CN117551014A - Purification method for preparing L-cystine - Google Patents
Purification method for preparing L-cystine Download PDFInfo
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- CN117551014A CN117551014A CN202311490591.0A CN202311490591A CN117551014A CN 117551014 A CN117551014 A CN 117551014A CN 202311490591 A CN202311490591 A CN 202311490591A CN 117551014 A CN117551014 A CN 117551014A
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- LEVWYRKDKASIDU-IMJSIDKUSA-N L-cystine Chemical compound [O-]C(=O)[C@@H]([NH3+])CSSC[C@H]([NH3+])C([O-])=O LEVWYRKDKASIDU-IMJSIDKUSA-N 0.000 title claims abstract description 112
- 235000019393 L-cystine Nutrition 0.000 title claims abstract description 112
- 239000004158 L-cystine Substances 0.000 title claims abstract description 112
- 229960003067 cystine Drugs 0.000 title claims abstract description 112
- 238000000746 purification Methods 0.000 title claims abstract description 35
- 238000000034 method Methods 0.000 title claims abstract description 18
- XUJNEKJLAYXESH-REOHCLBHSA-N L-Cysteine Chemical compound SC[C@H](N)C(O)=O XUJNEKJLAYXESH-REOHCLBHSA-N 0.000 claims abstract description 180
- 238000006243 chemical reaction Methods 0.000 claims abstract description 140
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims abstract description 96
- 235000013878 L-cysteine Nutrition 0.000 claims abstract description 90
- 239000004201 L-cysteine Substances 0.000 claims abstract description 90
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims abstract description 75
- IAZDPXIOMUYVGZ-UHFFFAOYSA-N Dimethylsulphoxide Chemical compound CS(C)=O IAZDPXIOMUYVGZ-UHFFFAOYSA-N 0.000 claims abstract description 66
- 239000011347 resin Substances 0.000 claims abstract description 36
- 229920005989 resin Polymers 0.000 claims abstract description 36
- 238000003756 stirring Methods 0.000 claims abstract description 32
- 238000001914 filtration Methods 0.000 claims abstract description 27
- 230000001105 regulatory effect Effects 0.000 claims abstract description 25
- 239000012295 chemical reaction liquid Substances 0.000 claims abstract description 23
- 230000035484 reaction time Effects 0.000 claims abstract description 18
- 239000000843 powder Substances 0.000 claims abstract description 15
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 claims abstract description 14
- 235000011114 ammonium hydroxide Nutrition 0.000 claims abstract description 14
- 230000000813 microbial effect Effects 0.000 claims abstract description 14
- 241001052560 Thallis Species 0.000 claims description 33
- 238000005406 washing Methods 0.000 claims description 28
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 22
- 239000012535 impurity Substances 0.000 claims description 22
- 238000001035 drying Methods 0.000 claims description 15
- 238000011068 loading method Methods 0.000 claims description 13
- 230000003472 neutralizing effect Effects 0.000 claims description 13
- 238000000926 separation method Methods 0.000 claims description 12
- 239000000126 substance Substances 0.000 claims description 12
- 150000001768 cations Chemical class 0.000 claims description 11
- 238000006911 enzymatic reaction Methods 0.000 claims description 11
- 238000010438 heat treatment Methods 0.000 claims description 11
- 238000002156 mixing Methods 0.000 claims description 11
- 238000004519 manufacturing process Methods 0.000 claims 4
- 239000013078 crystal Substances 0.000 abstract description 5
- 239000003814 drug Substances 0.000 abstract description 3
- 239000007788 liquid Substances 0.000 abstract 2
- 238000006386 neutralization reaction Methods 0.000 abstract 1
- 238000007254 oxidation reaction Methods 0.000 description 20
- 230000003647 oxidation Effects 0.000 description 12
- 239000011790 ferrous sulphate Substances 0.000 description 7
- 235000003891 ferrous sulphate Nutrition 0.000 description 7
- BAUYGSIQEAFULO-UHFFFAOYSA-L iron(2+) sulfate (anhydrous) Chemical compound [Fe+2].[O-]S([O-])(=O)=O BAUYGSIQEAFULO-UHFFFAOYSA-L 0.000 description 7
- 229910000359 iron(II) sulfate Inorganic materials 0.000 description 7
- 239000002994 raw material Substances 0.000 description 4
