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Preparation method and application of titanium heteropolyacid ionic liquid catalyst

A technology of heteropolyacid anions and ionic liquids, which is applied in the direction of catalytic reaction, organic carbonate preparation, chemical instruments and methods, etc., can solve the problems of easy deactivation, easy generation of by-products, poor activity, etc., and achieve non-combustible, good Effects of thermal and chemical stability

Pending Publication Date: 2022-02-08
SHENYANG POLYTECHNIC UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0005] Purpose of the invention: the present invention proposes a preparation method and application of a titanium-based heteropolyacid ionic liquid catalyst, the purpose of which is to solve the problem of poor activity of the existing catalyst for synthesizing diphenyl carbonate by transesterification, and by-products are easily generated during the reaction process , poor stability, easy deactivation and other problems

Method used

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  • Preparation method and application of titanium heteropolyacid ionic liquid catalyst
  • Preparation method and application of titanium heteropolyacid ionic liquid catalyst
  • Preparation method and application of titanium heteropolyacid ionic liquid catalyst

Examples

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Embodiment 1

[0034] (1) Preparation of intermediate A-imidazole ionic liquid

[0035] Weigh a certain amount of N-methylimidazole in the reactor, slowly add a certain amount of chlorobutane dropwise at a rate of 10-100mL / s under the condition of condensing and reflux, and control the reaction temperature at 70°C. After 26 hours of reaction, the The reaction solution was washed and filtered with acetonitrile for 4 times, and dried at 70°C for 8 hours by rotary evaporation to obtain light yellow intermediate A.

[0036] (2) Preparation of intermediate B-metal substituted titanium-based vacancy Keggin-type heteropolyacids

[0037] Weigh a certain amount of sodium molybdate and dissolve it in an appropriate amount of distilled water, heat to a slight boil, adjust the pH to 4, condense and reflux, and slowly add a certain amount of TiCl dropwise at a rate of 10-100ml / s 4Hydrochloric acid aqueous solution, after 2 hours of reaction after the dropwise addition, slowly drop a certain amount of Sn...

Embodiment 2

[0041] (1) Preparation of intermediate A-imidazole ionic liquid

[0042] Weigh a certain amount of N-methylimidazole in the reactor, slowly add a certain amount of chlorobutane dropwise at a rate of 10-100mL / s under reflux conditions, and control the reaction temperature at 90°C. After 22 hours of reaction, the The reaction solution was washed and filtered with acetonitrile for 5 times, and then dried at 90°C for 5 hours by rotary evaporation to obtain light yellow intermediate A.

[0043] (2) Preparation of intermediate B-metal substituted titanium-based vacancy Keggin-type heteropolyacids

[0044] Weigh a certain amount of sodium molybdate and dissolve it in an appropriate amount of distilled water, heat it to a slight boil, adjust the pH to 5, condense and reflux, and slowly add a certain amount of TiCl dropwise at a rate of 10-100ml / s 4 Hydrochloric acid aqueous solution, after the reaction for 2 hours after the dropwise addition, slowly drop a certain amount of zinc acet...

Embodiment 3

[0048] (1) Preparation of intermediate A-imidazole ionic liquid

[0049] Weigh a certain amount of N-methylimidazole in the reactor, slowly add a certain amount of chlorobutane dropwise at a rate of 10-100mL / s under the condition of condensing and reflux, and control the reaction temperature at 80°C. After 24 hours of reaction, the The reaction solution was washed and filtered with acetonitrile for 3 times, and dried at 80°C for 6 hours by rotary evaporation to obtain light yellow intermediate A.

[0050] (2) Preparation of intermediate B-metal substituted titanium-based vacancy Keggin-type heteropolyacids

[0051] Weigh a certain amount of sodium molybdate and dissolve it in an appropriate amount of distilled water, heat it to a slight boil, adjust the pH to 5, condense and reflux, and slowly add a certain amount of TiCl dropwise at a rate of 10-100ml / s 4 Hydrochloric acid aqueous solution, after 2 hours of reaction after the dropwise addition, slowly drop a certain amount o...

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Abstract

The invention relates to a preparation method and application of a titanium heteropolyacid ionic liquid catalyst. The structure of the titanium heteropolyacid ionic liquid catalyst comprises metal substituted titanium deficiency Keggin type heteropolyacid anions and imidazole organic cations, and an organic-inorganic functional hybrid material is formed. The preparation method comprises the following steps: preparing an intermediate A-imidazole ionic liquid; preparing an intermediate B-metal substituted titanium system vacancy Keggin type heteropolyacid; and preparing the titanium heteropolyacid ionic liquid catalyst. The invention solves the problems of poor activity, easy generation of by-products in the reaction process, poorer stability, easy inactivation and the like of the existing catalyst for synthesizing diphenyl carbonate by a transesterification method.

Description

technical field [0001] The invention relates to the technical field of catalysts, in particular to a preparation method and application of a titanium-based heteropolyacid ionic liquid catalyst. [0002] technical background [0003] Diphenyl carbonate (DPC) is an important organic reaction intermediate, as a key raw material for the synthesis of polycarbonate by replacing highly toxic phosgene and bisphenol A. The synthesis of diphenyl carbonate by transesterification does not produce three wastes, and the utilization rate of atoms is as high as 100%. The source of its industrial chain is propylene oxide, a derivative of propylene, and the greenhouse gas CO produced by the petrochemical industry. 2 , its final product polycarbonate and H 2 O, no three wastes are produced at all, and its prospects are broad, which fully meets the requirements of the green economic development advocated by the state. [0004] So far, the catalysts for the synthesis of diphenyl carbonate by tr...

Claims

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Application Information

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IPC IPC(8): B01J31/02B01J23/885B01J23/881B01J23/28C07C68/06C07C69/96
CPCB01J31/0284B01J31/0298B01J27/19B01J23/28B01J23/881B01J23/885C07C68/06B01J2231/49C07C69/96
Inventor 郭立颖冉维婷王海玥单立宁蒋泽众徐铁军王立岩郑荣荣陈书武杨旭鹏
Owner SHENYANG POLYTECHNIC UNIV
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