CN101095457B - Method of producing acid hydrolyzed casein - Google Patents
Method of producing acid hydrolyzed casein Download PDFInfo
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- CN101095457B CN101095457B CN2007100182457A CN200710018245A CN101095457B CN 101095457 B CN101095457 B CN 101095457B CN 2007100182457 A CN2007100182457 A CN 2007100182457A CN 200710018245 A CN200710018245 A CN 200710018245A CN 101095457 B CN101095457 B CN 101095457B
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Abstract
The invention discloses a method for producing acid-hydrolytic casein, which takes milk coarse protein that is used to extract butter as raw material, and comprises following steps: selecting, disintegrating, dissolving, filtering, acidifying, washing, dewatering, drying, purifying and getting casein, hydrolyzing with 4-12mol/ l hydrochloride or sulfate or phosphoric acid at 90-100 Deg. C for 2-4hours, condensing and washing repeatedly for 1-3 times, de-coloring with active carbon, exchanging with weak alkali or weak anion resin, spray drying at 120-160 Deg . C, and getting acid-hydrolytic casein. The invention is characterized by short hydrolysis time, simple process, short time for whole process of about 8-10 hours, reduced production period and cost, and suitability for mass industrialproduction.
Description
Technical field
The present invention relates to organic chemistry acid hydrolysis field, specifically a kind of is the production method of raw material production acid hydrolyzed casein with the milk crude protein behind the extraction butter.
Background technology
At present, domestic research field is all with concentration of hydrochloric acid 18%, solid-to-liquid ratio 1: 1.6,106 ℃ of hydrolysis temperatures, hydrolysis time 18 hours, after finishing, hydrolysis uses sodium hydroxide solution adjust pH 4.9～5.2, be that optimum reaction condition prepares acid hydrolyzed casein with activated carbon decolorizing then, its specific embodiment is: casein+18% hydrochloric acid soln (1: 1.6) is heated to 18 hours → filtration → usefulness of 106 ℃ → hydrolysis sodium hydroxide solution adjust pH, 4.9～5.2 → resins exchange, the first step: highly acidic cation 001 * 7 (732), second step: strongly basic anion 201 * 7 (717) → concentrate → drying → product → test package.Such production technique can only be used for the investigator and do some samples in the laboratory for research because hydrolysis time is long, power consumption is big, output capacity is low, can't carry out suitability for industrialized production at all.
Summary of the invention
Technical problem to be solved by this invention is to solve the deficiency of above-mentioned acid hydrolyzed casein technology, and a kind of hydrolysis time is short, technology is simple, the production method of the acid hydrolyzed casein of the low plant size production of production cost but provide.
Technical problem of the present invention solves by following technical proposals:
A kind of production method of acid hydrolyzed casein mainly is raw material with the casein, is prepared from step as follows:
(a) hydrolysis
Accurately taking by weighing 1 part of casein joins in the three-necked bottle, the hydrochloric acid that the distilled water that adds 1～4 part then successively stirred, added 1～4 part of 4～12mol/L stirs, warming while stirring, solution bulk boiling when temperature reaches 90～100 ℃, continue constant temperature and stir hydrolysis 3hr, treat to stop hydrolysis after the solution hydrolysis does not thoroughly have casein particle;
(b) filter
Add 1～4 part of distilled water in the hydrolyzed solution that (a) one-step hydrolysis is good, with 80～120 order nylon net filters;
(c) concentrate
Above-mentioned filtered liquid gradation is joined in the round-bottomed flask, and the 650～700mmHg that reduces pressure is concentrated into paste, adds 1～6 part of distilled water by negative pressure, stirs, and it is dissolved fully; And then be evaporated to paste, and thickening and washing is three times so repeatedly, can finish washing, and this moment, the pH value was 3.5～4.5;
(d) decolouring
Hydrolyzed solution that above-mentioned washing is good adds with (a) gac of one-step hydrolysis total solid content equal in quality mark 5～50% and refluxed 2.0～4.0 hours, and heat decompression 650～700mmHg filters, and it is light yellow that filtrate is;
(e) depickling
The light yellow filtrate pH value that above-mentioned decolouring is good is 2.0～3.0, residual a large amount of HCL in the filtrate, and HCL adopts strong basicity or weakly alkaline phenylethylene, or weakly alkaline epoxy system or weakly alkaline acrylic resin exchange depickling by 1: 4～1: 8 ratio single stage method;
(f) concentrated, dry
Acid hydrolyzed casein pH value of solution value after resins exchange is 6.5～7.0, and solution is after concentrating, in pressure 15～30MPa, 120～160 ℃ of following spraying dryings of temperature, and it is milky white or faint yellow that products obtained therefrom is.
