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Supported phosphotungstic acid catalyst and preparation thereof, and preparation method of methyl acetate

A phosphotungstic acid and catalyst technology, applied in the field of supported phosphotungstic acid catalyst and its preparation, can solve the problems of complex post-treatment process, many side reactions, equipment corrosion, etc., and achieve low price, less side reactions, and no corrosion of equipment. Effect

Active Publication Date: 2013-03-13
CHINA PETROLEUM & CHEM CORP +1
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  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0006] The purpose of the present invention is to overcome the shortcomings of existing catalysts for catalytic synthesis of methyl acetate, such as serious equipment corrosion, many side reactions, and complicated post-treatment processes, and provide a novel catalyst for synthesizing methyl acetate and acetic acid The preparation method of methyl ester

Method used

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  • Supported phosphotungstic acid catalyst and preparation thereof, and preparation method of methyl acetate
  • Supported phosphotungstic acid catalyst and preparation thereof, and preparation method of methyl acetate
  • Supported phosphotungstic acid catalyst and preparation thereof, and preparation method of methyl acetate

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Embodiment approach

[0032] According to one embodiment of the present invention, the preparation method of the supported phosphotungstic acid catalyst comprises: stirring a spherical mesoporous silica carrier, methanol and phosphotungstic acid at a temperature of 100-150° C. for 0.5-72 hours, and then pumping Filtration, in molar ratio, spherical mesoporous silica carrier (calculated as silica): methanol; phosphotungstic acid=1: 10-50: 0.005-0.1, preferably spherical mesoporous silica carrier: methanol: phosphorus Tungstic acid = 1: 15-25: 0.065-0.095, more preferably a spherical mesoporous silica carrier: methanol: phosphotungstic acid = 1: 18.02: 0.08, and then dry the solid with nitrogen to obtain a carrier of phosphotungstic acid Spherical mesoporous silica.

[0033] According to the present invention, the size of the spherical mesoporous silica can be changed in a wide range. Preferably, the average particle diameter of the spherical mesoporous silica carrier is 20-80 microns, and the specif...

specific Embodiment approach

[0034] According to a specific embodiment of the present invention, the preparation method of the supported phosphotungstic acid catalyst comprises the following steps:

[0035] In the first step, the three-block copolymer polyoxyethylene-polyoxypropylene-polyoxyethylene and N,N-dimethylformamide (DMF) are added to aqueous hydrochloric acid, and the molar feed ratio is

[0036] Tri-block copolymer polyethylene oxide-polyoxypropylene-polyoxyethylene: N, N-dimethylformamide (DMF): water: hydrogen chloride = 1: 300-700: 10000-20000: 100-500, preferably 1: 550-650: 10000-13000: 150-480, particularly preferably 1: 596: 11411: 326, wherein, the molar number of polyethylene oxide-polyoxypropylene-polyoxyethylene is based on polyethylene oxide-polyoxypropylene- The average molecular weight of polyethylene oxide was calculated as,

[0037] Stir at 25-60°C until dissolved;

[0038] In the second step, add ethyl orthosilicate to the solution obtained in the previous step, stir at 25-60...

Embodiment 1

[0058] This example is used to illustrate the supported phosphotungstic acid catalyst and its preparation method according to the present invention.

[0059] Add 2.0 grams of P123 and 15 grams of N,N-dimethylformamide (DMF) and 64ml of water to 11.2 grams of 37% hydrochloric acid, stir at 40°C until P123 is completely dissolved; then add 4.45 grams of orthosilicic acid Add ethyl ester to the above solution and stir at 40°C for 1 hour, then add 1 gram of industrial ES955 silica gel (particle diameter is 15-60 microns), crystallize at 120°C for 30 hours, filter, wash and dry to obtain the original powder Porous material: The original powder mesoporous material was calcined in a muffle furnace at 600°C for 24 hours to remove the template agent and obtain spherical mesoporous silica (named GJ-MBQ).

[0060] The above-mentioned spherical mesoporous silica GJ-MBQ was calcined at 400° C. for 10 hours under the protection of nitrogen to remove hydroxyl groups and residual moisture, th...

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Abstract

The invention provides a supported phosphotungstic acid catalyst which comprises a spherical mesoporous silica carrier and phosphotungstic acid supported on the spherical mesoporous silica carrier; on a basis of total weight of the catalyst, the catalyst comprises 10-50 wt% of the phosphotungstic acid, and 50-90 wt% of the spherical mesoporous silica carrier. The invention also provides a preparation method of the supported phosphotungstic acid catalyst. In addition, the invention also provides a preparation method of methyl acetate by using the supported phosphotungstic acid catalyst. The supported phosphotungstic acid catalyst of the invention can be recovered for recycle; when compared with a homogeneous catalyst-concentrated sulfuric acid, the supported phosphotungstic acid catalyst has better catalytic performance, and cause no corrosion to equipment.

Description

technical field [0001] The invention relates to a supported phosphotungstic acid catalyst and a preparation method thereof, and also relates to the application of the catalyst in the synthesis of methyl acetate. Background technique [0002] Methyl acetate is an important organic raw material with a wide range of uses, and can be used to synthesize acetic acid, acetic anhydride, methyl acetate, vinyl acetate and acetamide. [0003] The traditional synthetic method of methyl acetate is under the catalysis of homogeneous catalyst (sulfuric acid), synthesizes by esterification, but the shortcoming that this method exists is that sulfuric acid is serious to equipment corrosion, and conversion rate is low, shortcoming such as long reaction time. Moreover, methyl acetate can form an azeotrope with water or methanol, which is difficult to separate, and it is difficult to obtain high-purity methyl acetate (references: Wu Wenbing, Chen Liang, Zhang Shiling, New Progress in Methyl Ace...

Claims

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Application Information

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IPC IPC(8): B01J27/188B01J35/08C07C69/14C07C67/08
CPCY02P20/584
Inventor 亢宇张明森郭顺张伟杨菁梁中伟
Owner CHINA PETROLEUM & CHEM CORP
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