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Supported metallocene catalyst, preparation method and application thereof and methyl acrylate preparation method

A technology of metallocene catalysts and metallocene compounds, applied in the direction of catalyst activation/preparation, preparation of organic compounds, chemical instruments and methods, etc., can solve the problem of insufficient catalytic activity, achieve strong regeneration ability, improve product purity, reduce powder The effect of group reunion

Active Publication Date: 2018-11-13
CHINA PETROLEUM & CHEM CORP +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, the catalytic activity of the current silica gel carrier is not high enough after loading the metallocene compound. Therefore, it is necessary to develop an efficient and environmentally friendly catalyst for methyl acrylate

Method used

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  • Supported metallocene catalyst, preparation method and application thereof and methyl acrylate preparation method
  • Supported metallocene catalyst, preparation method and application thereof and methyl acrylate preparation method
  • Supported metallocene catalyst, preparation method and application thereof and methyl acrylate preparation method

Examples

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preparation example Construction

[0047] In the preparation method of the silica gel carrier in the prior art, the step of removing the template agent after spray drying is usually included, for example, the template agent is removed by a calcination method. Since the method of the present invention uses a ceramic membrane for filtration and / or washing treatment, the method for preparing the silica gel carrier of the present invention may not include the step of calcination to remove the template agent.

[0048] In the present invention, the average particle diameter of the silica gel carrier is 30-60 μm, and the specific surface area is 150-600 m 2 / g, the pore volume is 0.5-2.5mL / g, the pore size distribution is bimodal, and the most probable pore diameters corresponding to the bimodal are 1-4.5nm and 20-50nm.

[0049] Preferably, the silica gel carrier has an average particle diameter of 30-60 μm and a specific surface area of ​​200-400 m 2 / g, the pore volume is 1-2mL / g, the pore diameter distribution is ...

Embodiment 1

[0072] This example is used to illustrate the supported metallocene catalyst of the present invention and its preparation method

[0073] (1) Preparation of silica gel carrier

[0074] Concentration is that the water glass of 15% by weight, the sulfuric acid solution of 12% by weight, n-butanol and glycerol are mixed with the weight ratio of 5:1:1:1 and contact reaction at 20 ℃ for 1.5 hours, then use Sulfuric acid with a concentration of 98% by weight adjusted the pH value to 3, and then the obtained reaction material was suction-filtered and washed with a ceramic membrane filter until the sodium ion content was 0.02% by weight to obtain a silica gel filter cake. Among them, the operating pressure of the membrane module is 3.3bar, the inlet membrane pressure of the circulation side is 4bar, the outlet membrane pressure of the circulation side is 2.5bar, the membrane surface velocity of the circulation side is 4m / s, the pressure of the permeation side is 0.3bar, and the temper...

Embodiment 2

[0086] This example is used to illustrate the supported metallocene catalyst of the present invention and its preparation method

[0087] (1) Preparation of silica gel carrier

[0088] Concentration is that the water glass of 15% by weight, the sulfuric acid solution of 12% by weight, n-butanol and glycerol are mixed with the weight ratio of 6:3:1:1 and contact reaction at 60 ℃ for 3 hours, then use Sulfuric acid with a concentration of 98% by weight adjusted the pH value to 3, and then the obtained reaction material was suction-filtered and washed with a ceramic membrane filter until the sodium ion content was 0.02% by weight to obtain a silica gel filter cake. Among them, the operating pressure of the membrane module is 3bar, the inlet membrane pressure of the circulation side is 3.5bar, the outlet membrane pressure of the circulation side is 2.5bar, the membrane surface velocity of the circulation side is 4.5m / s, the pressure of the permeation side is 0.4bar, and the temper...

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Abstract

The invention relates to the field of supported metallocene catalysts and discloses a supported metallocene catalyst, a preparation method and application thereof and a methyl acrylate preparation method. The supported metallocene catalyst comprises a silica gel supporter and metallocene supported on the silica gel supporter. A preparation method of the silica gel supporter includes the steps of firstly, mixing sodium silicate, polyol, n-butyl alcohol and inorganic acid to obtain a mixture, and using a ceramic membrane filter to perform filtering and / or washing on the obtained mixture to obtain silica gel filter cake; secondly, subjecting the silica gel filter cake obtained in the first step to ball milling, and performing spray drying to obtain the silica gel supporter. The supported metallocene catalyst has the advantages that the supported metallocene catalyst is good in catalytic performance when being used in esterification reaction, the supported metallocene catalyst is recyclable and simple in recycling process, and the recycled catalyst is still high in reaction activity.

Description

technical field [0001] The present invention relates to the field of supported metallocene catalysts, in particular to a supported metallocene catalyst, a preparation method of a supported metallocene catalyst, a metallocene catalyst obtained by the method, an application of the metallocene catalyst and a Method for the preparation of methyl acrylate. Background technique [0002] Methyl acrylate is an important industrial raw material. The traditional process uses concentrated sulfuric acid as a catalyst in the process of preparing methyl acrylate. This process corrodes equipment and pollutes the environment, and the catalyst cannot be reused. [0003] At present, the common catalyst supports are mesoporous materials and silica gel supports. Silica gel is used repeatedly because of its good fluidity, large specific surface area and high pore melting ability to adsorb catalysts, making it a good carrier for catalysts. However, the catalytic activity of the current silica g...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J31/22B01J35/10B01J21/08B01J37/00C07C67/08C07C69/54
CPCC07C67/08B01J21/08B01J31/2295B01J37/009B01J2531/46B01J2531/49B01J2531/48B01J2531/0225B01J35/617B01J35/638B01J35/69B01J35/635B01J35/615C07C69/54Y02P20/584
Inventor 亢宇张明森
Owner CHINA PETROLEUM & CHEM CORP
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