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A kind of in-situ regeneration method of catalyst for producing acetonitrile by ammoniation of acetic acid

A technology of ammonification and in-situ regeneration of acetic acid, which is applied in the direction of catalyst regeneration/reactivation, physical/chemical process catalysts, chemical instruments and methods, etc. It can solve the problems of insufficient combustion of catalyst carbon deposits, easy sintering of catalysts, and successful regeneration of catalysts Low efficiency and other problems, to achieve the effect of effective regeneration and reuse, saving labor in time, and meeting the requirements of recycling

Active Publication Date: 2021-10-29
WEIFANG ZHONGHUI CHEM
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The applicant has found through research and experiments that the catalyst is easily sintered during the initial heating up and staged oxygen raising stages of this method, and the carbon deposits inside the catalyst are not fully burned, and the regeneration efficiency of the catalyst using this method is not high.

Method used

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  • A kind of in-situ regeneration method of catalyst for producing acetonitrile by ammoniation of acetic acid
  • A kind of in-situ regeneration method of catalyst for producing acetonitrile by ammoniation of acetic acid
  • A kind of in-situ regeneration method of catalyst for producing acetonitrile by ammoniation of acetic acid

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Experimental program
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Effect test

Embodiment 1

[0041] An in-situ regeneration method for a catalyst used in the process of producing acetonitrile by ammoniation of acetic acid comprises the steps of preparing a pretreatment solution, catalyst pretreatment, ultrasonic treatment, airflow contact treatment, oxidation calcining treatment, and secondary pore-forming treatment.

[0042] To configure the pretreatment solution, mix a predetermined number of N-methylpyrrolidone, acetonitrile, and water, and stir and mix at 200 RPM for 5 minutes to prepare the pretreatment solution.

[0043] The weight ratio of the N-methylpyrrolidone, acetonitrile and water is 30:90:10.

[0044] The acetonitrile has a purity greater than 99.9%, an ultraviolet light transmittance of 92% at UV200nm, 97% at 230nm, and 99% at 240nm.

[0045] The N-methylpyrrolidone has a purity greater than 99.9%, a moisture content of less than 0.02, a chromaticity of 12, and an electrical conductivity of 1.33×10 -8 s / m.

[0046] Described water is fresh water.

[...

Embodiment 2

[0059] An in-situ regeneration method for a catalyst used in the process of producing acetonitrile by ammoniation of acetic acid comprises the steps of preparing a pretreatment solution, catalyst pretreatment, ultrasonic treatment, airflow contact treatment, oxidation calcining treatment, and secondary pore-forming treatment.

[0060] To prepare the pretreatment solution, mix a predetermined number of N-methylpyrrolidone, acetonitrile, and water, and stir and mix at 250 RPM for 10 minutes to prepare the pretreatment solution.

[0061] The weight ratio of the N-methylpyrrolidone, acetonitrile and water is 50:80:10.

[0062] The acetonitrile has a purity greater than 99.9%, an ultraviolet light transmittance of 92% at UV200nm, 97% at 230nm, and 99% at 240nm.

[0063] The N-methylpyrrolidone has a purity greater than 99.9%, a moisture content of less than 0.02, a chromaticity of 12, and an electrical conductivity of 1.33×10 -8 s / m.

[0064] Described water is fresh water.

[0...

Embodiment 3

[0077] An in-situ regeneration method for a catalyst used in the process of producing acetonitrile by ammoniation of acetic acid comprises the steps of preparing a pretreatment solution, catalyst pretreatment, ultrasonic treatment, airflow contact treatment, oxidation calcining treatment, and secondary pore-forming treatment.

[0078] To configure the pretreatment solution, mix a predetermined number of N-methylpyrrolidone, acetonitrile, and water, and stir and mix at 300 RPM for 10 minutes to prepare the pretreatment solution.

[0079] The weight ratio of the N-methylpyrrolidone, acetonitrile and water is 50:85:20.

[0080] The acetonitrile has a purity greater than 99.9%, an ultraviolet light transmittance of 92% at UV200nm, 97% at 230nm, and 99% at 240nm.

[0081] The N-methylpyrrolidone has a purity greater than 99.9%, a moisture content of less than 0.02, a chromaticity of 12, and an electrical conductivity of 1.33×10 -8 s / m.

[0082] Described water is fresh water.

...

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Abstract

The invention provides an in-situ regeneration method for a catalyst used in the production of acetonitrile by the ammoniation of acetic acid, the regeneration method comprising: configuring a pretreatment liquid, catalyst pretreatment, ultrasonic treatment, airflow contact treatment, oxidation calcination treatment, and secondary pore-making treatment ; The configuration of the pretreatment liquid includes the following raw materials: N-methylpyrrolidone, acetonitrile, water. The beneficial effects of the present invention are: the specific surface area of ​​the catalyst can be changed from 50.2m before regeneration to 2 / g increased to 253‑278m 2 / g; pore volume from 0.03cm before regeneration 3 / g increased to 0.35‑0.37cm 3 / g; average pore diameter from 25.8nm before regeneration to 5.6-5.8nm after regeneration; catalytic yield increased from 65%-70% (calculated in acetic acid) before regeneration to 96.9% (calculated in acetic acid); after catalyst regeneration Compared with the new catalyst, the catalytic yield is only about 1.3% different.

Description

technical field [0001] The invention relates to the field of acetonitrile prepared by synthesis reaction, in particular to an in-situ regeneration method of a catalyst used for preparing acetonitrile by ammoniation of acetic acid. Background technique [0002] Acetonitrile is a colorless liquid, which can serve as an important reaction raw material in chemical reactions, and generally participates in reactions in the synthesis of pharmaceutical intermediates, vitamin preparation, and amino acid preparation. In addition, the more important role of acetonitrile is to play a role as a solvent. Industrial acetonitrile is often used as an excellent solvent for many reactions, and high-purity acetonitrile is mostly used as a mobile phase in liquid chromatography, or as an important solvent in biopharmaceuticals and peptide synthesis. At present, the methods for acetonitrile synthesis are mainly as follows: [0003] (1) Acrylonitrile by-product method: propylene, ammonia, etc. are...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): B01J38/02B01J38/12B01J21/20B01J21/04B01J35/10C07C253/00C07C253/20C07C255/03
CPCB01J38/52B01J38/02B01J38/12B01J21/20B01J21/04C07C253/00C07C253/20B01J35/633B01J35/647B01J35/615C07C255/03Y02P20/584
Inventor 吴绍帅袁宏李艳萍王占明张鑫刘卿李国明
Owner WEIFANG ZHONGHUI CHEM
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