CN114790137A - Method for recovering calcium lactate from waste liquid containing sodium lactate - Google Patents
Method for recovering calcium lactate from waste liquid containing sodium lactate Download PDFInfo
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- CN114790137A CN114790137A CN202210394663.0A CN202210394663A CN114790137A CN 114790137 A CN114790137 A CN 114790137A CN 202210394663 A CN202210394663 A CN 202210394663A CN 114790137 A CN114790137 A CN 114790137A
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- Prior art keywords
- lactate
- calcium
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- calcium chloride
- calcium lactate
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C51/00—Preparation of carboxylic acids or their salts, halides or anhydrides
- C07C51/41—Preparation of salts of carboxylic acids
- C07C51/412—Preparation of salts of carboxylic acids by conversion of the acids, their salts, esters or anhydrides with the same carboxylic acid part
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C51/00—Preparation of carboxylic acids or their salts, halides or anhydrides
- C07C51/42—Separation; Purification; Stabilisation; Use of additives
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C51/00—Preparation of carboxylic acids or their salts, halides or anhydrides
- C07C51/42—Separation; Purification; Stabilisation; Use of additives
- C07C51/43—Separation; Purification; Stabilisation; Use of additives by change of the physical state, e.g. crystallisation
Abstract
The invention relates to the technical field of chemical waste liquid recovery, in particular to a method for recovering calcium lactate from waste liquid containing sodium lactate. The invention comprises the following steps: concentrating the waste liquid containing sodium lactate until the content of sodium lactate is about 150-300 g/L; filtering the obtained concentrated solution, and filtering out insoluble impurities to obtain a clear solution; heating the obtained filtrate, and adding calcium chloride under stirring to completely dissolve the calcium chloride; stopping stirring after the calcium chloride is completely dissolved, adding crystal seeds while the calcium chloride is hot, and standing at room temperature for crystallization; after the crystallization is finished, filtering the solution to obtain a calcium lactate wet product 1; performing secondary crystallization on the wet calcium lactate product to obtain a wet calcium lactate product 2; and drying the wet calcium lactate product 2 to obtain a calcium lactate product meeting the feed-grade quality standard. The invention has simple process and low cost.
Description
Technical Field
The invention relates to the technical field of chemical waste liquid recovery, in particular to a method for recovering calcium lactate from waste liquid containing sodium lactate.
Background
In microbial fermentation processes, particularly in anaerobic fermentation processes, large amounts of lactic acid are often produced as a by-product. Lactic acid is mainly derived from incomplete oxidation of glucose, and accumulation of lactic acid lowers the pH of the system, thereby affecting the activity of organisms. To maintain the stability of the system, the pH is often adjusted by adding sodium hydroxide solution, which results in the production of large amounts of low purity sodium lactate as a by-product. The direct discharge of these waste liquids results in a large waste of resources and requires a large amount of capital for treatment due to the high concentration of COD. Therefore, the recovery and utilization of the lactic acid product in the waste liquid have certain significance.
Calcium lactate is a solid lactate salt, one of the lactate salts having a wide range of uses, and it is an excellent, well-recognized non-toxic calcium supplement. Calcium lactate has a very wide range of uses, and is used as a main calcium supplement for human and animals in the pharmaceutical industry; the product is used as a scale remover in toothpaste in the light industry; in the food industry, calcium lactate is a safe food additive, stabilizer, thickener, etc.
The preparation methods of calcium lactate reported at present are as follows:
calcium carbonate is used as a neutralizer to carry out lactic acid fermentation, and calcium lactate is directly produced by secondary crystallization after lime water is used for neutralizing fermentation liquor.
Adding calcium hydroxide or calcium oxide into 50% of finished lactic acid solution for neutralization reaction, filtering to remove insoluble impurities, cooling for crystallization, separating and drying to obtain the finished product. The method has simple process and higher cost.
