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Bi2O3-PbO-SBA-15 catalyst for synthesis of methylphenyl carbonate and preparation method and application of Bi2O3-PbO-SBA-15 catalyst

A technology of methyl phenyl carbonate, bi2o3-pbo-sba-15, applied in the direction of organic carbonate preparation, physical/chemical process catalyst, molecular sieve catalyst, etc., can solve the problem of unsatisfactory catalyst stability, low MPC selectivity, MPC has problems such as poor selectivity, and achieves the effects of easy separation, recovery and recycling, environmental friendliness, and good catalytic activity

Active Publication Date: 2019-10-18
HENAN INST OF SCI & TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Adopt Lewis acid homogeneous catalyst to be used for DMC and DPC transesterification to synthesize MPC, although can obtain the MPC of high purity, the stability of MPC yield and catalyst is all unsatisfactory; Loaded catalyst is used for DMC and DPC transesterification to synthesize MPC, Although the yield is high, the selectivity of MPC is poor, and the stability of the catalyst is also poor, so it is difficult to reuse; the bimetallic composite oxide catalyst is used to synthesize MPC by transesterification of DMC and DPC. Although it has good stability and can be reused, MPC less selective

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0027] A kind of Bi for synthesizing methyl phenyl carbonate 2 o 3 -PbO-SBA-15 catalyst, Pb in the catalyst 2+ with Bi 3+ The molar ratio of Bi is 6:1, Bi 2 o 3 The mass ratio of the mass sum of PbO and SBA-15 is 1:7.

[0028] The specific preparation method is as follows:

[0029] S1, Preparation of SBA-15

[0030] Add 10.0 g of triblock copolymer P123 into 300 mL of HCl solution with a concentration of 2.0 mol / L, and heat to 40 ° C under stirring conditions to completely dissolve the triblock copolymer P123 to obtain a transparent solution;

[0031] Slowly add 20.0g TEOS dropwise into the transparent solution, age for 24h under agitation, then transfer to a hydrothermal kettle and crystallize at 100°C for 24h to obtain the reaction product; the reaction product is washed 3 times with deionized water and ethanol respectively After filtration, the product was dried at 100°C for 12 hours, and then calcined at 500°C for 5 hours to obtain SBA-15;

[0032] S2, preparation ...

Embodiment 2

[0035] A kind of Bi for synthesizing methyl phenyl carbonate 2 o 3 -PbO-SBA-15 catalyst, Pb in the catalyst 2+ with Bi 3+ The molar ratio of Bi is 6:1, Bi 2 o 3 The mass ratio of the mass sum of PbO and SBA-15 is 1:7.

[0036] The specific preparation method is as follows:

[0037] S1, Preparation of SBA-15

[0038] SBA-15 preparation method is exactly the same as embodiment 1;

[0039] S2, Bi 2 o3 - Preparation of PbO-SBA-15 catalyst

[0040] Prepare the SBA-15 prepared in S1 into a SBA-15 suspension with a concentration of 0.2 g / mL, then add 0.79 g of lead nitrate and 0.15 g of bismuth acetate to 22 mL of the SBA-15 suspension, and heat under stirring to 50°C, mix well, then add ammonium carbonate dropwise until the pH of the solution is 9.5, then place the reaction solution at room temperature to age for 12 hours to obtain the reaction product, which is filtered and washed with deionized water and ethanol respectively to neutral, dried at 110°C for 24h, and then c...

Embodiment 3

[0042] A kind of Bi for synthesizing methyl phenyl carbonate 2 o 3 -PbO-SBA-15 catalyst, Pb in the catalyst 2+ with Bi 3+ The molar ratio of Bi is 6:1, Bi 2 o 3 The mass ratio of the mass sum of PbO and SBA-15 is 1:7.

[0043] The specific preparation method is as follows:

[0044] S1, Preparation of SBA-15

[0045] SBA-15 preparation method is exactly the same as embodiment 1;

[0046] S2, Bi 2 o 3 - Preparation of PbO-SBA-15 catalyst

[0047] Prepare the SBA-15 prepared in S1 into a SBA-15 suspension with a concentration of 0.15g / mL, then add 0.67g of lead chloride and 0.19g of bismuth nitrate pentahydrate into 29mL of the SBA-15 suspension, and stir Heated to 80°C under conditions to make it evenly mixed, then added ammonium carbonate dropwise until the pH of the solution was 10.0, and then aged the reaction solution at room temperature for 18 hours to obtain the reaction product, which was filtered and washed with deionized water and ethanol Bi 2 o 3 - PbO-SBA...

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Abstract

The invention discloses a Bi2O3-PbO-SBA-15 catalyst for synthesis of methylphenyl carbonate. The molar ratio of Pb<2+> to Bi<3+> in the catalyst is (5-6):1, and the mass ratio of the mass sum of Bi2O3and PbO to SBA-15 is 1:(4-24). The invention also provides a preparation method for the Bi2O3-PbO-SBA-15 catalyst for synthesis of methylphenyl carbonate. The synthesized Bi2O3-PbO-SBA-15 catalyst has the characteristics of a convenient and controllable synthesis route, a stable structure and the like, and has good catalytic activity for a transesterification reaction, so that MPC has high yieldand selectivity. The prepared catalyst is environmentally friendly, has the advantages of easy separation and recycling and good recycled use stability, and is a novel green catalyst.

Description

technical field [0001] The invention belongs to the technical field of organic synthesis catalysts, and specifically discloses a Bi 2 o 3 -PbO-SBA-15 catalyst, preparation method and application. Background technique [0002] As an important organic carbonate, methyl phenyl carbonate (MPC) is widely used in chemical industry, battery, pharmaceutical, material and other fields. MPC synthesis routes mainly include methyl chloroformate and phenol transesterification, phenyl chloroformate and methanol transesterification, dimethyl carbonate (DMC) and diphenyl carbonate (DPC) transesterification. The first two methods use highly toxic chloroformic esters as raw materials, which have potential safety hazards, are difficult to operate, and pollute the environment. Because DMC and DPC are transesterified to synthesize MPC, the environment is friendly, the reaction process is simple, and it is easy to operate. It is a green synthesis route and has become a research hotspot in rece...

Claims

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Application Information

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IPC IPC(8): B01J29/04C07C69/96C07C68/06
CPCB01J29/045C07C68/06B01J35/394C07C69/96
Inventor 王松林牛红英张齐英李长恭刘萍
Owner HENAN INST OF SCI & TECH
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