Double component carried catalyst for synthesizing diphenyl carbonate and its preparing method

A technology of supported catalyst and diphenyl carbonate, which is applied in the field of two-component supported catalyst and its preparation, can solve the problems of low yield and low efficiency of diphenyl carbonate, and achieve good repeatability, easy separation and stable good sex effect

Inactive Publication Date: 2003-01-22
HEBEI UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Although the supported catalyst has many advantages, the efficiency of the supported catalyst for the oxidative carbonylation of phenol to diphenyl carbonate is not high at present, and the yield of diphenyl carbonate is low. It is quite necessary to develop a new high-efficiency supported catalyst

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0025] Example 1 Preparation of two-component supported catalyst

[0026] 1. Grind the carrier HZSM-5 into fine particles in a mortar, sieve the 20-40 mesh HZSM-5 particles with a sampling sieve, put them in a muffle furnace for roasting at 550°C, and set aside;

[0027] 2. Take 3 grams of roasted HZSM-5, and use deionized water to measure the volume of the solution required for equal volume impregnation to 5ml;

[0028] 3. Take 0.0456 g of PdCl 2 , 0.6595 g Cu(OAc) 2 , dissolved in 5ml of ammonia water with a volume percentage of 2%-5%, let stand for a period of time until the solution is uniform;

[0029] 4. Add the impregnation solution drop by drop to 3 grams of the roasted HZSM-5 carrier, and impregnate with equal volume for 14 hours;

[0030] 5. Vacuum dry in a constant temperature water bath at 55°C for 8 hours;

[0031] 6. The dried catalyst was calcined in a muffle furnace at 550°C for 8 hours to obtain a two-component supported catalyst, which was taken out and p...

Embodiment 3

[0037] The preparation step of catalyst is identical with embodiment 1, but changes catalyst precursor PdCl 2 , Cu(OAc) 2 The consumption that makes the molar ratio of Cu, Pd also change in the prepared catalyst, as shown in table 1. Using the prepared catalyst to synthesize diphenyl carbonate by liquid-phase oxidative carbonylation, the reaction conditions are the same as in Example 2, and its catalytic performance is shown in Table 1.

[0038] Table 1 Effect of different Cu / Pd ratios on catalyst activity

[0039] Cu:Pd (molar ratio) 40 30 15 10 5

[0040] DPC * Yield / % 13.3 37.5 53.7 28.4 15.1

[0041] * DPC: diphenyl carbonate

Embodiment 4

[0043] The preparation step of catalyst is identical with embodiment 1, but changes PdCl 2 The amount of PdCl in the prepared catalyst 2 The loads vary, as shown in Table 2. The prepared catalyst was used to synthesize diphenyl carbonate by liquid-phase oxidative carbonylation, and the reaction conditions were the same as in Example 2. The catalytic performance is shown in Table 2.

[0044] Table 2 Different PdCl 2 Effect of Loading Amount on Catalyst Activity

[0045] Pd content / wt% 0.8 1 1.5 2 5

[0046] DPC * Yield / % 15.2 27.0 45.1 37.5 38.1

[0047] * DPC: diphenyl carbonate

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Abstract

The present invention relates to double-component carried catalyst PdCl2-Cu(OAc)2/zeolite for synthesizing diphenyl carbonate and its preparation. The catalyst consists of zeolite in 50-100 weight portions, PdCl2 in 0.1-10 weight portions and Cu(OAc)2 in 0.1-30 weight protions. It is prepared through equi-volume soaking and roasting at 250-750 deg.c. The catalyst system has also metal acetate as inorganic oxidation-reduction assistant, hydroquinone as organic oxidation-reduction assistant, and tetrabutyl ammonium bride as surfactant. The catalyst has very high catalytic activity and excellent selectivity to liquid phenol in synthesizing diphenyl carbonate. The catalyst is easy to separate from product, easy to recover and regenerate and has simple preparation process.

Description

technical field [0001] The invention belongs to a two-component supported catalyst and a preparation method thereof, in particular to a two-component supported catalyst PdCl for synthesizing diphenyl carbonate by phenol liquid-phase oxidative carbonylation 2 -Cu(OAc) 2 / Zeolite and its preparation method. Background technique [0002] Diphenyl carbonate is an important environmental chemical product, which can be used to synthesize many important medicines, pesticides and other organic compounds and polymer materials. The synthesis methods of diphenyl carbonate include phosgene method, transesterification method and phenol oxidative carbonylation method. The phosgene method has disadvantages such as complex process, highly toxic raw material phosgene, and serious environmental pollution, and is gradually being eliminated; the transesterification method uses dimethyl carbonate or dimethyl oxalate as raw materials, which has high cost and low reaction rate, and is harmful t...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J27/13B01J29/072B01J31/04C07C68/00
Inventor 王延吉刘宏伟赵茜赵新强
Owner HEBEI UNIV OF TECH
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