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Catalyst for synthesizing phenyl-methyl-formater, its preparing and applicating method

A technology of methyl phenylcarbamate and an application method, applied in the field of TiO2-ZnO catalysts, can solve the problems of unrecyclable homogeneous catalysts, difficult product separation, unfriendly environment, etc., and achieves high repeatability, easy separation and recovery, and stability. good effect

Inactive Publication Date: 2006-10-25
HEBEI UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0010] The technical problem to be solved by the present invention is: provide a kind of TiO that synthesizes methyl phenylcarbamate to use 2 -ZnO catalyst and its preparation and application method, the catalyst is a highly active heterogeneous catalyst, used for the synthesis of methyl phenylcarbamate by dimethyl carbonate amination method, overcoming the inability of the homogeneous catalyst to be recycled and separated from the product Difficulty, and the existing heterogeneous catalysts have the disadvantages of being unfriendly to the environment and having low activity

Method used

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  • Catalyst for synthesizing phenyl-methyl-formater, its preparing and applicating method

Examples

Experimental program
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Effect test

Embodiment 1

[0027] (1) Weigh 0.015mol of tetrabutyl titanate, dissolve it in 100ml of anhydrous methanol, and make a solution with a concentration of 0.15mol / L;

[0028] (2) Add deionized water dropwise to the tetrabutyl titanate methanol solution prepared in step (1), until the tetrabutyl titanate is completely hydrolyzed;

[0029] (3) Vacuum suction filtration of the hydrolyzate of tetrabutyl titanate obtained in step (2), and washing with the same amount of deionized water as in step (2);

[0030] (4) According to the molar weight and molar ratio of tetrabutyl titanate taken in (1) step ZnO: TiO 2 =1:1 calculation, weigh 0.015mol Zn(OOCCH 3 ) 2 2H 2 O, dissolved in 10ml of water to make a solution with a concentration of 1.5mol / L, mix the solution with the hydrolyzate of tetrabutyl titanate prepared in step (3), and dry at 80°C for 8 hours to obtain a catalyst precursor ;

[0031] (5) the catalyst precursor that (4) step makes is roasted 8 hours at 500 ℃, makes the TiO that synthe...

Embodiment 2-4

[0033] Identical to the preparation method of Example 1, just changing the roasting temperature of the catalyst precursor in the step (5) is respectively 400°C, 600°C, and 700°C to obtain the respective TiO used for the synthesis of methyl phenylcarbamate of the present invention. 2 - ZnO catalyst.

Embodiment 5-7

[0035] Same as the preparation method of Example 1, just change Zn(OOCCH 3 ) 2 2H 2 The amount of O used is 0.03mol, 0.0075mol, 0.0038mol, respectively, dissolved in 10ml of water to prepare solutions with concentrations of 3mol / L, 0.75mol / L, and 0.38mol / L, so that the molar ratio ZnO:TiO 2 Respectively 1: 0.5, 1: 2, 1: 4, make respective TiO used for synthesizing methyl phenylcarbamate of the present invention 2 - ZnO catalyst.

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Abstract

The present invention relates to a catalyst for synthesizing methyl carbanilate, its preparation process and application method. Said catalyst is formed from TiO2 and ZnO according to mole ratio of 1:0.2-5. The catalyst, phenylamine and methyl carbonate are added into a high-pressure kettle, heated to 90-200 deg.C and reacted for 1-20 hr so as to obtain the invented product methyl carbanilate. Said invention also provides the concrete steps of its preparation method of said catalyst.

Description

technical field [0001] The technical solution of the present invention relates to a catalyst comprising titanium dioxide and zinc oxide, specifically a TiO 2 -ZnO catalyst and methods for its preparation and application. technical background [0002] Methyl phenylcarbamate (MPC for short) is an intermediate for the synthesis of diphenylmethane diisocyanate (MDI for short). MDI is one of the important raw materials for the synthesis of polyurethane. Its polyurethane products are widely used in electromechanical, shipbuilding, aviation, civil engineering, light In industries such as industry. The synthesis methods of MDI are mainly divided into phosgene method and non-phosgene method, and phosgene method is the main method of industrialization at present. Due to the shortcomings of the phosgene method, such as highly toxic raw materials and by-product hydrochloric acid corrosion of equipment, people have paid more attention to the development of non-phosgene methods in recen...

Claims

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Application Information

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IPC IPC(8): B01J23/06B01J21/06C07C269/06C07C271/28
Inventor 王延吉李芳赵新强
Owner HEBEI UNIV OF TECH
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