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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 reduction of production cost, consumption reduction, and improvement of esterification rate. Effect

Active Publication Date: 2013-12-25
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 example is used to illustrate the preparation of the citrate ester provided by the present invention.

[0043] (1) Contains Fe 3+ , Al 3+ And Cu 2+ One or more ions in the preparation of citric acid:

[0044] The above 5L citric acid fermentation clear liquid (the content of citric acid monohydrate: 16g / 100mL) was added to 1250g calcium carbonate slurry (calcium carbonate concentration is 45% by weight) and reacted for 4 hours under the conditions of 75°C and pH 6 and left to stand. Separate the layers, discard the supernatant (ie, waste sugar water) to obtain calcium citrate slurry. After the calcium citrate slurry was vacuum-dried, 560 g of concentrated sulfuric acid was added for acid hydrolysis for 10 minutes, and after the reaction was completed, it was separated by filtration with a belt conveyor. The liquid product was the citric acid hydrolysis solution and the solid product was waste calcium sulfate. The citric acid hydrolysate is decolorized and then concentr...

Embodiment 2

[0048] This example is used to illustrate the preparation of the citrate ester provided by the present invention.

[0049] (1) Contains Fe 3+ , Al 3+ And Cu 2+ One or more ions in the preparation of citric acid:

[0050] The above 5L citric acid fermentation clear liquid (the content of citric acid monohydrate: 16g / 100mL) was added to 1250g calcium carbonate slurry (calcium carbonate concentration is 45% by weight) and reacted for 4 hours under the conditions of 85°C and pH 8. Separate the layers, discard the supernatant (ie, waste sugar water) to obtain calcium citrate slurry. After the calcium citrate slurry was vacuum-dried, 560 g of concentrated sulfuric acid was added for acid hydrolysis for 10 minutes, and after the reaction was completed, it was separated by filtration with a belt conveyor. The liquid product was the citric acid hydrolysis solution and the solid product was waste calcium sulfate. The acid hydrolysate of citric acid is decolorized and then concentrated to ob...

Embodiment 3

[0054] This example is used to illustrate the preparation of the citrate ester provided by the present invention.

[0055] (1) Contains Fe 3+ , Al 3+ And Cu 2+ One or more ions in the preparation of citric acid:

[0056] Add 2300g of D318 macroporous weakly basic acrylic anion exchange resin (Jiangsu Suqing Water Treatment Engineering Group Co., Ltd., OH) into 5L citric acid fermentation clear liquid (citric acid monohydrate content: 16g / 100mL) - The content is 15 mmol / g dry resin) for immersion exchange adsorption, separated by vacuum filtration, citric acid is adsorbed on the resin, and impurities such as sugar and protein are discharged with the waste liquid, and then washed with 2500mL of 10% by weight dilute sulfuric acid The citric acid eluate is obtained by removing, and the citric acid eluate is concentrated and crystallized to obtain 0.7 kg of citric acid crystals; wherein, the citric acid crystals contain Fe 3+ , Al 3+ And Cu 2+ , And Fe 3+ , Al 3+ And Cu 2+ The total cont...

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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 citrate ester. Background technique [0002] Citrate has the advantages of non-toxicity, good biodegradability, low volatility and excellent antibacterial properties, and is an environmentally friendly material. In recent years, research on citrate esters at home and abroad has been extremely active, and a variety of varieties suitable for different fields have been successfully developed. Citrate has a very broad application field, not only as a non-toxic and odorless green plasticizer, but also as a surfactant and metal chelating agent. [0003] As a plasticizer with excellent performance, citrate ester has attracted wide attention due to its good compatibility, high plasticizing efficiency, non-toxic, non-volatile, and strong weather resistance. It has become the first choice for green products that can replace phthalates as plasticizers. [0004] As an important surfactant, citrate has been widely used wor...

Claims

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Application Information

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Patent Type & Authority Patents(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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