Disclosure of Invention
The invention aims to solve the problems and provides a method for recovering calcium lactate from waste liquid containing sodium lactate, which comprises the following steps:
(1) concentrating the waste liquid containing sodium lactate until the content of sodium lactate is about 150-300 g/L.
(2) And (2) filtering the concentrated solution obtained in the step (1) to remove insoluble impurities to obtain a clear solution.
(3) And (3) heating the filtrate obtained in the step (2), and adding calcium chloride under the condition of stirring to completely dissolve the calcium chloride.
(4) And stopping stirring after the calcium chloride is completely dissolved, adding seed crystals while the calcium chloride is hot, and standing at room temperature for crystallization.
(5) After crystallization is completed, the solution is filtered to obtain the wet product 1 of calcium lactate.
(6) And (3) carrying out secondary crystallization on the wet calcium lactate product to obtain the wet calcium lactate product 2.
(7) And drying the wet calcium lactate product 2 to obtain a calcium lactate product meeting the feed-grade quality standard.
Preferably, the concentration in step (1) is performed by evaporation concentration or membrane concentration.
Preferably, the filtration in the step (2) adopts suction filtration, plate-frame filtration or ceramic membrane filtration.
Preferably, the calcium chloride is anhydrous calcium chloride or calcium chloride containing crystal water.
Preferably, the molar ratio of calcium chloride to sodium lactate in the step (3) is 0.4: 1-0.6: 1
Preferably, the heating temperature in the step (3) is 50-80 ℃.
Preferably, the drying is air drying or drying.
Compared with the prior art, the invention has the following beneficial effects:
sodium hydroxide is used in the Nisin fermentation process to neutralize lactic acid produced in the fermentation process, so that the fermentation pH is controlled, and the normal growth of thalli is ensured. The present invention utilizes the fact that the solubility of calcium lactate is less than that of calcium chloride, and calcium chloride is added to precipitate calcium lactate in the filtrate through a displacement reaction, so that the process for preparing calcium lactate is simplified, and the cost is greatly reduced.
Detailed Description
The technical solutions in the embodiments of the present invention are 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 obtained by a person skilled in the art without making any creative effort based on the embodiments in the present invention, belong to the protection scope of the present invention.
Example 1
Taking 10L of the primary filtrate, evaporating and concentrating at 70 deg.C until the content of sodium lactate is 162g/L, and the volume after concentration is 2.52L. A small amount of flocculent precipitate appeared during the concentration process, and the concentrated solution was filtered with a suction flask. The filtrate was heated to 60 ℃ with stirring, 200g of anhydrous calcium chloride was added, and dissolved after stirring for 1 hour. Stopping stirring, adding 0.2g of commercial calcium lactate as seed crystal, slowly cooling to room temperature, and standing for 16h to complete crystallization. The crystal liquid was filtered to obtain 684g of wet calcium lactate 1. Dissolving wet product 1 in 2L of 80 deg.C hot water, evaporating at 80 deg.C to 0.92L, cooling to room temperature, standing for crystallization for 19 hr, and filtering to obtain calcium lactate wet product 2. Drying wet calcium lactate product 2 at 40 deg.C for 5h to obtain 428g calcium lactate product with total yield of 76.7%.
Example 2
Taking 10L of the primary filtrate, and concentrating by evaporation at 75 deg.C until the content of sodium lactate is 225g/L, and the volume after concentration is 2.43L. A small amount of flocculent precipitate appeared during the concentration process, and the concentrated solution was filtered with a suction flask. The filtrate was heated to 70 ℃ with stirring, 243g of anhydrous calcium chloride was added, and dissolved after stirring for 1 hour. Stopping stirring, adding 0.2g of commercial calcium lactate as seed crystal, slowly cooling to room temperature, and standing for 18h to complete crystallization. The crystal liquid was filtered to obtain 653g of wet calcium lactate 1. Dissolving wet product 1 in 2L of 80 deg.C hot water, evaporating at 80 deg.C to 0.93L, cooling to room temperature, standing for crystallization for 16h, and filtering to obtain calcium lactate wet product 2. The wet calcium lactate product 2 was dried at 40 ℃ for 5h to obtain 498g of finished calcium lactate product with a yield of 69%.
