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Method for preparing carboxyl anhydride

A manufacturing method and technology of carboxylic anhydrides, which are applied in the field of manufacturing carboxylic anhydrides, can solve problems such as loss of rhodium catalysts, achieve the effects of reducing insoluble tars, expanding the range of reaction operations, and improving space-time yields

Inactive Publication Date: 2012-05-30
CHINA PETROCHEM DEVMENT
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0008] In many patents of the prior art, it is mentioned that tar residues are produced in the process of producing acetic anhydride and ethylene diacetate through carbonylation of esters and ethers, and the tar residues are easy to coat rhodium metal and make rhodium Catalyst loss, so the currently disclosed patented technologies all focus on the method of removing tar residue and recycling rhodium

Method used

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  • Method for preparing carboxyl anhydride
  • Method for preparing carboxyl anhydride
  • Method for preparing carboxyl anhydride

Examples

Experimental program
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Effect test

Embodiment 1

[0025] 0.29g of ethylene diacetate, 0.37g of IrCl 3 ·XH 2 O (wherein Ir atoms account for 52.5%) and 100 ml of ethanol were added into the reaction flask, heated to 100 degrees Celsius and then refluxed for 20 hours. After cooling to normal temperature, filter to obtain a black precipitated solid and a yellow-brown solution. Concentrate the yellow-brown solution and wash it with ether, then dry it to remove the solvent, and then measure the infrared spectrum of the product after the reaction ( figure 1 In (a)), and as a control experiment.

Embodiment 2

[0027] 0.22g of N-acetylimidazole, 0.37g of IrCl 3 ·XH 2 O (wherein Ir atoms account for 52.5%) and 100 ml of ethanol were added into the reaction flask, heated to 100 degrees Celsius and then refluxed for 20 hours. After being cooled to normal temperature, filter to obtain a yellow solid and a yellow solution. The yellow solution is concentrated and rinsed with ether, then dried to remove the solvent, and the infrared spectrum of the product after the reaction can be determined ( figure 1 In (b)), and as a control experiment.

Embodiment 3

[0029] 0.29g of ethylene diacetate, 0.22g of N-acetylimidazole, 0.37g of IrCl 3 ·XH 2 O (wherein Ir atoms account for 52.5%) and 100 ml of ethanol were added into the reaction flask, heated to 100 degrees Celsius and then refluxed for 20 hours. After being cooled to normal temperature, filter to obtain a yellow solid and a yellow solution. The yellow solution is concentrated and rinsed with ether, then dried to remove the solvent, and the infrared spectrum of the product after the reaction can be determined ( figure 1 in (c)).

[0030] By comparing the infrared spectrograms of embodiment 3 and embodiment 1 and embodiment 2, it can be clearly seen that the spectrogram signal of embodiment 3 is similar to the spectrogram signal of embodiment 2, that is, the N-acetyl imidazole and iridium ion Coordinating power is better. It shows that the addition of such protective agent in the present invention does have the effect of preventing the interaction between ethylene diacetate an...

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Abstract

The present invention relates to a method for preparing carboxyl anhydride. The method comprises adopting carboxylate derived from alcohol and carboxylic acid and carbon monoxide containing a small amount of hydrogen gas as raw material, and allowing oxonation in a liquid reaction medium in the presence of group VIIIB catalyst to produce carboxyl anhydride. The liquid reaction medium includes the group VIIIB catalyst, organic halide, carboxylate, alkali metal salt, carboxyl anhydride, carboxylic acid, a protectant N-acetylimidazole, and an organic additive ethylidene diacetate (EDA). The method avoids reaction of metal ions and EDA and decreases insoluble tar generated during reaction by using the protectant N-acetylimidazole, and improves whole oxonation rate by maintaining the content of the organic additive EDA at a constant level.

Description

technical field [0001] The invention relates to a method for producing carboxylic anhydride by carbonylation of derivatives of alcohols and carboxylic acids with carbon monoxide, in particular to a method for producing acetic anhydride by carbonylation of methyl acetate and carbon monoxide. Background technique [0002] Acetic anhydride is a well-known and commonly used chemical industry raw material. Its main use is to manufacture cellulose acetate chemicals, and it is also an important raw material for the synthesis of chemicals such as drugs, spices, and dyes. At present, there are three methods for producing acetic anhydride in the industrial process, which are ketene method, acetaldehyde oxidation method and methyl acetate carbonylation method. Among them, the ketene method, which belongs to the old process, is small in scale and has many manufacturers, is the mainstream, but due to Due to its high energy consumption and many disadvantages, the largest commercial produc...

Claims

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Application Information

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IPC IPC(8): C07C53/12C07C51/56
Inventor 王慧婷蔡嘉荣沈佳慧
Owner CHINA PETROCHEM DEVMENT
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