CN110903680B - Low-salt purification method of edible colorant - Google Patents
Low-salt purification method of edible colorant Download PDFInfo
- Publication number
- CN110903680B CN110903680B CN201911339673.9A CN201911339673A CN110903680B CN 110903680 B CN110903680 B CN 110903680B CN 201911339673 A CN201911339673 A CN 201911339673A CN 110903680 B CN110903680 B CN 110903680B
- Authority
- CN
- China
- Prior art keywords
- chloride
- salt
- stirring
- mixture
- barium
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Expired - Fee Related
Links
Classifications
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09B—ORGANIC DYES OR CLOSELY-RELATED COMPOUNDS FOR PRODUCING DYES, e.g. PIGMENTS; MORDANTS; LAKES
- C09B67/00—Influencing the physical, e.g. the dyeing or printing properties of dyestuffs without chemical reactions, e.g. by treating with solvents grinding or grinding assistants, coating of pigments or dyes; Process features in the making of dyestuff preparations; Dyestuff preparations of a special physical nature, e.g. tablets, films
- C09B67/0096—Purification; Precipitation; Filtration
Landscapes
- Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Organic Chemistry (AREA)
- Coloring Foods And Improving Nutritive Qualities (AREA)
Abstract
The invention discloses a low-salt purification method of edible pigment, which comprises the following steps: adding concentrated acid into the pigment reaction solution, adjusting the pH value of the reaction solution to 4.0-4.5, stirring and heating to 55-65 ℃; under the stirring state, adding mixed salt according to 3-7% of the volume of the reaction solution, stirring until the salt is dissolved, stopping stirring, cooling to 25-55 ℃, standing and crystallizing until the material is clear. The invention reduces the salt consumption of the traditional salting-out process by using the mixed salt, thereby achieving the effects of reducing the salt consumption and reducing the final solid waste of the wastewater. The effect of reducing 60-70% of salt dosage for salting out and reducing 50-60% of final process solid waste is achieved by adjusting the pH value of the pigment coupling liquid and mixing calcium chloride, barium chloride and sodium chloride for purifying the pigment.
Description
Technical Field
The invention belongs to a pigment purification process, and particularly relates to a low-salt purification method of an edible pigment.
Background
In the production process of the traditional synthetic edible pigment, a coupling solution of the pigment is obtained after diazotization reaction and coupling reaction, the coupling solution contains impurities such as unreacted intermediates, side reaction products and the like, and in order to obtain a product meeting the national standard, the reaction solution needs to be purified to obtain a solid pigment product meeting the requirements of purity and impurities.
In the purification method in the prior art, a large amount of sodium chloride is added to improve the concentration of sodium ions in the coupling liquid, and the pigment sodium salt crystals are separated out in a solid state by utilizing the same ion effect, so that a product meeting the requirements is obtained.
Because the molecular structure of the edible pigment has hydrophilicity and the nucleation of the edible pigment is difficult, in order to ensure that the pigment can be well crystallized in the purification process, the purification method in the prior art needs to greatly improve the supersaturation degree, and the added sodium chloride has extremely high dosage. The mother liquor after purification contains a large amount of sodium chloride and generates a large amount of production wastewater, and the wastewater becomes a large amount of solid waste through evaporation treatment, so that the cost and the pressure of environmental protection treatment are greatly increased.
Therefore, how to design a purification method with low salt dosage is very necessary to reduce the environmental protection and cost pressure.
Disclosure of Invention
In order to overcome the above-mentioned drawbacks of the prior art, the object of the present invention is to provide a method for low-salt purification of food colors.
The method can greatly reduce the salt dosage, salt precipitation purification is carried out by using mixed salt, the formation of crystal nucleus is accelerated by the water insolubility of calcium salt/barium salt, and then the crystallization process is controlled under low salinity to obtain the pigment crystal with the quality meeting the product requirement.
In order to realize one of the purposes of the invention, the adopted technical scheme is as follows:
a method for low-salt purification of food color comprises the following steps:
the method comprises the following steps: adding concentrated acid into the pigment reaction solution, adjusting the pH value of the reaction solution to 4.0-4.5, stirring and heating to 55-65 ℃;
step two: under the stirring state, adding mixed salt according to 3-7% of the volume of the reaction solution, stirring until the salt is dissolved, stopping stirring, cooling to 25-55 ℃, standing and crystallizing until the material is clear, wherein the added mixed salt comprises any one or more of a mixture of calcium chloride and sodium chloride, a mixture of barium chloride and sodium chloride, calcium chloride and a mixture of barium chloride and potassium chloride.
