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Method for preparing tetrahydrofuran acrylate through continuous esterification reaction and method for preparing catalyst

A technology for tetrahydrofuran acrylate and esterification reaction, which is applied in the direction of organic compound/hydride/coordination complex catalyst, physical/chemical process catalyst, catalytic reaction, etc., and can solve many side reactions, low production efficiency, complex process, etc. problems, to achieve the effect of reducing product chromaticity, prolonging service life and stabilizing pore structure

Active Publication Date: 2017-03-22
WANHUA CHEM GRP CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

This method overcomes the disadvantages of the existing batch production process that the product needs to be washed with alkali, neutralized and washed, a large amount of waste water is generated, the process is complicated, the production efficiency is low, and there are many side reactions.

Method used

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  • Method for preparing tetrahydrofuran acrylate through continuous esterification reaction and method for preparing catalyst

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0062] 1. Add 267g of saturated sodium chloride aqueous solution, 35g of gelatin and 1.8g of polyvinyl alcohol dispersant into a reactor equipped with a high-speed stirrer and a thermometer; Take 150g of o-chlorostyrene and 28g of divinylbenzene, based on the quality of o-chlorostyrene and divinylbenzene 1wt% of submicron silicon carbide whiskers, 0.1wt% of nano-sized tungsten oxide, 1wt% of nano-sized Add zirconia, 1wt% liquid paraffin porogen and 0.5wt% benzoyl peroxide initiator to the reactor, heat up to 60°C and stir for 2h; 3. Cool and filter after the reaction, wash and dry with 50°C hot water 4. Extract the porogen with excess petroleum ether, and sieve out the resin skeleton with a diameter of 0.4-0.6mm; 5. The resulting resin skeleton is swollen with excess dichloroethane; 2% concentrated sulfuric acid, heat up to 75°C and reflux for 1 hour; 7. Evaporate dichloroethane, then add 1% oleum based on the resin mass, heat up the reaction, cool down when the resin exchange...

Embodiment 2

[0065] 1. Add 225g of saturated sodium chloride aqueous solution, 51g of gelatin and 2.6g of polyvinyl alcohol dispersant into a reactor equipped with a high-speed stirrer and a thermometer; 2. Start stirring, and after the dispersant is evenly dispersed in the system, weigh Take 130g o-chlorostyrene and 41g divinylbenzene, based on o-chlorostyrene and divinylbenzene mass 3% submicron silicon carbide whiskers, 0.5% nano-sized tungsten oxide, 0.5% nano-sized zirconia , 2% liquid paraffin porogen and 0.2% benzoyl peroxide initiator were added to the reactor, and the temperature was raised to 45°C and stirred for 6 hours; 3. After the reaction was completed, it was cooled and filtered, washed with hot water at 70°C, and dried; 4. 1. Extract the porogen with excess petroleum ether, and sieve out the resin skeleton with a diameter of 0.4-0.6mm; 5. The obtained resin skeleton is swollen with excess dichloroethane; 6. After the swelling is completed, add 2% concentrated Sulfuric acid...

Embodiment 3

[0068] 1. Add 175g of saturated sodium chloride aqueous solution, 45g of gelatin and 2.2g of polyvinyl alcohol dispersant into a reactor equipped with a high-speed stirrer and a thermometer; Take 140g of o-chlorostyrene and 33g of divinylbenzene, based on the quality of o-chlorostyrene and divinylbenzene 5% submicron silicon carbide whiskers, 0.2% of nano-sized tungsten oxide, 0.1% of nano-sized zirconia , add 3% liquid paraffin porogen and 0.3% benzoyl peroxide initiator into the reactor, heat up to 50°C and stir for 4 hours; 3. Cool and filter after the reaction, wash with hot water at 60°C, and dry; 4. 1. Extract the porogen with excess petroleum ether, and screen the resin skeleton with a diameter of 0.4 to 0.6 mm; 5. The obtained resin skeleton is swollen with excess dichloroethane; 6. After the swelling is completed, add 3% concentrated Sulfuric acid, heat up to 78°C and reflux for 1 hour; 7. Distill out dichloroethane, then add 1% oleum based on the resin mass, and heat...

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Abstract

The invention discloses a method for preparing tetrahydrofuran acrylate through a continuous esterification reaction. The method comprises the following steps: taking acrylic acid and tetrahydrofurfuryl alcohol as raw materials, adopting a composite catalyst composed of a metal ion modified solid acid catalyst and graphite, adding submicron order silicon carbide whiskers, nanoscale tungsten oxide, nanoscale zirconium oxide, metal ions and the like into the catalyst for modifying an ion exchange resin, and realizing a two-stage continuous esterification reaction. According to the method, continuous production of the tetrahydrofuran acrylate is realized by controlling the temperature, reaction pressure and the like, the conversion rate can reach 100%, the monoester selectivity is 97%, the overall product yield is 97%, and the method disclosed by the invention is simple in operation, capable of obviously improving the production efficiency, reducing the production cost and greatly reducing the wastewater discharge, and has excellent large-scale industrial application value.

Description

technical field [0001] The invention relates to a preparation method of tetrahydrofuran acrylate, in particular to a method for preparing tetrahydrofuran acrylate by continuous esterification, and belongs to the field of photocurable materials. Background technique [0002] Tetrahydrofuran acrylate (hereinafter referred to as TFA) is an important special acrylate, the structural formula is [0003] The special structure of TFA endows its follow-up products with special properties. First, the cyclic ether group in the TFA molecule is more active than the straight-chain ether group, and the hydrogen on the α-position carbon of the ether bond also has certain activity. Therefore, the TFA can be cured at a lower temperature (about 100°C) when the acrylic resin and amino resin used together as a copolymerization component. Secondly, the molecular valence bond of TFA has a certain degree of flexibility, and it can be used together with other resins to achieve a plasticizing eff...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D307/12B01J31/38B01J35/10
CPCC07D307/12B01J31/38B01J2231/49B01J35/60
Inventor 鞠昌迅张琴花陈海波董龙跃赵晶赵文娟黎源华卫琦
Owner WANHUA CHEM GRP CO LTD
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