Chlorohydrin ball loaded amine substance modified heteropolyacid catalyst as well as preparation and application of chlorohydrin ball loaded amine substance modified heteropolyacid catalyst

A technology of amine substances and heteropolyacids, which is applied in the application field of chlorine ball-loaded amine substances modified heteropolyacid catalysts and its preparation, lauric acid and glycerol esterification, and can solve the problem of long catalyst preparation time and easy Soluble in polar solvents, small specific surface area, etc., to solve severe corrosion equipment, low preparation cost, simple separation and purification

Pending Publication Date: 2022-05-31
ZHEJIANG GONGSHANG UNIVERSITY
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  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] This application provides an ultrasonic preparation method and application of a heteropolyacid catalyst modified by chlorine ball-loaded amine substances, which solves the problem of the traditional heteropolyacid catalyst itself having a small specific surface area and being easily soluble in polar solvents during use. However, it is difficult to separate, and the catalyst preparation time is long, etc.

Method used

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  • Chlorohydrin ball loaded amine substance modified heteropolyacid catalyst as well as preparation and application of chlorohydrin ball loaded amine substance modified heteropolyacid catalyst
  • Chlorohydrin ball loaded amine substance modified heteropolyacid catalyst as well as preparation and application of chlorohydrin ball loaded amine substance modified heteropolyacid catalyst
  • Chlorohydrin ball loaded amine substance modified heteropolyacid catalyst as well as preparation and application of chlorohydrin ball loaded amine substance modified heteropolyacid catalyst

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Effect test

preparation example Construction

[0048] In order to solve the problems of serious corrosion of equipment, pollution of the environment, and complicated post-treatment of common catalysts, the application has the advantages of simple catalyst preparation, low preparation cost, and at the same time, it is loaded on a carrier, which is convenient for the separation and purification of the catalyst after the reaction, and proposes a chlorine ball supported The preparation method of amine substance modified heteropolyacid catalyst specifically comprises the following steps:

[0049] (1) Using chlorine balls and amines as raw materials, using acetonitrile as solvent, reacting in an ultrasonic synthesizer for a period of time, cooling to room temperature for filtration, and washing with ethyl acetate, 0.1mol / L HCl, water and methanol for many times , and then vacuum-dried to obtain an amine-modified chlorine ball ultrasonic synthesizer for use. In the step, the ultrasonic reaction temperature is 60-120° C., the ultr...

Embodiment 1

[0054] The present embodiment takes chlorine ball-piperazine-silicotungstic acid as an example, and the preparation method of the catalyst is as follows:

[0055](1) Using chlorine ball and piperazine as raw materials, using acetonitrile as solvent, under the conditions of reaction temperature of 80°C and ultrasonic power of 500W, placed in an ultrasonic synthesizer to react for 2.5h, cooled to room temperature after the reaction, and filtered with acetic acid. Ethyl ester, 0.1mol / L HCl, water and methanol were washed for several times, and then vacuum-dried to obtain piperazine-modified chlorine spheres, and the substance ratio of chlorine spheres to piperazine was 1:1.2.

[0056] (2) The piperazine-modified chlorine ball and silicotungstic acid were placed in a reaction vessel and reacted in an ultrasonic synthesizer. The reaction temperature was 80°C and the ultrasonic power was 500W. After vacuum drying treatment, piperazine modified chlorine spheres supported silicotungst...

Embodiment 2

[0065] In order to verify the catalytic effect of different reaction time catalysts, in the present example, in the 100mL there-necked flask equipped with the reflux condenser, add lauric acid 10g, glycerol 23g, catalyzer 0.4g (prepared in Example 1) successively, and place it in 150 The reaction was heated in an oil bath. The reaction product was taken every half hour (one hour after 3h), and the reaction product was analyzed by gas chromatography for its conversion rate and yield. The reaction results of monoglyceryl laurate obtained by changing the reaction time are shown in Table 1.

[0066] Table 1: The reaction results of monoglyceryl laurate obtained at different reaction times.

[0067]

[0068]

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Abstract

The invention discloses a chloromethylated bead loaded amine substance modified heteropolyacid catalyst and preparation and application thereof.The preparation method comprises the steps that chloromethylated beads and amine substances are mixed in an organic solvent to be subjected to a reaction, reaction liquid is obtained, and the obtained reaction liquid is washed and dried to obtain chloromethylated beads loaded with the amine substances; mixing the obtained chlorine balls loaded with the amine substances with a heteropolyacid aqueous solution for reaction, and then sequentially concentrating, washing and drying to obtain the chlorine ball loaded amine substance modified heteropolyacid catalyst. Taking alcohol and carboxylic acid as raw materials, taking the chloromethylated bead loaded amine substance modified heteropoly acid as a catalyst, and reacting in an oil bath at 130-170 DEG C for 0.5-4 hours; cooling after the reaction is finished, layering the catalyst and the reaction system, recovering the solid catalyst by filtering, washing the catalyst with diethyl ether, drying, and directly and repeatedly using for the next reaction. The problems that a traditional heteropolyacid catalyst is small in specific surface area, easy to dissolve in a polar solvent in the using process and difficult to separate, long in catalyst preparation time and the like are solved.

Description

technical field [0001] The present application relates to the technical field of ester preparation, in particular to a chlorine ball-loaded amine-modified heteropolyacid catalyst, a preparation method thereof, and an application in the esterification reaction of lauric acid and glycerol. Background technique [0002] Monoglyceryl laurate (GML) is not only an excellent emulsifier, but also a safe, efficient and broad-spectrum antibacterial agent. As a safe food additive, GML has been widely used in food, pharmaceutical, cosmetic and other industries. The common preparation method of GML is obtained by direct esterification of lauric acid and glycerol in the presence of a protic acid catalyst. The traditional catalytic method has problems such as cumbersome post-treatment, large environmental pollution, poor selectivity and low catalytic efficiency. [0003] As a new type of green and highly active catalyst, heteropolyacids can solve the problems of severe corrosion of equipm...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J31/06B01J31/40B01J23/30B01J37/34C07C67/08C07C69/30
CPCB01J31/06B01J31/4007B01J27/188B01J23/30B01J37/343C07C67/08B01J2231/49C07C69/30Y02P20/584
Inventor 韩晓祥蒋胜筹陈梓怡邓云莉赵孙超蔡锦旺
Owner ZHEJIANG GONGSHANG UNIVERSITY
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