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Load-type phosphotungstic acid catalyst and preparation method thereof as well as n-butyl acrylate preparation method

A technology of phosphotungstic acid and catalyst, which is applied in the field of preparation of n-butyl acrylate, can solve the problems of complex post-treatment process, equipment corrosion, and many side reactions, and achieve less side reactions, good catalytic performance, and simple post-treatment process Effect

Inactive Publication Date: 2013-03-06
CHINA PETROLEUM & CHEM CORP +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0007] The purpose of the present invention is to overcome the shortcomings of existing catalysts for catalytic synthesis of n-butyl acrylate, such as serious equipment corrosion, many side reactions, and complicated post-treatment processes, and to provide a novel catalyst for the synthesis of n-butyl acrylate. And the preparation method of n-butyl acrylate

Method used

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  • Load-type phosphotungstic acid catalyst and preparation method thereof as well as n-butyl acrylate preparation method
  • Load-type phosphotungstic acid catalyst and preparation method thereof as well as n-butyl acrylate preparation method
  • Load-type phosphotungstic acid catalyst and preparation method thereof as well as n-butyl acrylate preparation method

Examples

Experimental program
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Effect test

Embodiment approach

[0024] According to one embodiment of the present invention, the preparation method of the supported phosphotungstic acid catalyst comprises: stirring a hollow mesoporous silica carrier, n-butanol and phosphotungstic acid at a temperature of 100-150°C for 0.5-72 hours After suction filtration, according to molar ratio, hollow spherical mesoporous silica carrier: n-butanol: phosphotungstic acid = 1: 10-50: 0.005-0.1, preferably hollow spherical mesoporous silica carrier: n-butanol: Phosphotungstic acid = 1: 10-20: 0.01-0.06, more preferably hollow spherical mesoporous silica carrier: n-butanol: phosphotungstic acid = 1: 10.51: 0.02, and then dry the solid with nitrogen to obtain a supported Hollow spheres of mesoporous silica of phosphotungstic acid.

[0025] According to the present invention, the size of the hollow spherical mesoporous silica can be changed in a wide range, preferably, the average particle diameter of the hollow spherical mesoporous silica carrier can be 3-20...

Embodiment 1

[0044] Preparation of hollow sphere mesoporous silica support:

[0045] Add 1.0 gram of three-stage copolymer polyethylene glycol-polyglycerol-polyethylene glycol (Aldrich Company, P123) and 1.69 gram of ethanol into the buffer solution (pH=4.4) of acetic acid and sodium acetate of 28ml, in Stir at 15°C until polyethylene glycol-polyglycerol-polyethylene glycol is completely dissolved, then add 6g of trimethylpentane to the above solution, stir at 15°C for 8 hours, then add 2.13g of tetramethoxy Add base silane to the above solution, stir at 15°C for 20 hours, transfer the solution to a polytetrafluoroethylene-lined reaction kettle, and crystallize in an oven at 120°C for 30 hours, then filter, wash with distilled water, and dry to obtain a hollow Spherical mesoporous silica raw powder.

[0046] The hollow spherical mesoporous silica raw powder was calcined in a muffler furnace at 550° C. for 24 hours to obtain hollow spherical mesoporous silica (named MS-1).

[0047] Prepar...

experiment Embodiment 1

[0072] This experimental example is used to illustrate the catalytic activity of the supported phosphotungstic acid catalyst according to the present invention.

[0073] The supported phosphotungstic acid catalyst (MS-HPA) in Example 1 was vacuum-dried at 150°C for 6 hours, and after cooling to room temperature, weighed 0.4 grams, then weighed 8.9 grams of n-butanol and 7.2 grams of acrylic acid, and Put them into a 100ml three-neck flask in turn, stir for 4 hours under heating at 130°C, cool to room temperature, centrifuge, recover the solid catalyst therein, and analyze the composition of the reaction product liquid by gas chromatography. The result is: the conversion of acrylic acid is 90%, and the selectivity to n-butyl acrylate was 87%.

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Abstract

The invention provides a load-type phosphotungstic acid catalyst. The catalyst comprises a hollow-sphere mesoporous silica carrier and phosphotungstic acid loaded on the hollow-sphere mesoporous silica carrier. When the total weight of the catalyst is taken as a reference, the content of the phosphotungstic acid is 5-50 wt%, and the content of the hollow-sphere mesoporous silica carrier is 50-95 wt%. The invention further provides a preparation method of the load-type phosphotungstic acid catalyst and an n-butyl acrylate preparation method with the load-type phosphotungstic acid catalyst. The load-type phosphotungstic acid catalyst provided by the invention can be repeatedly used through recovery, has better catalytic performance compared with that of a homogeneous catalyst, namely concentrated sulfuric acid, and does not erode equipment.

Description

technical field [0001] The invention relates to a supported phosphotungstic acid catalyst and a preparation method thereof, and also relates to a preparation method of n-butyl acrylate using the catalyst. Background technique [0002] N-butyl acrylate (abbreviated as BA) is a colorless and transparent liquid, flammable, prone to self-polymerization or copolymerization, and is an important monomer for synthetic polymers. Adhesives, etc., are also used in textile auxiliaries. [0003] At present, the main synthesis method of n-butyl acrylate is to synthesize by esterification under the catalysis of sulfuric acid and heteropoly acid, etc., but the disadvantages of this method are that sulfuric acid causes serious corrosion to equipment, many side reactions, and the amount of waste liquid discharge Big and other shortcomings. Phosphotungstic acid H 3 PW 12 o 40 (referred to as HPA) is a very strong acidic catalyst, mainly used for homogeneous and heterogeneous organic catal...

Claims

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Application Information

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IPC IPC(8): B01J31/18B01J35/10C07C69/54C07C67/08
Inventor 亢宇张明森黄文氢郭顺
Owner CHINA PETROLEUM & CHEM CORP
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