Preparation method of catalyst for synthesizing diphenyl carbonate through transesterification

A technology of diphenyl carbonate and catalyst, which is applied in the field of preparation of catalyst for transesterification synthesis of diphenyl carbonate, can solve the problems of difficult separation, easy deactivation, difficult recycling, etc., and achieves increased dispersity, high activity and selectivity The effect of improving the adsorption speed and penetration speed

Active Publication Date: 2019-09-20
湖北三宁碳磷基新材料产业技术研究院有限公司 +1
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0004] The invention provides a method for preparing a catalyst for synthesizing diphenyl carbonate by transesterification, which can solve the problems of difficult separation, easy deactivation and difficult recycling of existing catalysts, and has high stability, high activity, easy separation and regeneration The advantages

Method used

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  • Preparation method of catalyst for synthesizing diphenyl carbonate through transesterification
  • Preparation method of catalyst for synthesizing diphenyl carbonate through transesterification
  • Preparation method of catalyst for synthesizing diphenyl carbonate through transesterification

Examples

Experimental program
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Effect test

Embodiment 1

[0024] Using nitric acid with a mass concentration of 5wt%, fully mix 5% zinc oxide, 10% silicon dioxide and 85% alumina by mass fraction, extrude into a rod, with a diameter of about 1 mm, dry at 20°C for 2 hours, and dry at 50°C for 6 hours , calcined at 500°C for 5h, and cut into about 1cm to obtain Catalyst 1.

[0025] Phenol and dimethyl carbonate carry out pressurized reaction under the above-mentioned catalyst, transesterification obtains methyl phenyl carbonate, the molar ratio of dimethyl carbonate and phenol is 1, and catalyst dosage is 0.1wt%, pressure 0.5MPa, reaction time 5h. The reaction is carried out in a rectification tower with a bottom temperature of 180°C, a tower top temperature of 65°C, and a reflux ratio of 5.

[0026] The methyl phenyl carbonate obtained above was subjected to a decompression reaction under the above catalyst conditions, the catalyst dosage was 0.5wt%, the pressure was 0.05MPa, the reaction temperature was 160°C, and the reaction time ...

Embodiment 2

[0028] Use nitric acid with a mass concentration of 5wt%, fully mix the mass fraction of 10% zinc oxide, 25% titanium dioxide and 65% alumina, extrude into a strip, with a diameter of about 5mm, dry at 35°C for 7h, and dry at 90°C for 4h, 450 ℃ calcination for 2 hours, and cut into about 1.5 cm to obtain catalyst 2.

[0029] Phenol and dimethyl carbonate are subjected to pressurized reaction under the above catalyst, transesterification to obtain methyl phenyl carbonate, the molar ratio of dimethyl carbonate to phenol is 3, the catalyst dosage is 1wt%, the pressure is 1.5MPa, and the reaction time is 3h . The reaction is carried out in a rectification tower with a bottom temperature of 200°C, a tower top temperature of 90°C, and a reflux ratio of 15.

[0030] The methyl phenyl carbonate obtained above was subjected to a decompression reaction under the above catalyst conditions, the catalyst dosage was 1.5wt%, the pressure was 0.7MPa, the reaction temperature was 180°C, and t...

Embodiment 3

[0032] Use nitric acid with a mass concentration of 20 wt%, fully mix the mass fraction of 20% zirconia, 45% titanium dioxide and 35% TS molecular sieve, extrude into a rod, with a diameter of about 8mm, dry at 30°C for 12h, and dry at 80°C for 5h, 400 It was calcined at ℃ for 10 hours, cut into about 0.5 cm, and catalyst 3 was obtained.

[0033] Phenol and dimethyl carbonate were subjected to pressurized reaction under the above-mentioned catalyst, transesterified to obtain methyl phenyl carbonate, the molar ratio of dimethyl carbonate to phenol was 5, the catalyst dosage was 5 wt%, the pressure was 2 MPa, and the reaction time was 1 h. The reaction is carried out in a rectification tower, the temperature of the bottom of the tower is 230°C, the temperature of the top of the tower is 50°C, and the reflux ratio is 8.

[0034] The methyl phenyl carbonate obtained above was subjected to a decompression reaction under the above catalyst conditions, the catalyst dosage was 2.0wt%,...

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Abstract

The invention discloses a preparation method of a catalyst for synthesizing diphenyl carbonate through transesterification. The method comprises the following steps: uniformly mixing a catalyst active component and a supporter by using nitric acid, shaping the mixture, drying the mixture at 20-40 DEG C for 1-15 hours, drying the mixture at 40-150 DEG C for 1-24 hours, and finally roasting the mixture at 300-900 DEG C for 1-20 hours to obtain a solid acid-base bifunctional center catalyst for synthesizing diphenyl carbonate through transesterification. The catalyst is an acid-base bifunctional catalyst and has an acid center and an alkaline center. The preparation method is extrusion molding. The formed catalyst is in the shape of bar-shaped columns, so that the problems that the homogeneous catalyst is not easy to separate and the active components of the heterogeneous catalyst are lost are solved. The catalyst prepared by the method has high activity and selectivity for transesterification of dimethyl carbonate and phenol, the phenol conversion rate can reach 50% or above, the product selectivity is greater than 99%, and the diphenyl carbonate purity is greater than 99.5%. The method is simple to operate, economic and environment-friendly, easily available in materials and easy to industrialize.

Description

technical field [0001] The invention belongs to the field of catalyst preparation, and relates to a preparation method of a catalyst for synthesizing diphenyl carbonate by transesterification. Background technique [0002] Diphenyl carbonate is an important new intermediate of engineering plastics. It is non-polluting and low-toxic. It is mainly used in the plastics industry and is often used to synthesize polycarbonate. The synthesis methods of diphenyl carbonate mainly include phosgene method, transesterification method and phenol oxidative carbonylation method. [0003] The catalysts for the synthesis of diphenyl carbonate from phenol and dimethyl carbonate are mainly divided into organotin catalysts, titanocene catalysts, supported catalysts, metal oxide catalysts, and ionic liquid catalysts. JP8188558, EP0780361, and JP10032361 introduced a class of organotitanium and organotin catalysts, such as tetrabutyl titanate, dibutyltin oxide, etc., which belong to homogeneous ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J23/06B01J29/89B01J23/28C07C68/06C07C69/96
CPCB01J23/06B01J29/89B01J23/28B01J23/002C07C68/065B01J2523/00B01J2229/186B01J2523/27B01J2523/31B01J2523/41B01J2523/47B01J2523/48B01J2523/68C07C69/96Y02P20/584
Inventor 孙苏红於国伟陈坤徐保明张小元李善华
Owner 湖北三宁碳磷基新材料产业技术研究院有限公司
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