2, clarification: adding a proper amount of filter aid into the fermentation liquor, and introducing the fermentation liquor into a plate-and-frame filter press for filter pressing to obtain clear liquor;
s3, decoloring: introducing the clarified liquid into a decoloring tank for decoloring;
s4, protein removal: introducing the decolorized clear solution into a treatment tank, and removing impurity proteins by using a resin adsorption method to obtain a treatment solution;
s5, ultrafiltration treatment: introducing the treatment solution into an ultrafiltration membrane system, performing circulating filtration, and removing 60-90% of protein, 99% of monosaccharide and disaccharide, ash content and the like in the solution by an ultrafiltration concentration mode to improve the purity of the product;
s6, drying: and (4) collecting the ultrafiltration membrane concentrated solution obtained by the step S5, and performing spray drying to obtain a powdery finished product.
The high-temperature enzyme deactivation treatment temperature in the step S1 is 70 ℃, and the treatment time is 2 h.
The filter aid in the step S2 comprises any one or a combination of more of diatomite, perlite, cellulose and asbestos, and the mass of the filter aid accounts for 1% of the total mass of the fermentation liquor.
The decoloring processing in step S3 specifically includes the following steps: adding activated carbon into the clear solution, and stirring to uniformly mix the solution.
The mass of the active carbon accounts for 0.1 percent of the total mass of the clarified liquid, the decoloring temperature is 20 ℃, and the stirring treatment time is 100 min.
The step S3 further includes hydrogen peroxide treatment after the activated carbon is decolored, and specifically includes the following steps: the solution decolorized by activated carbon was added with a hydrogen peroxide solution in an amount of 0.1% by mass based on the total mass of the solution, and the pigment in the solution was further removed by the hydrogen peroxide treatment.
The ultrafiltration treatment in the step S5 adopts a roll-type ultrafiltration membrane, the molecular weight of the roll-type ultrafiltration membrane is 2000 daltons, the ultrafiltration treatment pressure is 3bar, and the temperature is 10 ℃.
The circulating filtration in the step S5 specifically includes the following steps: and (3) introducing the concentrated solution subjected to ultrafiltration treatment into a circulating tank, and adding dialysis water into the circulating tank when the solid content of the feed liquid reaches 15%.
The mass ratio of the dialysis water to the feed liquid is 1: 1.
example two
The difference from the first embodiment is that: the high-temperature enzyme deactivation treatment temperature in the step S1 is 80 ℃, and the treatment time is 1.5 h;
the mass of the filter aid in the step S2 accounts for 2% of the total mass of the fermentation liquor;
the mass of the active carbon accounts for 0.5 percent of the total mass of the clarified liquid, the decoloring temperature is 50 ℃, and the stirring treatment time is 60 min;
the step S3 further includes hydrogen peroxide treatment after the activated carbon is decolored, and specifically includes the following steps: adding a hydrogen peroxide solution into the solution subjected to the activated carbon decoloration treatment, wherein the mass of the hydrogen peroxide solution accounts for 0.3% of the total mass of the solution;
the ultrafiltration treatment in the step S5 adopts a roll-type ultrafiltration membrane, the molecular weight of the roll-type ultrafiltration membrane is 5000 daltons, the ultrafiltration treatment pressure is 7bar, and the temperature is 25 ℃;
the circulating filtration in the step S5 specifically includes the following steps: and (3) introducing the concentrated solution subjected to ultrafiltration treatment into a circulating tank, and adding dialysis water into the circulating tank when the solid content of the feed liquid reaches 20%.
EXAMPLE III
The difference from the first embodiment is that: the high-temperature enzyme deactivation treatment temperature in the step S1 is 90 ℃, and the treatment time is 1 h;
the mass of the filter aid in the step S2 accounts for 3% of the total mass of the fermentation liquor;
the mass of the active carbon accounts for 1 percent of the total mass of the clarified liquid, the decoloring temperature is 80 ℃, and the stirring treatment time is 20 min;
the step S3 further includes hydrogen peroxide treatment after the activated carbon is decolored, and specifically includes the following steps: adding a hydrogen peroxide solution into the solution subjected to the activated carbon decoloration treatment, wherein the mass of the hydrogen peroxide solution accounts for 0.5% of the total mass of the solution;
the ultrafiltration treatment in the step S5 adopts a roll-type ultrafiltration membrane, the molecular weight of the roll-type ultrafiltration membrane is 10000 daltons, the ultrafiltration treatment pressure is 10bar, and the temperature is 40 ℃;
the circulating filtration in the step S5 specifically includes the following steps: and (3) introducing the concentrated solution subjected to ultrafiltration treatment into a circulating tank, and adding dialysis water into the circulating tank when the solid content of the feed liquid reaches 30%.
