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Preparation method of carboxylic acid vinyl ester

A technology of vinyl carboxylate and carboxylic acid, which is applied in the field of catalytic conversion of carboxylic acid and acetylene into vinyl ester, and can solve problems such as difficulties in industrial scale-up

Active Publication Date: 2012-08-01
江西元道分子化学股份有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

According to the data provided by the invention, the production capacity of 4kg / h needs to provide 1.1m 3 Catalyst flow rate per hour, what is more troublesome is that the vinyl esters in the large amount of recycled vinyl ester-rich catalysts need to be separated in time to effectively return the vinyl ester-depleted catalysts to the reaction zone. Therefore, There are great difficulties in industrial scale-up

Method used

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  • Preparation method of carboxylic acid vinyl ester

Examples

Experimental program
Comparison scheme
Effect test

example 1

[0071] Example 1 (the present invention)

[0072] see figure 1 One embodiment of the invention is shown. Carry out continuous vinylation reaction in the production equipment of the present invention, the reactor R length is 400cm, and diameter is 45cm, and guide tube diameter is 20cm, rectifying tower F is filled with the bulk packing of 5mm * 5mm (diameter * height), 20 pieces Theoretical plate, rectification column diameter 50mm. Add 640ml of neononanoic acid solution containing 40% neononanoic acid zinc (from the carboxylic acid obtained by carbonylation after dimerization of isobutylene) from tube B of reactor R, heat the reaction solution to 220°C, and 3 The speed of / h is passed into acetylene gas from A, and the excess circulating acetylene overflows from the top E of the tower and returns to A. By adjusting the flow rate of reflux D and production C, the content of vinyl ester at the production outlet is controlled. The test results are shown in the table below.

example 2

[0073] Example 2 (comparative test)

[0074] The equipment is the same as Example 1, except that the ventilation volume of acetylene is 0.15m 3 / h.

example 3

[0075] Example 3 (comparative experiment)

[0076] Equipment and condition are the same as example 1, just without rectifying tower F.

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Abstract

The invention discloses a preparation method of carboxylic acid vinyl ester. The method comprises the following steps of: undergoing a gas-liquid reaction on acetylene and carboxylic acid in a circulatory flow bubbling reactor under the action of a liquid phase catalyst, wherein the catalyst is a zinc salt or cadmium salt of the carboxylic acid; a honeycomb duct is arranged in the reactor; and a rectifying device is arranged on the top of the reactor; introducing acetylene from the bottom of the reactor; introducing a vaporization product into the rectifying device from the top of the reactor for separating; and conveying a liquid phase catalyst solution and a reflux liquid drained from the rectifying tower to the bottom of the reactor through the honeycomb duct to form high-speed circulation in the reactor. A loop reactor is adopted, and reaction rectification is used together, so that the reaction efficiency is increased greatly through the loop reactor, the transformation ratio of a product is increased through a reaction rectification technology, and the reaction energy consumption is lowered.

Description

technical field [0001] This invention relates to the catalytic conversion of carboxylic acids and acetylene to vinyl esters. Background technique [0002] Known methods commonly used to react carboxylic acids with acetylene to form vinyl esters are described in Ullman's Encyclopedia of Industrial Chemistry, A27, 430-434. The reaction of acetylene and carboxylic acid is as follows: [0003] R-COOH+C 2 h 2 →R-COO-CH=CH 2 [0004] The catalyst used in this reaction is usually a zinc salt of carboxylic acid in the reactant, which can be dissolved in excess carboxylic acid (DE1238010, DE1210810) or an inert solvent such as paraffin oil with a boiling point higher than the reaction temperature. Since the reaction is carried out at atmospheric pressure, a high acetylene cycle is required. According to the vapor partial pressure of reactants and products, the produced vinyl ester, unreacted carboxylic acid and excess recycled acetylene are discharged out of the reactor togethe...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C69/15C07C67/04
Inventor 于翔
Owner 江西元道分子化学股份有限公司