- 235000013305 food Nutrition 0.000 description 3
- 230000001590 oxidative effect Effects 0.000 description 3
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 3
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 2
- 230000003197 catalytic effect Effects 0.000 description 2
- 239000007800 oxidant agent Substances 0.000 description 2
- 230000001376 precipitating effect Effects 0.000 description 2
- 239000011541 reaction mixture Substances 0.000 description 2
- 238000004904 shortening Methods 0.000 description 2
- 238000007086 side reaction Methods 0.000 description 2
- 102000011782 Keratins Human genes 0.000 description 1
- 108010076876 Keratins Proteins 0.000 description 1
- 241000276425 Xiphophorus maculatus Species 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 239000000654 additive Substances 0.000 description 1
- 230000000996 additive effect Effects 0.000 description 1
- 239000003513 alkali Substances 0.000 description 1
- 239000000729 antidote Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 235000008429 bread Nutrition 0.000 description 1
- 150000001720 carbohydrates Chemical class 0.000 description 1
- 239000002537 cosmetic Substances 0.000 description 1
- 235000013365 dairy product Nutrition 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 229940079593 drug Drugs 0.000 description 1
- 239000003172 expectorant agent Substances 0.000 description 1
- 230000003419 expectorant effect Effects 0.000 description 1
- 239000003205 fragrance Substances 0.000 description 1
- 239000004519 grease Substances 0.000 description 1
- 238000010409 ironing Methods 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
- 102000004169 proteins and genes Human genes 0.000 description 1
- 108090000623 proteins and genes Proteins 0.000 description 1
- 238000005057 refrigeration Methods 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C319/00—Preparation of thiols, sulfides, hydropolysulfides or polysulfides
- C07C319/26—Separation; Purification; Stabilisation; Use of additives
- C07C319/28—Separation; Purification
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
The invention discloses a purification method for preparing L-cystine, which particularly relates to the technical field of biological medicine, wherein L-cystine reaction liquid is added into dimethyl sulfoxide which is equimolar with the L-cysteine reaction liquid to carry out greenhouse reaction, then sodium hydroxide is used for neutralization, crystal L-cystine is separated out by filtration, dimethyl sulfoxide is added and pH value is regulated when the L-cystine reaction liquid with low concentration is purified, stirring reaction is carried out again to obtain L-cystine conversion liquid, the L-cystine conversion liquid is loaded into a resin column and is fully washed and eluted by ammonia water, the pH value is regulated by hydrochloric acid, white powder is separated out, separated, washed and dried to obtain L-cystine, the pH value is reduced by adding hydrochloric acid to destroy microbial cells, meanwhile, the solubility of target products L-cysteine and L-cystine is increased, and the dimethyl sulfoxide can be used under the condition of low pH value without regulating the pH value, the reaction time is shortened, and the yield of L-cystine is further improved.
Description
Technical Field
The invention relates to the technical field of biological medicines, in particular to a purification method for preparing L-cystine.
Background
L-cystine is an organic substance, is white hexagonal platy crystal or white crystal powder, is dissolved in dilute acid and alkali solution, is extremely insoluble in water and insoluble in ethanol, exists in a small amount in protein, is contained in keratin such as hair, fingers and the like, is used as a raw material for producing antidote and expectorant in medicine, is used as a dairy additive and bread quick-acting promoter in the food industry, can generate various special fragrances after being heated with saccharides in food, can prevent grease from being oxidized, and has wide application in the food processing process; the cosmetic industry is a raw material for producing cold-ironing essence.