Above-mentioned casein is a main raw material with the milk crude protein that extracts behind the butter, obtains after impurity is removed in people's wage adjustment choosing, after the pulverizing, dissolving, filtration, acidifying, washing, dehydration, dry purifying.
Product index:
1, physical and chemical index:
Sense organ: milky white or faint yellow fine granularity powder;
Smell: the smell that special happiness is arranged;
Nitrogen content: 〉=10.0～14.0%
Moisture :≤6.0%
Ash content :≤3.0%
PH value: 6.5～7.0
2, microbiological indicator:
Total plate count≤30cfu/g
Coliform MPN/100g≤40
Pathogenic bacterium must not detect
3, heavy metal index:
Arsenic (in As)≤0.0002%
Plumbous (in Pb)≤0.002%
Hydrolysis time of the present invention is short, technology is simple, the whole technology deadline only needs 8～10hr; shortened the production cycle greatly; but reduced the production of production cost plant size, no matter all be better than traditional technology from hydrolysis time, power consumption, output capacity, production cost.
Embodiment
Below in conjunction with embodiment the present invention is further elaborated.
Embodiment 1:
1 hydrolysis
Accurately taking by weighing the 100g casein joins in the 1000ml three-necked bottle, the distilled water that adds 100ml then successively stirs, the concentrated hydrochloric acid of 100ml12mol/L stirs, install prolong, electronic stirring, electric mantle, warming while stirring, solution bulk boiling when temperature reaches 90 ℃, continue constant temperature and stir hydrolysis 3hr, treat to stop hydrolysis after the solution hydrolysis does not thoroughly have casein particle.
2 filter
In the good hydrolyzed solution of the 1st one-step hydrolysis, add 100ml distilled water, with 80 order nylon net filters.
3 concentrate
Above-mentioned filtered liquid gradation is joined in the 1000ml round-bottomed flask, be concentrated into paste, add 100ml distilled water, reduce the Rotary Evaporators rotating speed, it is dissolved fully by negative pressure with the Rotary Evaporators 650mmHg that reduces pressure.And then be evaporated to paste, and thickening and washing is three times so repeatedly, can finish washing, and this moment, the pH value 3.5.
4 decolourings
The hydrolyzed solution that above-mentioned washing is good adds the gac of pressing solid content massfraction 5% and refluxed 4.0 hours, filters with filter flask, B heat decompression 650mmHg, and it is light yellow that filtrate is, and the pH value is 2.0.
5 depicklings
Light yellow filtrate after the decolouring is collected the exchange fluid component of 6.5～7.0 sections of pH values through the exchange of strongly basic anion 201 * 7 (717) resin single stage method.
6 dryings
After the good solution concentration of resins exchange, in pressure 15MPa, 120 ℃ of following spraying dryings of temperature, it is milky white or faint yellow that products obtained therefrom is.
Example 2
1 hydrolysis
Accurately taking by weighing the 200g casein joins in the 1000ml three-necked bottle, the distilled water that adds 400ml then successively stirs, the sulfuric acid of 400ml 4mol/L stirs, install prolong, electronic stirring, electric mantle, warming while stirring, solution bulk boiling when temperature reaches 100 ℃, continue constant temperature and stir hydrolysis 3hr, treat to stop hydrolysis after the solution hydrolysis does not thoroughly have casein particle.