Examples of the experiments
The pullulan content in the product prepared in each example of the present invention was determined according to the following procedure:
1) taking the same amount of finished product powder prepared in the first to third embodiments, taking three parts of the finished product powder in each embodiment, adding the same amount of distilled water, and uniformly mixing to obtain a sample solution;
2) each sample solution was divided into two equal portions, and one portion was adjusted with acid solution to H+The concentration is 0.2-0.8 mol/L, and boiling water bath is carried out for 1-5 min; adjusting H with acid solution+The concentration is 2.0-3.0 mol/L, and the boiling water bath lasts for 20-60 min; measuring the glucose content in the hydrolysate by a biosensing analyzer method, wherein the glucose content is A and B respectively;
3) the pullulan content was calculated according to the following formula:
in the formula: 162: the molecular weight of the pullulan monosaccharide units; 180: molecular weight of glucose.
The measured pullulan content was compared with the mass of the sample solution, and the results were calculated as the percentage of pullulan in each sample solution as shown in the following table:
as can be seen from the above table, the pullulan content in the product powder prepared by the embodiments of the present invention is stabilized at more than 90%, and the product purity is high.
Although embodiments of the present invention have been shown and described, it will be appreciated by those skilled in the art that changes, modifications, substitutions and alterations can be made in these embodiments without departing from the principles and spirit of the invention, the scope of which is defined in the appended claims and their equivalents.
Claims (9)
1. A pullulan film concentration process is characterized in that: the method specifically comprises the following steps:
s1, preprocessing: introducing fermentation liquor containing pullulan polysaccharide and more impurities into a pretreatment tank, and carrying out high-temperature enzyme deactivation treatment;
s2, clarification: adding a proper amount of filter aid into the fermentation liquor, and introducing the fermentation liquor into a plate-and-frame filter press for filter pressing to obtain clear liquor;
s3, decoloring: introducing the clarified liquid into a decoloring tank for decoloring;
s4, protein removal: introducing the decolorized clear solution into a treatment tank, and removing impurity proteins by using a resin adsorption method to obtain a treatment solution;
s5, ultrafiltration treatment: introducing the treatment solution into an ultrafiltration membrane system, and performing circulating filtration;
s6, drying: and (4) collecting the ultrafiltration membrane concentrated solution obtained by the step S5, and performing spray drying to obtain a powdery finished product.
2. The pullulan film concentration process according to claim 1, wherein: the high-temperature enzyme deactivation treatment temperature in the step S1 is 70-90 ℃, and the treatment time is 1-2 h.
3. The pullulan film concentration process according to claim 1, wherein: the filter aid in the step S2 comprises any one or a combination of more of diatomite, perlite, cellulose and asbestos, and the mass of the filter aid accounts for 1-3% of the total mass of the fermentation liquor.
4. The pullulan film concentration process according to claim 1, wherein: the decoloring processing in step S3 specifically includes the following steps: adding activated carbon into the clear solution, and stirring to uniformly mix the solution.
5. The pullulan film concentration process according to claim 4, wherein: the mass of the active carbon accounts for 0.1-1% of the total mass of the clarified liquid, the decoloring treatment temperature is 20-80 ℃, and the stirring treatment time is 20-100 min.
6. The pullulan film concentration process according to claim 5, wherein: the step S3 further includes hydrogen peroxide treatment after the activated carbon is decolored, and specifically includes the following steps: adding a hydrogen peroxide solution into the solution subjected to the activated carbon decoloration treatment, wherein the mass of the hydrogen peroxide solution accounts for 0.1-0.5% of the total mass of the solution.
7. The pullulan film concentration process according to claim 1, wherein: the ultrafiltration treatment in the step S5 adopts a roll-type ultrafiltration membrane, the molecular weight of the roll-type ultrafiltration membrane is 2000-10000 Dalton, the ultrafiltration treatment pressure is 3-10bar, and the temperature is 10-40 ℃.
8. The pullulan film concentration process according to claim 1, wherein: the circulating filtration in the step S5 specifically includes the following steps: introducing the concentrated solution into a circulating tank, and adding dialysis water into the circulating tank when the solid content of the feed liquid reaches 15-30%.
9. The pullulan film concentration process according to claim 8, wherein: the mass ratio of the dialysis water to the feed liquid is 1: 1.
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| CN202110607784.4A CN113527533A (en) | 2021-06-01 | 2021-06-01 | Pullulan film concentration process |
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Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US3912591A (en) * | 1972-09-04 | 1975-10-14 | Hayashibara Biochem Lab | Process for the production of pullulan |
| CN103172757A (en) * | 2012-12-31 | 2013-06-26 | 天津北洋百川生物技术有限公司 | Extracting process of pulullan polysaccharide |
-
2021
- 2021-06-01 CN CN202110607784.4A patent/CN113527533A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US3912591A (en) * | 1972-09-04 | 1975-10-14 | Hayashibara Biochem Lab | Process for the production of pullulan |
| CN103172757A (en) * | 2012-12-31 | 2013-06-26 | 天津北洋百川生物技术有限公司 | Extracting process of pulullan polysaccharide |
Non-Patent Citations (1)
| Title |
|---|
| 万玉军等: ""工业化发酵生产普鲁兰多糖的提取条件优化"", 《食品与发酵工业》 * |
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