In a preferred embodiment of the invention, the pigment comprises any one or more of carmine, allura red, amaranth, sunset yellow, tartrazine or indigo.
In a preferred embodiment of the invention, the concentrated acid is any one or more of hydrochloric acid or sulfuric acid.
In a preferred embodiment of the present invention, the elevated temperature is 60 ℃.
In a preferred embodiment of the invention, the mixed salt is a mixture of calcium chloride and sodium chloride.
In a preferred embodiment of the present invention, the mixture of calcium chloride and sodium chloride is mixed in the following ratio: 0.2 percent of calcium chloride and 99.8 percent of sodium chloride.
In a preferred embodiment of the invention, the mixed salt is a mixture of barium chloride and potassium chloride.
In a preferred embodiment of the present invention, the mixture of barium chloride and potassium chloride is mixed in the following ratio: 0.2 percent of barium chloride and 99.8 percent of potassium chloride.
In a preferred embodiment of the present invention, the temperature-reduced purification temperature is 35-55 ℃.
In a preferred embodiment of the invention, the stirring until the salt is dissolved is 30 minutes after the mixed salt is added.
The invention has the beneficial effects that:
the invention reduces the salt consumption of the traditional salting-out process by using the mixed salt, thereby achieving the effects of reducing the salt consumption and reducing the final solid waste of the wastewater.
The effect of reducing 60-70% of salt dosage for salting out and reducing 50-60% of final process solid waste is achieved by adjusting the pH value of the pigment coupling liquid and mixing calcium chloride, barium chloride and sodium chloride for purifying the pigment.
Detailed Description
The invention is further described with reference to the following examples:
example 1:
9000L of edible colorant carmine is placed in a 12000L preparation pot, stirring is started, 150kg of hydrochloric acid is added, the pH value of the solution is adjusted to 4.2, the temperature is raised to 60 ℃, 450 kg of mixed salt (calcium chloride (0.2%) + sodium chloride (99.8%)) is added, stirring is carried out for 30 minutes, then heat preservation and standing are carried out for 12 hours at the temperature of 35-38 ℃, after the materials are separated out and cleaned, the materials are added into a filter for filter pressing, and after the filter pressing is finished, the waste water is evaporated to obtain 900 kg of final solid waste.
Example 2:
luring 9000L of edible colorant in a 12000L preparation pot, starting stirring, adding 180kg of hydrochloric acid, adjusting the pH value of the solution to 4.0, heating to 60 ℃, adding 500 kg of mixed salt (barium chloride (0.2%) + sodium chloride (99.8%)), stirring for 30 minutes, keeping the temperature and standing for 12 hours at 40-45 ℃, adding a filter for filter pressing after the materials are separated out, and evaporating the wastewater after the filter pressing to obtain 1000 kg of final solid waste.
Example 3:
9000L of edible colorant indigo blue is put into a 12000L preparation pot, stirring is started, 100kg of sulfuric acid is added, the pH value of the solution is adjusted to 4.0, the temperature is raised to 55 ℃, 480 kg of mixed salt (barium chloride (0.2%) + potassium chloride (99.8%)) is added, stirring is carried out for 30 minutes, then heat preservation and standing are carried out for 12 hours at the temperature of 40-43 ℃, after the materials are separated out, the materials are added into a filter for filter pressing, and after the filter pressing is finished, the waste water is evaporated to obtain 950 kg of final solid waste.
Example 4:
9000L of edible colorant amaranth is placed in a 12000L preparation pot, stirring is started, 120kg of hydrochloric acid is added, the pH value of the solution is adjusted to 4.5, the temperature is raised to 60 ℃, 600 kg of mixed salt (calcium chloride (1.0%) + potassium chloride (99.0%)) is added, stirring is carried out for 30 minutes, then heat preservation and standing are carried out for 12 hours at the temperature of 50-55 ℃, after the materials are separated out, the materials are added into a filter for filter pressing, and after the filter pressing is finished, the waste water is evaporated to obtain 1200 kg of final solid waste.
