CN112625463B - Salting-out refining method for synthetic edible pigment - Google Patents
Salting-out refining method for synthetic edible pigment Download PDFInfo
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- CN112625463B CN112625463B CN202011528111.1A CN202011528111A CN112625463B CN 112625463 B CN112625463 B CN 112625463B CN 202011528111 A CN202011528111 A CN 202011528111A CN 112625463 B CN112625463 B CN 112625463B
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- solution
- concentrated solution
- salting
- sodium chloride
- precipitator
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- 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
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02A—TECHNOLOGIES FOR ADAPTATION TO CLIMATE CHANGE
- Y02A40/00—Adaptation technologies in agriculture, forestry, livestock or agroalimentary production
- Y02A40/90—Adaptation technologies in agriculture, forestry, livestock or agroalimentary production in food processing or handling, e.g. food conservation
Abstract
The invention discloses a salting-out refining method for synthetic edible pigment, which is characterized by comprising the following steps: the method comprises the following steps: separating the pigment coupling solution into two parts of pure water and concentrated solution after membrane treatment, wherein the volume ratio of the pure water to the concentrated solution is (2-4): 1; step two: adding a small amount of sodium chloride into the concentrated solution obtained in the step one, wherein the amount of the sodium chloride is 3-5% of the weight of the concentrated solution; step three: adding a precipitator into the product obtained in the step two, standing until the solution is clear, and filtering to obtain a product; the dosage of the precipitator is 0.05-0.2%, and the standing operation temperature is 40-60 ℃. The invention greatly reduces the dosage of the sodium chloride for salting out and reduces the generation of waste water by concentration.
Description
Technical Field
The invention belongs to the field of pigment preparation, and particularly relates to a salting-out refining method for a synthetic edible pigment.
Background
The synthetic edible pigment has the basic structure of organic sodium sulfonate containing benzene ring/naphthalene ring structure, and exists in the coupling liquid obtained through reaction after reaction production.
However, in the process, a large amount of high-salt high-COD wastewater is generated, so that great pressure is applied to the ecological environment, and the environmental protection cost is greatly increased when the wastewater is treated.
Disclosure of Invention
In order to overcome the defects of the prior art, the invention aims to provide a salting-out refining method for relatively environment-friendly synthetic food pigment, so as to reduce the using amount of sodium chloride and reduce the amount of wastewater after final salting-out.
In order to realize one of the purposes of the invention, the adopted technical scheme is as follows:
a salting-out refining method of synthetic food pigment comprises the following steps:
the method comprises the following steps: separating the pigment coupling solution into two parts of pure water and concentrated solution after membrane treatment, wherein the volume ratio of the pure water to the concentrated solution is (2-4): 1;
step two: adding a small amount of sodium chloride into the concentrated solution obtained in the step one, wherein the amount of the sodium chloride is 3-5% of the weight of the concentrated solution;
step three: adding a precipitator into the product obtained in the step two, standing until the solution is clear, and filtering to obtain a product;
the dosage of the precipitator is 0.05-0.2%, and the standing operation temperature is 40-60 ℃.
In a preferred embodiment of the present invention, the first step is specifically: after 500ml of dye coupling solution was passed through the membrane, the coupling solution was divided into 375ml of pure water and 125ml of concentrate.
The dye coupling liquid is any one or more of carmine coupling liquid, sunset yellow coupling liquid, lemon yellow coupling liquid or allure red coupling liquid.
In a preferred embodiment of the invention, the added precipitator is any one or more of calcium chloride, zinc chloride and ferrous chloride, and the amount of the precipitator is 0.05-0.1% of the concentrated solution.
In a preferred embodiment of the present invention, the final amount of wastewater is 120-150g based on 500g of the initial coupling solution.
The main innovation points of the invention are as follows: the invention utilizes the membrane treatment technology to treat the heavy nitrogen liquid, so that the solution enters a supersaturated state, and the precipitation of the product is promoted by adding the precipitator.
Detailed Description
The invention is further described with reference to the following examples:
example 1:
after 500g of carmine coupled solution is subjected to membrane treatment, the coupled solution is divided into 346g of pure water and 154g of concentrated solution, 4g of sodium chloride is added into the concentrated solution, the mixture is stirred and dissolved, 0.15g of calcium chloride is added, the temperature is kept at 50 ℃ until the solution is clear, a carmine product is obtained after filtration, the yield is 92%, and the amount of high-concentration wastewater is 120 g.
Example 2:
after 500g of sunset yellow coupling solution is processed by a membrane, the coupling solution is divided into 375g of pure water and 125g of concentrated solution, 3g of sodium chloride is added into the concentrated solution, the mixture is stirred and dissolved, 0.25g of ferrous chloride is added, the temperature is kept at 60 ℃ until the solution is clear, the sunset yellow product is obtained after filtration, the yield is 95%, and the amount of high-concentration wastewater is 111 g.
Example 3:
after 500g of lemon yellow coupling liquid is processed by a membrane, the coupling liquid is divided into 375g of pure water and 125g of concentrated liquid, 3g of sodium chloride is added into the concentrated liquid, the mixture is stirred and dissolved, 0.06g of zinc chloride is added, the mixture is heated to 60 ℃ and kept at the constant temperature until the solution is clear, and a lemon yellow product is obtained after filtration, the yield is 95%, and the amount of high-concentration wastewater is 140 g.