2 filter
With adding 400ml distilled water in the good hydrolyzed solution of the first step hydrolysis, with 120 order nylon net filters.
3 concentrate
Above-mentioned filtered liquid gradation is joined in the 1000ml round-bottomed flask, be concentrated into paste, add 600ml distilled water, reduce the Rotary Evaporators rotating speed, it is dissolved fully by negative pressure with the Rotary Evaporators 700mmHg that reduces pressure.And then being evaporated to paste, thickening and washing is three times so repeatedly.Can finish washing, this moment, the pH value 4.5.
4 decolourings
The hydrolyzed solution that above-mentioned washing is good adds and the gac of the 1st one-step hydrolysis total solid content equal in quality mark 50% refluxed 2.0 hours, and with filter flask, B heat decompression 700mmHg filtration, it is light yellow that filtrate is.
5 depicklings
Light yellow filtrate after decolouring this moment is 6.5～7.0 sections exchange fluid component through strongly basic anion 701 (331) resin single stage method exchange collection pH value.
6 dryings
After the good solution concentration of resins exchange, in pressure 30MPa, 160 ℃ of following spraying dryings of temperature, it is milky white or faint yellow that products obtained therefrom is.
Example 3
1 hydrolysis
Accurately taking by weighing the 200g casein joins in the 1000ml three-necked bottle, the distilled water that adds 200ml then successively stirs, the phosphoric acid of 200ml 6mol/L stirs, install prolong, electronic stirring, electric mantle, warming while stirring, solution bulk boiling when temperature reaches 95 ℃, continue constant temperature and stir hydrolysis 3hr, treat to stop hydrolysis after the solution hydrolysis does not thoroughly have casein particle.
2 filter
With adding 100ml distilled water in the good hydrolyzed solution of the first step hydrolysis, with 100 order nylon net filters.
3 concentrate
Above-mentioned filtered liquid gradation is joined in the 1000ml round-bottomed flask, be concentrated into paste, add 200ml distilled water, reduce the Rotary Evaporators rotating speed, it is dissolved fully by negative pressure with the Rotary Evaporators 700mmHg that reduces pressure.And then being evaporated to paste, thickening and washing is three times so repeatedly.Can finish washing, this moment, the pH value 4.0.
4 decolourings
The hydrolyzed solution that above-mentioned washing is good adds and the gac of (1) one-step hydrolysis total solid content equal in quality mark 30% refluxed 3 hours, and with filter flask, B heat decompression 690mmHg filtration, it is light yellow that filtrate is.
5 depicklings
Light yellow filtrate after decolouring this moment is collected the exchange fluid component of 6.5～7.0 sections of pH values through the exchange of strongly basic anion 705 (D313) resin single stage method.
6 dryings
After the good solution concentration of resins exchange, in pressure 20MPa, 150 ℃ of following spraying dryings of temperature, it is milky white or faint yellow that products obtained therefrom is.