Example 3
Taking 10L of the primary filtrate, evaporating and concentrating at 85 deg.C until the content of sodium lactate is 262g/L, and the volume after concentration is 2.13L. A small amount of flocculent precipitate appeared during the concentration process, and the concentrated solution was filtered with a suction flask. The filtrate was heated to 80 ℃ with stirring, 600g of calcium chloride hexahydrate were added, stirred for 1h and dissolved. Stopping stirring, adding 0.2g of commercial calcium lactate as seed crystal, slowly cooling to room temperature, and standing for 24h to complete crystallization. The crystal liquid was filtered to obtain 960g of wet calcium lactate 1. Dissolving wet product 1 in 2L of 80 deg.C hot water, evaporating at 80 deg.C to 1.1L, cooling to room temperature, standing for crystallization for 20 hr, and filtering to obtain calcium lactate wet product 2. Drying wet calcium lactate product 2 at 45 deg.C for 5 hr to obtain 585g calcium lactate product with yield of 76.97%.
The present invention provides a method for preparing high purity calcium lactate by using a fermentation byproduct containing sodium lactate. The calcium lactate product with high purity is obtained by pre-treating the by-product, adding a certain amount of calcium salt, carrying out precipitation and displacement reaction, and then crystallizing.
Claims (7)
1. A method for recovering calcium lactate from waste liquid containing sodium lactate is characterized by comprising the following steps:
(1) concentrating the waste liquid containing sodium lactate until the content of sodium lactate is about 150-300 g/L;
(2) filtering the concentrated solution obtained in the step (1) to remove insoluble impurities to obtain a clear solution;
(3) heating the filtrate obtained in the step (2), and adding calcium chloride under the condition of stirring to completely dissolve the calcium chloride;
(4) stopping stirring after the calcium chloride is completely dissolved, adding crystal seeds while the calcium chloride is hot, and standing at room temperature for crystallization;
(5) after the crystallization is finished, filtering the solution to obtain a calcium lactate wet product 1;
(6) performing secondary crystallization on the wet calcium lactate product to obtain a wet calcium lactate product 2;
(7) and drying the wet calcium lactate product 2 to obtain a calcium lactate product meeting the feed-grade quality standard.
2. The method of claim 1, wherein the concentration in step (1) is performed by evaporation concentration or membrane concentration.
3. The method for recovering calcium lactate from waste liquid containing sodium lactate as claimed in claim 1, wherein the filtration in step (2) is suction filtration, plate-and-frame filtration or ceramic membrane filtration.
4. Method for recovering calcium lactate from a waste liquid containing sodium lactate as claimed in claim 1, wherein the calcium chloride is anhydrous calcium chloride or calcium chloride containing crystal water.
5. The method for recovering calcium lactate from waste liquid containing sodium lactate as claimed in claim 1, wherein the molar ratio of calcium chloride to sodium lactate in the step (3) is 0.4: 1-0.6: 1.
6. the method of claim 1, wherein the heating temperature in step (3) is 50-80 ℃.
7. The method of claim 1, wherein the drying is air drying or oven drying.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202210394663.0A CN114790137A (en) | 2022-04-15 | 2022-04-15 | Method for recovering calcium lactate from waste liquid containing sodium lactate |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202210394663.0A CN114790137A (en) | 2022-04-15 | 2022-04-15 | Method for recovering calcium lactate from waste liquid containing sodium lactate |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN114790137A true CN114790137A (en) | 2022-07-26 |
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Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN202210394663.0A Pending CN114790137A (en) | 2022-04-15 | 2022-04-15 | Method for recovering calcium lactate from waste liquid containing sodium lactate |
Country Status (1)
| Country | Link |
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| CN (1) | CN114790137A (en) |
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2022
- 2022-04-15 CN CN202210394663.0A patent/CN114790137A/en active Pending
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