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Preparation and application of compound catalyst for preparing diphenyl carbonate

A technology of diphenyl carbonate and dimethyl carbonate, applied in the field of composite heterogeneous catalysts, can solve problems such as low activity and selectivity of heterogeneous catalysts, and achieve the effect of ensuring activity and selectivity and good technical effect

Active Publication Date: 2019-04-26
CHINA PETROLEUM & CHEM CORP +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] The technical problem to be solved by this invention is the problem of heterogeneous catalyst activity and low selectivity existing in the prior art, and a new method for preparing diphenyl carbonate from dimethyl carbonate and phenol is provided, which has a catalyst The characteristics of low dosage, high activity and not easy to lose

Method used

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  • Preparation and application of compound catalyst for preparing diphenyl carbonate
  • Preparation and application of compound catalyst for preparing diphenyl carbonate

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0029] Dissolve 8g of tetrapropylammonium hydroxide and 0.1g of sodium hydroxide in 60ml of deionized water, add 3g of carbon nanospheres (20nm in diameter), heat at 80°C for 3h, add 20.8g of tetraethyl silicate and stir, transfer to In the autoclave, let it stand at 160°C for 3 days, wash the solid and dry it, then roast it at 400°C for 24h.

[0030] To obtain 10g of solid, dissolve 6g of titanium tetrachloride in 10g of toluene, mix and stir for 30min, extract the solvent toluene to obtain a white solid, impregnate with 10g of phenol, add methanol, filter and wash to obtain catalyst sample TS1. The catalyst loading is 20%, the pore size is 20nm, and the molecular sieve diameter is about 300nm.

Embodiment 2

[0032] Dissolve 8g of tetrapropylammonium hydroxide and 0.1g of sodium hydroxide in 60ml of deionized water, add 4g of carbon nanospheres (30nm in diameter), heat at 80°C for 3h, add 20.8g of tetraethyl silicate and stir, transfer to In the autoclave, let it stand at 170°C for 4 days, wash the solid and dry it, then roast it at 500°C for 24h.

[0033] To obtain 10g of solid, dissolve 6g of tetrabutyl titanate in 10g of toluene, mix and stir for 30min, extract the solvent toluene to obtain a white solid, impregnate with 10g of phenol, add methanol, filter and wash to obtain catalyst sample TS2 , The catalyst loading is 20%, the pore size is 30nm, and the molecular sieve diameter is about 400nm.

Embodiment 3

[0035] Dissolve 8g of tetrapropylammonium hydroxide and 0.1g of sodium hydroxide in 60ml of deionized water, add 5g of carbon nanospheres (50nm in diameter), heat at 80°C for 3h, add 20.8g of tetraethyl silicate, stir, and transfer to In the autoclave, let it stand at 170°C for 6 days, wash the solid and dry it, then roast it at 400°C for 48h.

[0036] Obtain 10g of solid, dissolve 6g of titanium sulfate in 10g of water, mix and stir for 30min, draw out the solvent water to obtain a white solid, impregnate with 10g of phenol, add methanol, filter, and wash to obtain a catalyst sample TS3 with catalyst loading The amount is 20%, the pore size is 50nm, and the molecular sieve diameter is about 500nm.

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Abstract

The invention relates to a catalyst for preparing diphenyl carbonate through an interesterification reaction of dimethyl carbonate and phenol and a preparation method of the catalyst. The problems oflow activity and easy loss of heterogeneous catalysts in the prior art are mainly solved. Titanium active components are confined in a nanoreactor, the catalyst is a pseudo-homogeneous heterogeneous catalyst, and comprises the nanoreactor and titanate active components. According to the technical scheme of the catalyst, the problem of catalyst loss in a reaction of synthesis of the diphenyl carbonate through interesterification of the phenol and the dimethyl carbonate is well solved, and the catalyst can be used for industrial production of the diphenyl carbonate.

Description

Technical field [0001] The invention relates to a restricted composite heterogeneous catalyst and its catalytic application in the reaction of phenol transesterification to synthesize diphenyl carbonate. technical background [0002] Diphenyl carbonate (DPC) is a raw material for the preparation of polycarbonate by non-phosgene method. Its traditional preparation method is phosgene method. Due to the potential harm of highly toxic phosgene to the environment and safe production, it is subject to policy restrictions. The process of synthesizing diphenyl carbonate by transesterification reaction of phenol (PhOH) and dimethyl carbonate (DMC) under the action of a catalyst avoids the use of highly toxic raw material phosgene, and the main by-product methanol can also be recycled as the starting raw material carbonic acid The synthesis of dimethyl ester is the most promising green process route for industrialization. [0003] Currently, the transesterification of dimethyl carbonate and...

Claims

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Application Information

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IPC IPC(8): B01J31/02B01J37/10B01J37/08B01J37/02B01J35/10C07C69/96C07C68/06
CPCC07C68/06B01J31/0214B01J31/0272B01J37/0203B01J37/082B01J37/10B01J2231/49B01J2229/186B01J35/651B01J35/647C07C69/96
Inventor 戈军伟何文军
Owner CHINA PETROLEUM & CHEM CORP
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