In the preparation process of L-cystine, the purification work is usually needed, at present, an oxidation method of oxidizing L-cysteine into L-cystine, and then carrying out electrolytic reduction after separation is mostly adopted, the traditional oxidation method is usually a direct air oxidation method or a ferrous sulfate catalytic oxidation method, the reaction time of the direct air oxidation method is long, if the oxidation time is insufficient, the yield is reduced, and ferrous sulfate belongs to a weak oxidant, and although the side reaction is less, the raw material consumption is less, the reaction time is long, the efficiency and the yield are low, and how to improve the purification yield of L-cystine is the problem which needs to be solved at present.
Disclosure of Invention
In order to overcome the defects in the prior art, the invention provides a purification method for preparing L-cystine, which aims to solve the technical problems that: the traditional oxidation method is usually a direct air oxidation method or a ferrous sulfate catalytic oxidation method, the reaction time of the direct air oxidation method is long, if the oxidation time is insufficient, the yield is reduced, and the ferrous sulfate belongs to a weak oxidant, and has the problems of less side reaction, less raw material consumption, long reaction time, low efficiency and low yield.
In order to achieve the above purpose, the present invention provides the following technical solutions: a purification method for preparing L-cystine comprises the following steps:
s1, centrifuging a solution containing L-cysteine to remove microbial enzyme reaction liquid of thalli, regulating the pH value of the obtained L-cysteine reaction liquid through hydrochloric acid, adding activated carbon, heating, and filtering out thalli and impurities;
s2, stirring and mixing the L-cysteine reaction solution with the thalli and impurities removed, simultaneously adding dimethyl sulfoxide which is equimolar with the L-cysteine reaction solution for greenhouse reaction, neutralizing with sodium hydroxide, and filtering to separate out crystalline L-cystine;
s3, adding dimethyl sulfoxide and adjusting the pH value when purifying the low-concentration L-cysteine reaction solution, and then stirring for reaction to obtain an L-cystine conversion solution;
s4, loading the L-cystine conversion solution to a resin column, fully washing, eluting with ammonia water, adjusting the pH value by hydrochloric acid, separating out white powder, separating, washing and drying to obtain L-cystine, wherein the L-cystine obtained at present and the L-cystine crystallized in S2 are the same purified substances, and thus the purpose of separation and purification is achieved.
As a further aspect of the invention: in the step S1, the mass fraction of the L-cysteine reaction solution is controlled to be 8-10%, and the pH value of the L-cysteine reaction solution is adjusted to be 1 by hydrochloric acid.
As a further aspect of the invention: in the step S2, the greenhouse reaction time is controlled to be 7.5-8.5 hours, and sodium hydroxide is utilized to neutralize to pH 5.
As a further aspect of the invention: in the step S3, the mass concentration of the low-concentration L-cysteine reaction solution is 3.1-3.3g/L, the mass fraction of the added dimethyl sulfoxide is 1-3%, the pH value is regulated to be 1, and the stirring reaction time is controlled to be 6.5-7.5h.
As a further aspect of the invention: in the step S4, the resin column is a 001 multiplied by 7 cation resin column, and the pH value is adjusted to 5.0 by hydrochloric acid.
The invention has the beneficial effects that: adding dimethyl sulfoxide which is equimolar with the L-cysteine reaction solution into the L-cysteine reaction solution for greenhouse reaction, neutralizing by sodium hydroxide, filtering and separating out crystalline L-cystine, adding dimethyl sulfoxide and regulating the pH value when purifying the low-concentration L-cysteine reaction solution, stirring and reacting to obtain the L-cystine conversion solution, loading the L-cystine conversion solution into a resin column, fully washing, eluting by ammonia water, regulating the pH value by hydrochloric acid, separating out white powder, separating, washing and drying to obtain the L-cystine, reducing the pH value by adding hydrochloric acid to destroy microbial cells, increasing the solubility of target products L-cystine and L-cystine, using the dimethyl sulfoxide under the condition of low pH value, shortening the reaction time, and further improving the purification yield of the L-cystine.