Example 4:
after 500g of allura red coupling solution is processed by a membrane, the coupling solution is divided into 350g of pure water and 150g of concentrated solution, 4g of sodium chloride is added into the concentrated solution, the mixture is stirred and dissolved, 0.15g of calcium chloride is added, the mixture is heated to 60 ℃ and kept at a constant temperature until the solution is clear, and the allura red product is obtained after filtration, wherein the yield is 90%, and the amount of high-concentration wastewater is 122 g.
Comparative example 1:
comparative example 1 is a prior art salting-out comparative example:
directly salting out 500g of allura red coupling solution, adding 45g of sodium chloride, heating to 55 ℃, keeping the temperature until the product is not separated out, and filtering to obtain the allura red product, wherein the yield is 85%, and the amount of high-concentration wastewater is 415 g.
Comparative example 2:
and (3) directly salting out 500g of lemon yellow coupling solution, adding 20g of sodium chloride, heating to 40 ℃, keeping the temperature until the product is not separated out, and filtering to obtain the lemon yellow product, wherein the yield is 78%, and the high-concentration wastewater amount is 431 g.
The principle on which the invention is based is that:
the method is characterized in that a reverse osmosis membrane is utilized to concentrate a coupling solution, the saturation degree of the solution is improved, a small amount of sodium chloride is added (the addition amount of the sodium chloride is selected to be within the range of the invention because the addition amount of the sodium chloride is too small, the supersaturation degree is insufficient, the refining time is long, the yield of a product is lost, the addition amount of the sodium chloride is too large, the cost is increased, the salt content of wastewater is increased, and the wastewater is difficult to treat), and a trace amount of precipitator is added when the solution is supersaturated (the addition amount of the precipitator is selected to be within the range of the invention because the salting-out refining time is long, the product is increased excessively, the product quality is reduced), and the solid separated out by combining an edible pigment and the precipitator is used as a crystal nucleus to separate out the product stably, so that the product is obtained stably.
Under the new process condition, because the reaction liquid is saturated through the preconcentration by the membrane separation method, on the basis, a small amount of sodium chloride is added to separate out the product, the salt consumption is greatly reduced (reaching hundreds of times of reduction) compared with the prior art, and the final wastewater amount is also greatly reduced.
Claims (2)
1. A salting-out refining method for synthetic food pigment is characterized by comprising the following steps:
the method comprises the following steps: separating the pigment coupling solution into two parts of pure water and concentrated solution after membrane treatment, wherein the volume ratio of the pure water to the concentrated solution is (2-4): 1;
step two: adding a small amount of sodium chloride into the concentrated solution obtained in the step one, wherein the amount of the sodium chloride is 3-5% of the weight of the concentrated solution;
step three: adding a precipitator into the product obtained in the step two, standing until the solution is clear, and filtering to obtain a product;
standing at 40-60 deg.C;
the pigment coupling liquid is any one or more of carmine coupling liquid, sunset yellow coupling liquid, lemon yellow coupling liquid or allure red coupling liquid;
the added precipitator is one or more of calcium chloride, zinc chloride and ferrous chloride, and the dosage of the precipitator is 0.05-0.1% of the weight of the concentrated solution.
2. The salting process according to claim 1, wherein the final amount of wastewater is 120-150g based on 500g of the initial coupling solution.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202011528111.1A CN112625463B (en) | 2020-12-22 | 2020-12-22 | Salting-out refining method for synthetic edible pigment |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202011528111.1A CN112625463B (en) | 2020-12-22 | 2020-12-22 | Salting-out refining method for synthetic edible pigment |
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| CN112625463A CN112625463A (en) | 2021-04-09 |
| CN112625463B true CN112625463B (en) | 2022-08-26 |
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Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4452608A (en) * | 1982-03-05 | 1984-06-05 | Ciba-Geigy Corporation | Process for the preparation of metal complex dye formulations using membrane separation |
| JPS6264868A (en) * | 1985-09-17 | 1987-03-23 | Mitsubishi Chem Ind Ltd | Preparation of water-soluble dye having lithium sulfonate or ammonium sulfonate group |
| CN101333344A (en) * | 2007-06-26 | 2008-12-31 | 上海染料研究所有限公司 | Method for reducing organic impurity content in sunset yellow |
| CN102911278A (en) * | 2012-10-18 | 2013-02-06 | 成都连接流体分离科技有限公司 | Membrane concentration process used for carrageenan production |
| CN110903680A (en) * | 2019-12-23 | 2020-03-24 | 上海染料研究所有限公司 | Low-salt purification method of edible colorant |
-
2020
- 2020-12-22 CN CN202011528111.1A patent/CN112625463B/en active Active
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4452608A (en) * | 1982-03-05 | 1984-06-05 | Ciba-Geigy Corporation | Process for the preparation of metal complex dye formulations using membrane separation |
| JPS6264868A (en) * | 1985-09-17 | 1987-03-23 | Mitsubishi Chem Ind Ltd | Preparation of water-soluble dye having lithium sulfonate or ammonium sulfonate group |
| CN101333344A (en) * | 2007-06-26 | 2008-12-31 | 上海染料研究所有限公司 | Method for reducing organic impurity content in sunset yellow |
| CN102911278A (en) * | 2012-10-18 | 2013-02-06 | 成都连接流体分离科技有限公司 | Membrane concentration process used for carrageenan production |
| CN110903680A (en) * | 2019-12-23 | 2020-03-24 | 上海染料研究所有限公司 | Low-salt purification method of edible colorant |
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| CN112625463A (en) | 2021-04-09 |
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