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Preparation method of citrate

A technology of citric acid ester and citric acid, applied in the field of preparation of citric acid ester, can solve the problems of low yield of citric acid ester, large amount of catalyst, complicated process, etc., and achieves lower production cost, lower consumption, and higher esterification rate. Effect

Active Publication Date: 2012-04-18
COFCO BIOTECHNOLOGY CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0006] The purpose of the present invention is to overcome the disadvantages of complex procedures, large amount of catalyst, low yield of citric acid ester and more impurities generated by esterification reaction when the existing method is used to prepare citric acid ester, and to provide a A preparation method capable of simplifying procedures, reducing catalyst consumption, higher yield of citric acid ester, and producing citric acid ester with less impurities

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0042] This embodiment is used to illustrate the preparation of the citric acid ester provided by the invention.

[0043] (1) Contains Fe 3+ 、Al 3+ and Cu 2+ Preparation of citric acid with one or more ions in:

[0044] The above 5L citric acid fermentation serum (citric acid monohydrate content: 16g / 100mL) was added to 1250g calcium carbonate slurry (calcium carbonate concentration was 45% by weight) and reacted for 4 hours at 75°C and pH 6, and allowed to stand Separate the layers, discard the supernatant (i.e. waste sugar water) to obtain calcium citrate slurry. After the calcium citrate slurry was vacuum-dried, 560g of concentrated sulfuric acid was added to carry out the acid hydrolysis reaction for 10 minutes. After the reaction was finished, it was filtered and separated by a tape machine. The liquid product was citric acid acid hydrolysis solution, and the solid product was waste calcium sulfate. Concentrate and crystallize the citric acid acid hydrolysis solution ...

Embodiment 2

[0048] This embodiment is used to illustrate the preparation of the citric acid ester provided by the invention.

[0049] (1) Contains Fe 3+ 、Al 3+ and Cu 2+ Preparation of citric acid with one or more ions in:

[0050] The above 5L citric acid fermentation clear liquid (citric acid monohydrate content: 16g / 100mL) was added to 1250g calcium carbonate slurry (calcium carbonate concentration was 45% by weight) and reacted for 4 hours at 85°C and pH 8, and allowed to stand Separate the layers, discard the supernatant (i.e. waste sugar water) to obtain calcium citrate slurry. After the calcium citrate slurry was vacuum-dried, 560g of concentrated sulfuric acid was added to carry out the acid hydrolysis reaction for 10 minutes. After the reaction was finished, it was filtered and separated by a tape machine. The liquid product was citric acid acid hydrolysis solution, and the solid product was waste calcium sulfate. The citric acid acid solution is concentrated after decoloriza...

Embodiment 3

[0054] This embodiment is used to illustrate the preparation of the citric acid ester provided by the invention.

[0055] (1) Contains Fe 3+ 、Al 3+ and Cu 2+ Preparation of citric acid with one or more ions in:

[0056] With 5L of citric acid fermentation clear liquid (citric acid monohydrate content: 16g / 100mL), add 2300g of D318 macroporous weakly basic acrylic anion exchange resin (Jiangsu Suqing Water Treatment Engineering Group Co., Ltd., OH - Content is 15 millimoles / gram dry resin) carries out immersion exchange adsorption, separates with vacuum filtration, and citric acid is adsorbed on the resin, and the impurity such as sugar, albumen is discharged with waste liquid, washes with the dilute sulfuric acid of 10% by weight of 2500mL then Remove, promptly obtain citric acid eluent, after citric acid eluent is through concentration, crystallization, obtain 0.7kg to citric acid crystal; Wherein, contain Fe in the citric acid crystal 3+ 、Al 3+ and Cu 2+ , and Fe 3+ 、...

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Abstract

The invention provides a preparation method of citrate. The method comprises the following step of: undergoing a contact reaction on citric acid and monohydric alcohol in the presence of a catalyst to obtain citrate, wherein the citric acid is citric acid containing one or more of Fe<3+>, Al<3+> and Cu<2+> prepared with at least one of the following methods: in a method I, a clear citric acid zymotic fluid is separated and purified with a calcium salt method to obtain the citric acid containing one or more of Fe<3+>, Al<3+> and Cu<2+>; and in a method II, a clear citric acid zymotic fluid is separated and purified with a chromatography to obtain the citric acid containing one or more of Fe<3+>, Al<3+> and Cu<2+>. By adopting the method disclosed by the invention for preparing the citric acid, the procedure can be simplified, the dosage of a catalyst can be reduced, and the yield and purity of the citrate are increased.

Description

technical field [0001] The invention relates to a preparation method of citric acid ester. Background technique [0002] Citric acid ester has the advantages of non-toxicity, good biodegradability, low volatility and excellent anti-bacterial properties, and is an environmentally friendly material. In recent years, the research on citric acid esters at home and abroad has been extremely active, and a variety of varieties suitable for different fields have been successfully developed. The application field of citric acid ester is very broad, not only as a non-toxic and tasteless green plasticizer, but also as a surfactant and a metal chelating agent. [0003] As a plasticizer with excellent performance, citrate has attracted wide attention due to its advantages of good compatibility, high plasticizing efficiency, non-toxicity, non-volatile and strong weather resistance. At present, it has become the preferred green environmental protection product that can replace phthalates...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C69/704C07C67/08
Inventor 陈修熊结青张健全王勇顾宗池
Owner COFCO BIOTECHNOLOGY CO LTD
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