Detailed Description
The following description of the technical solutions in the embodiments of the present invention will be clear and complete, and it is obvious that the described embodiments are only some embodiments of the present invention, but not all embodiments. All other embodiments, which can be made by those skilled in the art based on the embodiments of the invention without making any inventive effort, are intended to be within the scope of the invention.
The invention provides a purification method for preparing L-cystine, which comprises the following steps:
s1, centrifuging a solution containing L-cysteine to remove microbial enzyme reaction liquid of thalli, regulating the pH value of the obtained L-cysteine reaction liquid through hydrochloric acid, adding activated carbon, heating, and filtering out thalli and impurities;
s2, stirring and mixing the L-cysteine reaction solution with the thalli and impurities removed, simultaneously adding dimethyl sulfoxide which is equimolar with the L-cysteine reaction solution for greenhouse reaction, neutralizing with sodium hydroxide, and filtering to separate out crystalline L-cystine;
s3, adding dimethyl sulfoxide and adjusting the pH value when purifying the low-concentration L-cysteine reaction solution, and then stirring for reaction to obtain an L-cystine conversion solution;
s4, loading the L-cystine conversion solution to a resin column, fully washing, eluting with ammonia water, adjusting the pH value by hydrochloric acid, separating out white powder, separating, washing and drying to obtain L-cystine, wherein the L-cystine obtained at present and the L-cystine crystallized in S2 are the same purified substances, and thus the purpose of separation and purification is achieved.
In S1, the mass fraction of the L-cysteine reaction solution is controlled to be 8-10%, and the pH value of the L-cysteine reaction solution is adjusted to be 1 by hydrochloric acid.
In S2, the time of the greenhouse reaction is controlled to be 7.5-8.5 hours, and sodium hydroxide is utilized to neutralize to pH 5.
In S3, the mass concentration of the low-concentration L-cysteine reaction solution is 3.1-3.3g/L, the mass fraction of the dimethyl sulfoxide is 1-3%, the pH value is regulated to 1, and the stirring reaction time is controlled to be 6.5-7.5h.
In S4, the resin column is a 001×7 cation resin column, and the pH value is adjusted to 5.0 by hydrochloric acid.
Example 1:
s1, centrifuging a solution containing L-cysteine to remove microbial enzyme reaction liquid of thalli, regulating the pH value of the obtained L-cysteine reaction liquid through hydrochloric acid, adding activated carbon, heating, and filtering out thalli and impurities;
in S1, the mass fraction of the L-cysteine reaction solution is controlled to be 10%, and the pH value of the L-cysteine reaction solution is adjusted to be 1 by hydrochloric acid.
S2, stirring and mixing the L-cysteine reaction solution with the thalli and impurities removed, simultaneously adding dimethyl sulfoxide which is equimolar with the L-cysteine reaction solution for greenhouse reaction, neutralizing with sodium hydroxide, and filtering to separate out crystalline L-cystine;
in S2, the time of the greenhouse reaction is controlled to be 8 hours, and sodium hydroxide is utilized to neutralize to pH 5.
S3, adding dimethyl sulfoxide and adjusting the pH value when purifying the low-concentration L-cysteine reaction solution, and then stirring for reaction to obtain an L-cystine conversion solution;
in S3, the mass concentration of the low-concentration L-cysteine reaction solution is 3.2g/L, the mass fraction of the added dimethyl sulfoxide is 2.5%, the pH value is regulated to be 1, and the stirring reaction time is controlled to be 7h.
S4, loading the L-cystine conversion solution to a resin column, fully washing, eluting with ammonia water, adjusting the pH value by hydrochloric acid, separating out white powder, separating, washing and drying to obtain L-cystine, wherein the L-cystine obtained at present and the L-cystine crystallized in S2 are the same purified substances, and thus the purpose of separation and purification is achieved;
in S4, the resin column is a 001×7 cation resin column, and the pH value is adjusted to 5.0 by hydrochloric acid.
In conclusion, the conversion rate of the oxidation reaction is 97%, and the purification yield of the L-cystine is 98%.
