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A kind of supported metallocene catalyst and its preparation method and application and the preparation method of n-butyl acetate

A metallocene catalyst, metallocene compound technology, applied in the preparation of organic compounds, chemical instruments and methods, physical/chemical process catalysts, etc., can solve the problems of easy loss of catalytic effect, complex process, equipment corrosion, etc., to prevent equipment Corrosion, reduce side reactions, and do not corrode the effect of equipment

Active Publication Date: 2015-08-19
CHINA PETROLEUM & CHEM CORP +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0006] The object of the present invention is to overcome the shortcomings such as severe equipment corrosion, complex process, and easy loss of catalytic effect in existing catalysts for catalytic synthesis of n-butyl acetate, and provide a novel catalyst for the synthesis of n-butyl acetate and its Preparation method and application and preparation method of n-butyl acetate

Method used

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  • A kind of supported metallocene catalyst and its preparation method and application and the preparation method of n-butyl acetate
  • A kind of supported metallocene catalyst and its preparation method and application and the preparation method of n-butyl acetate
  • A kind of supported metallocene catalyst and its preparation method and application and the preparation method of n-butyl acetate

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preparation example Construction

[0053] The present invention also provides a method for preparing a catalyst, wherein the method comprises: ball milling the doughnut-shaped mesoporous silica carrier together with a metallocene compound, and making the metallocene compound supported on the doughnut-shaped mesoporous silica On the silicon carrier, based on the total weight of the donut-shaped mesoporous silica carrier and the metallocene compound, the amount of the metallocene compound is 0.1-2% by weight, and the amount of the donut-shaped mesoporous silica carrier The amount is 98-99.9% by weight, more preferably, based on the total weight of the donut-shaped mesoporous silica carrier and the metallocene compound, the amount of the metallocene compound is 0.15-1.5% by weight, the donut The dosage of the shape mesoporous silica carrier is 98.5-99.85% by weight.

[0054] According to the present invention, the particle diameter of the donut-shaped mesoporous silica carrier is 3-20 microns, preferably 3-10 micr...

Embodiment approach

[0056] According to one embodiment of the present invention, the preparation method of the supported metallocene catalyst comprises: adding the doughnut-shaped mesoporous silica and the metallocene compound into the ball milling tank of the ball mill, and the inner wall of the ball milling tank is polytetrafluoroethylene Vinyl lining, the diameter of the grinding ball is 2-3mm, and the rotation speed is 300-500r / min. Continuously grind for 0.1-100 hours at a temperature of 15-100° C. in a ball mill tank, and then take out the solid powder to obtain donut-shaped mesoporous silica loaded with metallocene. The number of grinding balls depends on the size of the grinding jar, for a grinding jar size of 50-150ml, 1 grinding ball can be used. The material of the grinding ball can be agate, polytetrafluoroethylene, preferably polytetrafluoroethylene.

specific Embodiment approach

[0057] According to a specific embodiment of the present invention, the preparation method of the supported metallocene catalyst comprises the following steps:

[0058] In the first step, the triblock copolymer polyethylene oxide-polyoxypropylene-polyethylene oxide (EO 20 PO 70 EO 20 , abbreviated as P123) and N, N-dimethylformamide (DMF), added to hydrochloric acid, according to the molar feed ratio,

[0059] Tri-block copolymer polyethylene oxide-polyoxypropylene-polyoxyethylene: N, N-dimethylformamide (DMF): water: hydrogen chloride = 1: 300-700: 10000-20000: 100-500 (actual ratio 1:596:11411:326), where the molar number of polyoxyethylene-polyoxypropylene-polyoxyethylene is calculated based on the average molecular weight of polyoxyethylene-polyoxypropylene-polyoxyethylene,

[0060] Mix until the solids are fully dissolved;

[0061] In the second step, add tetraethyl orthosilicate to the solution obtained in the previous step, stir for 1-10 minutes at a temperature of ...

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Abstract

The invention discloses a supported metallocene catalyst, a preparation method thereof, and an n-butyl acetate preparation method. The catalyst is composed of 98-99.9wt% of a support and 0.1-2wt% of a metallocene supported on the support, and the support is donut-shaped meso-porous silica; and the particle diameter and the specific surface area of the support are 3-20mum and 600-1000m<2> / g respectively; and the structure of the metallocene is represented by formula 1. In the catalyst, the metallocene is supported on the specific donut-shaped meso-porous silica support, so the esterifying catalysis activity of the supported metallocene catalyst is high, and is still high after repeated use, thereby the supported metallocene catalyst can be recovered and recycled. The formula 1 is shown in the specification.

Description

technical field [0001] The invention relates to a supported metallocene catalyst and its preparation method, and also relates to the application of the catalyst in esterification reaction and the preparation method of n-butyl acetate. Background technique [0002] In 1992, Mobile Company synthesized mesoporous material (Beck J S, Vartuli J C, Roth W J, et al. J. Am. Chem. Soc., 1992, 114(27): 10834-10843), which has high The specific surface, regular pore structure and narrow pore size distribution have made mesoporous materials attract great attention in the fields of catalysis, separation, medicine and other fields; in 1998, Zhao Dongyuan and others synthesized a new type of material - mesoporous material SBA -15 (D.Y.Zhao, J.L.Feng, Q.S.Huo, et al Science 279 (1998) 548-550), the material has a highly ordered cubic single crystal mesoporous material pore size (6-30nm), large pore volume (1.0cm 3 / g), high mechanical strength maintained by thicker pore walls (4-6nm), and ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): B01J31/22C07C67/08C07C69/14
CPCY02P20/584
Inventor 亢宇张明森杨菁王洪涛张伟
Owner CHINA PETROLEUM & CHEM CORP