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A kind of silver ammonium phosphotungstate compound salt catalyzes the method for synthesizing citrate

A technology of silver ammonium phosphotungstate and citrate, applied in chemical instruments and methods, preparation of organic compounds, preparation of carboxylic acid esters, etc., can solve the problems of poor reusability, complicated preparation process, and low activity, and achieve Environmental friendliness, simple preparation process, high surface area effect

Inactive Publication Date: 2016-09-28
SHAOYANG UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, the above-mentioned heteropolyacid salt catalysts have defects such as low activity, complicated preparation process, large dosage or poor reusability.

Method used

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  • A kind of silver ammonium phosphotungstate compound salt catalyzes the method for synthesizing citrate

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0015] Add 19.21 g citric acid (0.1 mol), 33.35 g n-butanol (0.45 mol) and 0.38 g (NH 4 ) 0.5 Ag 0.5 h 2 PW 12 o 40 Catalyst, start stirring, raise the temperature to 155°C, start timing when the reflux phenomenon starts to appear in the condenser tube, and react for 4 hours. After the reaction system was cooled to room temperature, it was separated by filtration, and the filtrate was detected by gas chromatography. The product yields are shown in Table 1.

Embodiment 2

[0017] Using the same reaction conditions and detection method as in Example 1, only the amount of catalyst was changed to 0.20 g, and the product yield is shown in Table 1.

Embodiment 3

[0019] Using the same reaction conditions and detection method as in Example 1, only the amount of catalyst was changed to 0.80 g, and the product yield is shown in Table 1.

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Abstract

The invention relates to a method for catalytic synthesis of citric acid ester by a (NH4)xAgyH3-x-yPW12O40 composite salt. The (NH4)xAgyH3-x-yPW12O40 composite salt is adopted as the catalyst, under the conditions that an amount ratio of citric acid to alcohol is 1:3-6 and a mass ratio of the catalyst to citric acid is 1-5:100, esterification reaction is carried out at 130-180DEG C for 2-6h so as to synthesize citric acid ester. According to the invention, the (NH4)xAgyH3-x-yPW12O40 composite salt has the characteristics of high catalytic activity, low dosage, simple separation from the reaction system, direct recycle without any treatment, and excellent repeated use performance. The reaction process can achieve zero emission, and is environment friendly.

Description

technical field [0001] The invention relates to a method for synthesizing citric acid ester, in particular to a method for catalyzing the synthesis of citric acid ester with silver ammonium phosphotungstate compound salt. Background technique [0002] Citrate is a non-toxic plasticizer with a wide range of uses. It has the advantages of non-toxicity, low volatility, high plasticizing efficiency and good compatibility. As one of the green alternatives to traditional phthalate plasticizers, the U.S. Food and Drug Administration has approved the use of citrate plasticizers in food packaging materials, medical appliances and personal hygiene products, etc. . In recent years, citric acid esters have become the first environmentally friendly plasticizers at home and abroad. [0003] In the traditional production process of citrate, concentrated sulfuric acid is mainly used as a catalyst. Concentrated sulfuric acid is cheap and has high catalytic activity. However, there are ma...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C67/08C07C69/704B01J27/188
CPCB01J27/188B01J2523/18B01J2523/51B01J2523/69C07C67/08C07C69/704
Inventor 周喜李泽贤
Owner SHAOYANG UNIV