Example 2:
s1, centrifuging a solution containing L-cysteine to remove microbial enzyme reaction liquid of thalli, regulating the pH value of the obtained L-cysteine reaction liquid through hydrochloric acid, adding activated carbon, heating, and filtering out thalli and impurities;
in S1, the mass fraction of the L-cysteine reaction solution is controlled to be 8%, and the pH value of the L-cysteine reaction solution is adjusted to be 1 by hydrochloric acid.
S2, stirring and mixing the L-cysteine reaction solution with the thalli and impurities removed, simultaneously adding dimethyl sulfoxide which is equimolar with the L-cysteine reaction solution for greenhouse reaction, neutralizing with sodium hydroxide, and filtering to separate out crystalline L-cystine;
in S2, the time of the greenhouse reaction is controlled at 8.5h, and the reaction mixture is neutralized to pH 5 by sodium hydroxide.
S3, adding dimethyl sulfoxide and adjusting the pH value when purifying the low-concentration L-cysteine reaction solution, and then stirring for reaction to obtain an L-cystine conversion solution;
in S3, the mass concentration of the low-concentration L-cysteine reaction solution is 3.0g/L, the mass fraction of the dimethyl sulfoxide is 2%, the pH value is regulated to 1, and the stirring reaction time is controlled to be 7h.
S4, loading the L-cystine conversion solution to a resin column, fully washing, eluting with ammonia water, adjusting the pH value by hydrochloric acid, separating out white powder, separating, washing and drying to obtain L-cystine, wherein the L-cystine obtained at present and the L-cystine crystallized in S2 are the same purified substances, and thus the purpose of separation and purification is achieved;
in S4, the resin column is a 001×7 cation resin column, and the pH value is adjusted to 5.0 by hydrochloric acid.
In conclusion, the conversion rate of the oxidation reaction is 96%, and the purification yield of the L-cystine is 96.3%.
Example 3:
s1, centrifuging a solution containing L-cysteine to remove microbial enzyme reaction liquid of thalli, regulating the pH value of the obtained L-cysteine reaction liquid through hydrochloric acid, adding activated carbon, heating, and filtering out thalli and impurities;
in S1, the mass fraction of the L-cysteine reaction solution is controlled to be 9%, and the pH value of the L-cysteine reaction solution is adjusted to be 1 by hydrochloric acid.
S2, stirring and mixing the L-cysteine reaction solution with the thalli and impurities removed, simultaneously adding dimethyl sulfoxide which is equimolar with the L-cysteine reaction solution for greenhouse reaction, neutralizing with sodium hydroxide, and filtering to separate out crystalline L-cystine;
in S2, the time of the greenhouse reaction is controlled at 8.5h, and the reaction mixture is neutralized to pH 5 by sodium hydroxide.
S3, adding dimethyl sulfoxide and adjusting the pH value when purifying the low-concentration L-cysteine reaction solution, and then stirring for reaction to obtain an L-cystine conversion solution;
in S3, the mass concentration of the low-concentration L-cysteine reaction solution is 3.3g/L, the mass fraction of the added dimethyl sulfoxide is 3%, the pH value is regulated to be 1, and the stirring reaction time is controlled to be 7.3h.
S4, loading the L-cystine conversion solution to a resin column, fully washing, eluting with ammonia water, adjusting the pH value by hydrochloric acid, separating out white powder, separating, washing and drying to obtain L-cystine, wherein the L-cystine obtained at present and the L-cystine crystallized in S2 are the same purified substances, and thus the purpose of separation and purification is achieved;
in S4, the resin column is a 001×7 cation resin column, and the pH value is adjusted to 5.0 by hydrochloric acid.
In conclusion, the conversion rate of the oxidation reaction is 93%, and the purification yield of the L-cystine is 91.6%.