Claims (5)
1. the production method of an acid hydrolyzed casein is raw material with the casein mainly, is prepared from step as follows:
(a) hydrolysis
Accurately taking by weighing 1 part of casein joins in the three-necked bottle, the hydrochloric acid that the distilled water that adds 1～4 part then successively stirred, added 1～4 part of 4～12mol/L stirs, warming while stirring, solution bulk boiling when temperature reaches 90～100 ℃, continue constant temperature and stir hydrolysis 3hr, treat to stop hydrolysis after the solution hydrolysis does not thoroughly have casein particle;
(b) filter
Add 1～4 part of distilled water in the hydrolyzed solution that (a) one-step hydrolysis is good, with 80～120 order nylon net filters;
(c) concentrate
Above-mentioned filtered liquid gradation is joined in the round-bottomed flask, and the 650～700mmHg that reduces pressure is concentrated into paste, adds 1～6 part of distilled water by negative pressure, stirs, and it is dissolved fully; And then be evaporated to paste, and thickening and washing is three times so repeatedly, can finish washing, and this moment, the pH value was 3.5～4.5;
(d) decolouring
Hydrolyzed solution that above-mentioned washing is good adds with (a) gac of one-step hydrolysis total solid content equal in quality mark 5～50% and refluxed 2.0～4.0 hours, and heat decompression 650～700mmHg filters, and it is light yellow that filtrate is;
(e) depickling
The light yellow filtrate pH value that above-mentioned decolouring is good is 2.0～3.0, and residual a large amount of HCL in the filtrate, HCL adopt strong basicity or weakly alkaline phenylethylene, or weakly alkaline epoxy system or weakly alkaline acrylic resin exchange depickling by 1: 4～1: 8 ratio single stage method;
(f) concentrated, dry
Acid hydrolyzed casein pH value of solution value after resins exchange is 6.5～7.0, and solution is after concentrating, in pressure 15～30MPa, 120～160 ℃ of following spraying dryings of temperature, and it is milky white or faint yellow that products obtained therefrom is.
2. the production method of acid hydrolyzed casein according to claim 1, it is characterized in that the milk crude protein after described casein is with extraction butter is a main raw material, after impurity, pulverizing, dissolving, filtration, acidifying, washing, dehydration, dry purifying are removed in people's wage adjustment choosing, obtain.
3. the production method of acid hydrolyzed casein according to claim 1 is characterized in that described concentrated hydrochloric acid replaced by sulfuric acid.
4. according to the production method of claim 1 or 3 described acid hydrolyzed caseins, it is characterized in that described concentrated hydrochloric acid or sulfuric acid replaced by phosphoric acid.
5. the production method of acid hydrolyzed casein according to claim 1, it is characterized in that described strong basicity or weakly alkaline polystyrene show: 201 * 7 (717), D201, D202 (763), D301,709, weakly alkaline epoxy system has: 701 (331), and the weakly alkaline acrylic acid series has: 703 (D311), 705 (D313).
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| CN2007100182457A CN101095457B (en) | 2007-06-23 | 2007-06-23 | Method of producing acid hydrolyzed casein |
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| CN2007100182457A CN101095457B (en) | 2007-06-23 | 2007-06-23 | Method of producing acid hydrolyzed casein |
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| CN101095457B true CN101095457B (en) | 2010-04-07 |
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Families Citing this family (3)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN101824085B (en) * | 2010-04-09 | 2012-11-07 | 中国农业大学 | Method for separating alpha s-casein |
| CN108552404A (en) * | 2018-06-24 | 2018-09-21 | 甘肃农业大学 | A kind of pharmaceutical grade caseinhydrolysate and preparation method thereof |
| CN110526963A (en) * | 2019-09-24 | 2019-12-03 | 浙江工商大学 | A kind of non-enzymatic hydrolysis hypoallergenic casein preparation method for inhibiting antigen that submission is immunized |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1833031A (en) * | 2003-08-01 | 2006-09-13 | 卡尔皮斯株式会社 | Casein hydrolyzate, process for producing the same and use thereof |
| CN1931872A (en) * | 2006-09-27 | 2007-03-21 | 上海实业联合集团长城药业有限公司 | Casein hydrolysate and its prepn process |
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Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1833031A (en) * | 2003-08-01 | 2006-09-13 | 卡尔皮斯株式会社 | Casein hydrolyzate, process for producing the same and use thereof |
| CN1931872A (en) * | 2006-09-27 | 2007-03-21 | 上海实业联合集团长城药业有限公司 | Casein hydrolysate and its prepn process |
Non-Patent Citations (2)
| Title |
|---|
| 杨叶昆等.酪蛋白的酸水解及其棕色化反应产物在卷烟加香中的应用.烟草科技 2001年01期.2001,(2001年01期),8-10. |
| 杨叶昆等.酪蛋白的酸水解及其棕色化反应产物在卷烟加香中的应用.烟草科技 2001年01期.2001,(2001年01期),8-10. * |
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