Example 5:
9000L of edible colorant sunset yellow is placed in a 12000L preparation pot, stirring is started, 150kg of hydrochloric acid is added, the pH value of the solution is adjusted to 4.3, the temperature is raised to 60 ℃, 300 kg of mixed salt (calcium chloride (0.1%) + barium chloride (0.1%) + potassium chloride (99.8%)) is added, the mixture is stirred for 30 minutes, the mixture is kept at the temperature of between 35 and 38 ℃ and stands for 12 hours, the mixture is added into a filter for filter pressing after being separated and cleaned, and the waste water is evaporated to obtain 800 kg of final solid waste after the filter pressing is finished.
Example 6:
9000L of edible colorant lemon yellow is placed in a 12000L preparation pot, stirring is started, 145kg of hydrochloric acid is added, the pH value of the solution is adjusted to 4.3, the temperature is raised to 60 ℃, 300 kg of mixed salt (calcium chloride (0.1%) + barium chloride (0.1%) + sodium chloride (99.8%)) is added, stirring is carried out for 30 minutes, heat preservation and standing are carried out at 35-40 ℃ for 12 hours, after the materials are clarified, the materials are added into a filter for filter pressing, and after the filter pressing is finished, the waste water is evaporated to obtain 840 kg of final solid waste.
Comparative example 1:
comparative example 1 is a prior art salting-out comparative example:
9000L of edible colorant carmine is put into a 12000L preparation pot, stirring is started, 150kg of hydrochloric acid is added, the pH value of the solution is adjusted to 4.2, the temperature is raised to 60 ℃, 1500 kg of sodium chloride is added, stirring is carried out for 30 minutes, heat preservation and standing are carried out for 5 hours at 35-38 ℃, the materials are separated out and cleaned, then the materials are added into a filter for filter pressing, and after the filter pressing is finished, the waste water is evaporated to obtain 2000 kg of final solid waste.
Compared with the example 1, the same weight of edible color carmine is prepared, 1500 kg of sodium chloride is needed in the prior art, only 450 kg of mixed salt is needed in the example 1 of the invention, and the solid waste is far lower than that in the comparative example.
Comparative example 2:
9000L of edible colorant indigo blue is put into a 12000L preparation pot, stirring is started, 100kg of hydrochloric acid is added, the pH value of the solution is adjusted to 4.0, the temperature is raised to 60 ℃, 2200 kg of sodium chloride is added, stirring is carried out for 30 minutes, heat preservation and standing are carried out for 4 hours at 40-43 ℃, the materials are added into a filter for filter pressing after being clarified, and after the filter pressing is finished, the waste water is evaporated to obtain 2500 kg of final solid waste.
Compared with example 3, when the edible colorant indigo blue with the same weight is prepared, 2200 kg of sodium chloride is needed in the prior art, only 480 kg of mixed salt is needed in example 3, and the solid waste is far lower than that in the comparative example.
In conclusion, the invention achieves the effects of reducing 60-70% of salt dosage for salting out and reducing 50-60% of final process solid waste by adjusting the pH value of the pigment coupling liquid and mixing calcium chloride, barium chloride and sodium chloride for purifying the pigment.
Claims (4)
1. A method for low-salt purification of food pigments is characterized by comprising the following steps:
the method comprises the following steps: adding concentrated acid into the pigment reaction solution, adjusting the pH value of the reaction solution to 4.0-4.5, stirring and heating to 55-65 ℃;
step two: under the stirring state, adding mixed salt according to 3% -7% of the volume of the reaction solution, stirring until the salt is dissolved, stopping stirring, cooling to 35-55 ℃, standing and crystallizing until the material is clear, wherein the added mixed salt comprises any one of a mixture of calcium chloride and sodium chloride, a mixture of barium chloride and potassium chloride, a mixture of calcium chloride, barium chloride and sodium chloride, and a mixture of calcium chloride, barium chloride and potassium chloride;
the pigment comprises any one of carmine, allura red, amaranth, sunset yellow, lemon yellow or indigo blue;
the mixing proportion of the mixture of the calcium chloride and the sodium chloride is as follows: 0.2 percent of calcium chloride and 99.8 percent of sodium chloride;
the mixing proportion of the mixture of the barium chloride and the potassium chloride is as follows: 0.2% of barium chloride and 99.8% of potassium chloride;
the mixing proportion of the mixture of the barium chloride and the sodium chloride is as follows: 0.2% of barium chloride and 99.8% of sodium chloride;
the mixing ratio of the calcium chloride to the mixture of the barium chloride and the sodium chloride is as follows: 0.1% of calcium chloride, 0.1% of barium chloride and 99.8% of sodium chloride;
the mixing proportion of the calcium chloride and the mixture of the barium chloride and the potassium chloride is as follows: 0.1% of calcium chloride, 0.1% of barium chloride and 99.8% of potassium chloride.