Example 4:
s1, centrifuging a solution containing L-cysteine to remove microbial enzyme reaction liquid of thalli, regulating the pH value of the obtained L-cysteine reaction liquid through hydrochloric acid, adding activated carbon, heating, and filtering out thalli and impurities;
in S1, the mass fraction of the L-cysteine reaction solution is controlled to be 8%, and the pH value of the L-cysteine reaction solution is adjusted to be 1 by hydrochloric acid.
S2, stirring and mixing the L-cysteine reaction solution with the thalli and impurities removed, simultaneously adding dimethyl sulfoxide which is equimolar with the L-cysteine reaction solution for greenhouse reaction, neutralizing with sodium hydroxide, and filtering to separate out crystalline L-cystine;
in S2, the time of the greenhouse reaction is controlled at 7h, and the reaction solution is neutralized to pH 5 by sodium hydroxide.
S3, adding dimethyl sulfoxide and adjusting the pH value when purifying the low-concentration L-cysteine reaction solution, and then stirring for reaction to obtain an L-cystine conversion solution;
in S3, the mass concentration of the low-concentration L-cysteine reaction solution is 3.1g/L, the mass fraction of the dimethyl sulfoxide is 1%, the pH value is regulated to 1, and the stirring reaction time is controlled to be 6.8h.
S4, loading the L-cystine conversion solution to a resin column, fully washing, eluting with ammonia water, adjusting the pH value by hydrochloric acid, separating out white powder, separating, washing and drying to obtain L-cystine, wherein the L-cystine obtained at present and the L-cystine crystallized in S2 are the same purified substances, and thus the purpose of separation and purification is achieved;
in S4, the resin column is a 001×7 cation resin column, and the pH value is adjusted to 5.0 by hydrochloric acid.
In conclusion, the conversion rate of the oxidation reaction is 95.5%, and the purification yield of the L-cystine is 92%.
Example 5:
s1, centrifuging a solution containing L-cysteine to remove microbial enzyme reaction liquid of thalli, regulating the pH value of the obtained L-cysteine reaction liquid through hydrochloric acid, adding activated carbon, heating, and filtering out thalli and impurities;
in S1, the mass fraction of the L-cysteine reaction solution is controlled to be 8.5%, and the pH value of the L-cysteine reaction solution is adjusted to be 1 by hydrochloric acid.
S2, stirring and mixing the L-cysteine reaction solution with the thalli and impurities removed, simultaneously adding dimethyl sulfoxide which is equimolar with the L-cysteine reaction solution for greenhouse reaction, neutralizing with sodium hydroxide, and filtering to separate out crystalline L-cystine;
in S2, the time of the greenhouse reaction is controlled at 7h, and the reaction solution is neutralized to pH 5 by sodium hydroxide.
S3, adding dimethyl sulfoxide and adjusting the pH value when purifying the low-concentration L-cysteine reaction solution, and then stirring for reaction to obtain an L-cystine conversion solution;
in S3, the mass concentration of the low-concentration L-cysteine reaction solution is 3.25g/L, the mass fraction of the added dimethyl sulfoxide is 2%, the pH value is regulated to be 1, and the stirring reaction time is controlled to be 6.8h.
S4, loading the L-cystine conversion solution to a resin column, fully washing, eluting with ammonia water, adjusting the pH value by hydrochloric acid, separating out white powder, separating, washing and drying to obtain L-cystine, wherein the L-cystine obtained at present and the L-cystine crystallized in S2 are the same purified substances, and thus the purpose of separation and purification is achieved;
in S4, the resin column is a 001×7 cation resin column, and the pH value is adjusted to 5.0 by hydrochloric acid.
In summary, the conversion rate of the oxidation reaction is 94.8%, and the purification yield of the L-cystine is 90.5%.
Example 6:
s1, centrifuging a solution containing L-cysteine to remove microbial enzyme reaction liquid of thalli, adding activated carbon, heating, and filtering out thalli and impurities;
in S1, the mass fraction of the L-cysteine reaction solution is controlled to be 10%, and the pH value of the L-cysteine reaction solution is adjusted to be 1 by hydrochloric acid.
