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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  • 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 a

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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Example Embodiment

[0033] Example 1

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

[0035] After weighing a certain amount of N- methylimidazole in the reactor, is condensed under reflux in 10-100mL / s rate was slowly added dropwise amount of n-butyl chloride, the reaction temperature was controlled at 70 ℃, 26h is the reaction, the The reaction solution was filtered off and washed 4 times with acetonitrile by rotary evaporation, and dried 70 deg.] C 8h, to give a pale yellow intermediate A.

[0036] (2) Absence of a titanium-based Keggin type heteropoly acid metal substituted B- Preparation of intermediate

[0037] Weigh a quantity of sodium molybdate was dissolved in an appropriate amount of distilled water and heated to a gentle boil, adjusted to pH 4, at a reflux condenser and 10-100ml / s rate was slowly added dropwise a quantity of TiCl 4Aqueous hydrochloric acid, after 2 h, then dripped at 10-100 ml / s, a certain amount of SNCL 2 Aqueous hydrochloric acid, after completion of the...

Example Embodiment

[0040] Example 2

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

[0042] Weigh a certain amount of N-methylimidazole in the reactor, slowly drop a quantifiable chlorine nikane under 10-100 mL / s under condensation reflux, and the reaction temperature is controlled at 90 ° C, and after 22 h, The reaction liquid was washed 5 times with acetonitrile, evaporated, 90 ° C for 5 h, resulting in a light yellow intermediate A.

[0043] (2) Preparation of intermediate B-metallic substituted titanium lack keggin type heteropolyacid

[0044] Weigh a certain amount of molybdate sodium molybdate in an appropriate amount of distilled water, and heated to a microbeiled, adjusting pH 5, condensed reflux, slowly drop a certain amount of TiCl at 10-100 ml / s rate. 4 After the aqueous hydrochloride, the reaction was dripped for 2 h, the same amount of zinc acetate solution was slowly dripped at 10-100 ml / s, and then the reaction was added to 2 h, and a quantitative potassium chlo...

Example Embodiment

[0047] Example 3

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

[0049] Weigh a certain amount of N-methylimidazole in the reactor, slowly add a quantity of chlorine nikane at 10-100 ml / s under condensation reflux, and the reaction temperature is controlled at 80 ° C, and after 24 h, The reaction solution was filtered 3 times with acetonitrile, evaporated, 80 ° C for 6 h, resulting in a pale yellow intermediate A.

[0050] (2) Preparation of intermediate B-metallic substituted titanium lack keggin type heteropolyacid

[0051] Weigh a certain amount of molybdate sodium molybdate in an appropriate amount of distilled water, and heated to a microbeiled, adjusting pH 5, condensed reflux, slowly drop a certain amount of TiCl at 10-100 ml / s rate. 4 Aqueous hydrochloric acid, after the reaction is added to 2 h, the same amount of FESO is slowly dripped at 10-100 ml / s rate. 4 After 2 h, the dripping was added, and a quantitative potassium chloride was added, and wh...

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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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