2. The method for low-salt purification of food colors according to claim 1, wherein the concentrated acid is any one or more of hydrochloric acid or sulfuric acid.
3. The method for low-salt purification of food colors according to claim 1, wherein the elevated temperature is 60 ℃.
4. The method for low-salt purification of food colors according to claim 1, wherein the stirring until the salt is dissolved is stirring for 30 minutes after adding the mixed salt.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201911339673.9A CN110903680B (en) | 2019-12-23 | 2019-12-23 | Low-salt purification method of edible colorant |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201911339673.9A CN110903680B (en) | 2019-12-23 | 2019-12-23 | Low-salt purification method of edible colorant |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN110903680A CN110903680A (en) | 2020-03-24 |
| CN110903680B true CN110903680B (en) | 2021-09-03 |
Family
ID=69827455
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201911339673.9A Expired - Fee Related CN110903680B (en) | 2019-12-23 | 2019-12-23 | Low-salt purification method of edible colorant |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN110903680B (en) |
Families Citing this family (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112111171B (en) * | 2020-09-21 | 2022-04-08 | 恒升化工有限公司 | C.I. acid yellow 23 dye and clean production process thereof |
| CN112625463B (en) * | 2020-12-22 | 2022-08-26 | 上海染料研究所有限公司 | Salting-out refining method for synthetic edible pigment |
Citations (11)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS58198567A (en) * | 1982-05-13 | 1983-11-18 | Sumitomo Chem Co Ltd | Bifunctional reactive compound |
| CN1052492A (en) * | 1988-10-20 | 1991-06-26 | 山道士有限公司 | fiber-reactive azo dyes |
| CN1973001A (en) * | 2004-06-23 | 2007-05-30 | 日本化药株式会社 | Azo compound, ink composition, and colored object |
| CN101248141A (en) * | 2005-09-15 | 2008-08-20 | 日本化药株式会社 | Azo compound, ink composition, recording method, and colored object |
| CN100569862C (en) * | 2004-04-09 | 2009-12-16 | 日本化药株式会社 | Azo-compound, ink composite and colouring agent |
| CN101817772A (en) * | 2009-12-09 | 2010-09-01 | 兰州理工大学 | Method for preparing lutein by using marigold |
| CN102295839A (en) * | 2011-06-29 | 2011-12-28 | 新疆奥斯曼生物资源有限公司 | Preparation method of carhamus tincwrius L. haematochrome |
| CN102585540A (en) * | 2011-12-30 | 2012-07-18 | 上海染料研究所有限公司 | Method for preparing edible pigment such as new red |
| CN104877368A (en) * | 2015-05-14 | 2015-09-02 | 吕永赛 | Chrysophenine G production process |
| CN107898682A (en) * | 2017-11-17 | 2018-04-13 | 新疆奥斯曼生物资源有限公司 | A kind of safflower compounded thing and preparation method and a kind of lipstick and preparation method |
| CN110330812A (en) * | 2019-07-08 | 2019-10-15 | 山东中惠生物科技股份有限公司 | A kind of natural pigment color lake and preparation method thereof |
-
2019
- 2019-12-23 CN CN201911339673.9A patent/CN110903680B/en not_active Expired - Fee Related
Patent Citations (11)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS58198567A (en) * | 1982-05-13 | 1983-11-18 | Sumitomo Chem Co Ltd | Bifunctional reactive compound |
| CN1052492A (en) * | 1988-10-20 | 1991-06-26 | 山道士有限公司 | fiber-reactive azo dyes |
| CN100569862C (en) * | 2004-04-09 | 2009-12-16 | 日本化药株式会社 | Azo-compound, ink composite and colouring agent |
| CN1973001A (en) * | 2004-06-23 | 2007-05-30 | 日本化药株式会社 | Azo compound, ink composition, and colored object |
| CN101248141A (en) * | 2005-09-15 | 2008-08-20 | 日本化药株式会社 | Azo compound, ink composition, recording method, and colored object |