S2, stirring and mixing the L-cysteine reaction solution with the thalli and impurities removed, carrying out greenhouse reaction, neutralizing with sodium hydroxide, and filtering to separate out crystalline L-cystine;
in S2, the time of the greenhouse reaction is controlled to be 24 hours, and the reaction is neutralized to pH 5 by sodium hydroxide.
S3, when the low-concentration L-cysteine reaction solution is purified, precipitating crystals, filtering, washing with water and drying to obtain the L-cystine conversion solution.
S4, loading the L-cystine conversion solution to a resin column, fully washing, eluting with ammonia water, adjusting the pH value by hydrochloric acid, separating out white powder, separating, washing and drying to obtain L-cystine, wherein the L-cystine obtained at present and the L-cystine crystallized in S2 are the same purified substances, and thus the purpose of separation and purification is achieved;
in S4, the resin column is a 001×7 cation resin column, and the pH value is adjusted to 5.0 by hydrochloric acid.
In conclusion, the conversion rate of the oxidation reaction is 39%, and the purification yield of the L-cystine is 37.2%.
Example 7:
s1, centrifuging a solution containing L-cysteine to remove microbial enzyme reaction liquid of thalli, adding activated carbon, heating, and filtering out thalli and impurities;
in S1, the mass fraction of the L-cysteine reaction solution is controlled to be 8%, and the pH value of the L-cysteine reaction solution is adjusted to be 1 by hydrochloric acid.
S2, stirring and mixing the L-cysteine reaction solution with the thalli and impurities removed, carrying out greenhouse reaction, neutralizing with sodium hydroxide, and filtering to separate out crystalline L-cystine;
in S2, the time of the greenhouse reaction is controlled to be 15h, and sodium hydroxide is utilized to neutralize to pH 5.
S3, when the low-concentration L-cysteine reaction solution is purified, introducing air in an amount of 2.5L/min, reacting for 14 hours, precipitating crystals, filtering, washing with water, and drying to obtain the L-cystine conversion solution.
S4, loading the L-cystine conversion solution to a resin column, fully washing, eluting with ammonia water, adjusting the pH value by hydrochloric acid, separating out white powder, separating, washing and drying to obtain L-cystine, wherein the L-cystine obtained at present and the L-cystine crystallized in S2 are the same purified substances, and thus the purpose of separation and purification is achieved;
in S4, the resin column is a 001×7 cation resin column, and the pH value is adjusted to 5.0 by hydrochloric acid.
In conclusion, the conversion rate of the oxidation reaction is 48%, and the purification yield of the L-cystine is 45%.
Example 8:
s1, centrifuging a solution containing L-cysteine to remove microbial enzyme reaction liquid of thalli, regulating the pH value of the obtained L-cysteine reaction liquid through hydrochloric acid, adding activated carbon, heating, and filtering out thalli and impurities;
the pH of the L-cysteine reaction solution was adjusted to 1 by hydrochloric acid.
S2, stirring and mixing the L-cysteine reaction solution with the thalli and impurities removed, simultaneously adding ferrous sulfate with the same mole as the L-cysteine reaction solution for greenhouse reaction, neutralizing with sodium hydroxide, and filtering to separate out crystalline L-cystine;
in S2, the time of the greenhouse reaction is controlled to be 10 hours, and the reaction is neutralized to pH 5 by sodium hydroxide.
S3, when purifying the low-concentration L-cysteine reaction solution, adding ferrous sulfate, placing the solution on a reciprocating shaking table for overnight oxidation, vacuum concentrating, placing the solution in a refrigerator for refrigeration overnight, adjusting the pH value, and stirring the solution for reaction to obtain a conversion solution of L-cystine;
in S3, the mass concentration of the low-concentration L-cysteine reaction solution is 3.3g/L, the mass fraction of the added ferrous sulfate is 5%, the pH value is regulated to be 1, and the stirring reaction time is controlled to be 9h.
S4, loading the L-cystine conversion solution to a resin column, fully washing, eluting with ammonia water, adjusting the pH value by hydrochloric acid, separating out white powder, separating, washing and drying to obtain L-cystine, wherein the L-cystine obtained at present and the L-cystine crystallized in S2 are the same purified substances, and thus the purpose of separation and purification is achieved;
in S4, the resin column is a 001×7 cation resin column, and the pH value is adjusted to 5.0 by hydrochloric acid.
In conclusion, the conversion rate of the oxidation reaction is 78.5%, and the purification yield of the L-cystine is 73%.
From the above, the present invention is as follows: adding dimethyl sulfoxide which is equimolar with the L-cysteine reaction solution into the L-cysteine reaction solution for greenhouse reaction, neutralizing by sodium hydroxide, filtering and separating out crystalline L-cystine, adding dimethyl sulfoxide and regulating the pH value when purifying the low-concentration L-cysteine reaction solution, stirring and reacting to obtain the L-cystine conversion solution, loading the L-cystine conversion solution into a resin column, fully washing, eluting by ammonia water, regulating the pH value by hydrochloric acid, separating out white powder, separating, washing and drying to obtain the L-cystine, reducing the pH value by adding hydrochloric acid to destroy microbial cells, increasing the solubility of target products L-cystine and L-cystine, using the dimethyl sulfoxide under the condition of low pH value, shortening the reaction time, and further improving the purification yield of the L-cystine.
The last points to be described are: while the invention has been described in detail in the foregoing general description and with reference to specific embodiments, the foregoing embodiments are merely illustrative of the technical aspects of the invention and are not limiting thereof; although the invention has been described in detail with reference to the foregoing embodiments, it will be understood by those of ordinary skill in the art that: the technical scheme described in the foregoing embodiments can be modified or some or all of the technical features thereof can be replaced by equivalents; such modifications and substitutions do not depart from the spirit of the invention.
Claims (5)
1. A purification method for preparing L-cystine, comprising the steps of:
s1, centrifuging a solution containing L-cysteine to remove microbial enzyme reaction liquid of thalli, regulating the pH value of the obtained L-cysteine reaction liquid through hydrochloric acid, adding activated carbon, heating, and filtering out thalli and impurities;
s2, stirring and mixing the L-cysteine reaction solution with the thalli and impurities removed, simultaneously adding dimethyl sulfoxide which is equimolar with the L-cysteine reaction solution for greenhouse reaction, neutralizing with sodium hydroxide, and filtering to separate out crystalline L-cystine;
s3, adding dimethyl sulfoxide and adjusting the pH value when purifying the low-concentration L-cysteine reaction solution, and then stirring for reaction to obtain an L-cystine conversion solution;
s4, loading the L-cystine conversion solution to a resin column, fully washing, eluting with ammonia water, adjusting the pH value by hydrochloric acid, separating out white powder, separating, washing and drying to obtain L-cystine, wherein the L-cystine obtained at present and the L-cystine crystallized in S2 are the same purified substances, and thus the purpose of separation and purification is achieved.
2. The purification method for producing L-cystine according to claim 1, wherein: in the step S1, the mass fraction of the L-cysteine reaction solution is controlled to be 8-10%, and the pH value of the L-cysteine reaction solution is adjusted to be 1 by hydrochloric acid.
3. The purification method for producing L-cystine according to claim 1, wherein: in the step S2, the greenhouse reaction time is controlled to be 7.5-8.5 hours, and sodium hydroxide is utilized to neutralize to pH 5.
4. The purification method for producing L-cystine according to claim 1, wherein: in the step S3, the mass concentration of the low-concentration L-cysteine reaction solution is 3.1-3.3g/L, the mass fraction of the added dimethyl sulfoxide is 1-3%, the pH value is regulated to be 1, and the stirring reaction time is controlled to be 6.5-7.5h.
5. The purification method for producing L-cystine according to claim 1, wherein: in the step S4, the resin column is a 001 multiplied by 7 cation resin column, and the pH value is adjusted to 5.0 by hydrochloric acid.
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