| CN101817772A (en) * | 2009-12-09 | 2010-09-01 | 兰州理工大学 | Method for preparing lutein by using marigold |
| CN102295839A (en) * | 2011-06-29 | 2011-12-28 | 新疆奥斯曼生物资源有限公司 | Preparation method of carhamus tincwrius L. haematochrome |
| CN102585540A (en) * | 2011-12-30 | 2012-07-18 | 上海染料研究所有限公司 | Method for preparing edible pigment such as new red |
| CN104877368A (en) * | 2015-05-14 | 2015-09-02 | 吕永赛 | Chrysophenine G production process |
| CN107898682A (en) * | 2017-11-17 | 2018-04-13 | 新疆奥斯曼生物资源有限公司 | A kind of safflower compounded thing and preparation method and a kind of lipstick and preparation method |
| CN110330812A (en) * | 2019-07-08 | 2019-10-15 | 山东中惠生物科技股份有限公司 | A kind of natural pigment color lake and preparation method thereof |
Non-Patent Citations (4)
| Title |
|---|
| 溶蒽素绿IB生产技术改进试验.《染料与染色》.1977,(第04期),16-17. * |
| 王燕.硫酸铵和氯化钠混合盐析米曲霉蛋白酶的研究.《食品工业科技》.2009,第30卷(第06期),150-152、155. * |
| 赵伟良.混合盐析法从柑桔皮中提取果胶.《精细化工》.1995,第12卷(第06期),55-57. * |
| 陈忻等.柚皮的综合利用及色素稳定性研究.《资源开发与市场》.2000,(第05期),270-271. * |
Also Published As
| Publication number | Publication date |
|---|---|
| CN110903680A (en) | 2020-03-24 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| US6218574B1 (en) | Process for purifying long-chain dicarboxylic acid | |
| CN110903680B (en) | Low-salt purification method of edible colorant | |
| CN108329205B (en) | Preparation method of bis (2-acetoxybenzoic acid) calcium urea compound | |
| CN110745803A (en) | Method for preparing potassium dihydrogen phosphate from wet-process phosphoric acid | |
| CN112552167B (en) | Preparation method of calcium gluconate | |
| CN103265467B (en) | A kind of crystallisation by cooling refines the method for L-PROLINE | |
| CN101880291B (en) | Preparation method of cefpirome sulfate sterile powder | |
| CN104355990B (en) | Method for recycling and mechanically using L- (+) -tartaric acid in D-ethyl ester production | |
| CN115676788B (en) | High-purity potassium dihydrogen phosphate and preparation method thereof | |
| CN108516568B (en) | Production method of potassium nitrate | |
| CN105753728A (en) | Medicinal L-valine dilution crystallization method | |
| CN104447758A (en) | Synthesis process of pyrazolo[3,4-d]pyrimidine compounds | |
| CN105566098A (en) | Method for combined production of high purity crystalline calcium acetate and waterless calcium acetate | |
| KR940000810B1 (en) | Process for the preparation of crystallized glutamic acid | |
| CN110606863B (en) | Preparation method of N-acetylneuraminic acid dihydrate | |
| CN108610352B (en) | Method for preparing mezlocillin sodium by solvent crystallization | |
| CN113072047A (en) | Production process for continuously preparing monopotassium phosphate | |
| CN1706792A (en) | Purifying process of 3,4,5-trimethoxyl benzoic acid | |
| CN113880118B (en) | Preparation method of NaCl target salt | |
| CN116199601B (en) | Refining and purifying process of high-content chlorothalonil | |
| CN114751818B (en) | Preparation method of azelaic acid alpha crystal form | |
| CN115850057A (en) | Preparation method of calcium gluconate monohydrate | |
| CN109369740B (en) | Method for preparing crystalline salicin by using by-products in salicin production | |
| CN110511254A (en) | A kind of method for crystallising of Clindamycin Hydrochloride | |
| CN116354819A (en) | Process for preparing aspirin and its related intermediate |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| GR01 | Patent grant | ||
| GR01 | Patent grant | ||
| CF01 | Termination of patent right due to non-payment of annual fee | ||
| CF01 | Termination of patent right due to non-payment of annual fee |
Granted publication date: 20210903 Termination date: 20211223 |