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Loaded phosphoric acid catalyst and preparation method thereof and preparation method of n-butyl acetate

A phosphoric acid catalyst and catalyst technology, which is applied in the preparation of organic compounds, carboxylic acid ester preparation, chemical instruments and methods, etc., can solve the problems of many side reactions, large waste liquid discharge, serious equipment corrosion, etc., and achieve good catalytic performance , less side effects

Inactive Publication Date: 2012-05-16
CHINA PETROLEUM & CHEM CORP +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0005] The purpose of the present invention is to overcome the shortcomings of existing catalysts for catalytic synthesis of n-butyl acetate, such as serious equipment corrosion, many side reactions, and large waste liquid discharges, and provide a novel catalyst for the synthesis of n-butyl acetate. Catalyst and preparation method of n-butyl acetate

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  • Loaded phosphoric acid catalyst and preparation method thereof and preparation method of n-butyl acetate
  • Loaded phosphoric acid catalyst and preparation method thereof and preparation method of n-butyl acetate
  • Loaded phosphoric acid catalyst and preparation method thereof and preparation method of n-butyl acetate

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preparation example Construction

[0018] The present invention also provides a method for preparing a catalyst, wherein the method includes: impregnating a mesoporous silica carrier with a phosphoric acid solution, so that the phosphoric acid is loaded on the mesoporous silica carrier, and the loading amount of the phosphoric acid is such that In the obtained catalyst, based on the total weight of the catalyst, the content of the phosphoric acid is 5-60% by weight, and the content of the mesoporous silica carrier is 40-95% by weight. More preferably, based on the total weight of the catalyst, the content of the phosphoric acid is 5-10% by weight, and the content of the mesoporous silica carrier is 90-95% by weight.

[0019] 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 is 3-20 microns, and the specific surface area is 200 -300 square meters per gra...

Embodiment 1

[0036] Add 1.0 gram of three-stage copolymer polyoxyethylene-polyoxypropylene-polyoxyethylene (Aldrich Company, P123) and 1.69 gram of ethanol to the buffer solution of acetic acid and sodium acetate of pH=4.4 of 28ml, at 15 ℃ Stir until the polyoxyethylene-polyoxypropylene-polyoxyethylene is completely dissolved, then add 6g of trimethylpentane to the above solution, stir at 15°C for 8 hours, then add 2.13g of tetramethoxysilane to the above In the solution, after stirring for 20 hours at 15°C, transfer the solution to a polytetrafluoroethylene-lined reactor, crystallize in an oven at 60°C for 24 hours, filter, wash with distilled water, and dry to obtain hollow sphere mesoporous dioxide Silicon powder.

[0037] The hollow spherical mesoporous silica raw powder was calcined in a muffle furnace at 550° C. for 24 hours to obtain hollow spherical mesoporous silica (named MS-1).

[0038] At 35°C, 1 gram of hollow spherical mesoporous silica and 1 gram of phosphoric acid were sti...

experiment Embodiment 1

[0047] This experimental example is used to illustrate the catalytic activity of the supported phosphoric acid catalyst according to the present invention.

[0048] Dry the supported phosphoric acid catalyst (MS-HP)v in vacuum at 150°C for 6 hours, and after cooling to room temperature, weigh 0.4g, then weigh 18.5g of n-butanol and 6g of acetic acid, and put them into 100ml of In the three-necked flask, it was stirred for 3 hours under the heating condition of 120°C. After cooling to room temperature, it was centrifuged to recover the solid catalyst therein, and the liquid composition of the reaction product was analyzed by gas chromatography. Ester selectivity was 99%. It is determined through calculation that the catalytic efficiency of the catalyst is 99%.

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Abstract

The invention provides a loaded phosphoric acid catalyst, and the catalyst comprises a hollow ball mesoporous silica carrier and phosphoric acid loaded on the hollow ball mesoporous silica carrier; on a basis of the total weight of the catalyst, the content of the phosphoric acid is 5-60 wt%, and the content of the hollow ball mesoporous silica carrier is 40-95 wt%. The invention also provides a preparation method of the catalyst. In addition, the invention also provides a preparation method of the loaded phosphoric acid catalyst of n-butyl acetate. The loaded phosphoric acid catalyst of the invention can be recovered and used repeatedly; compared with a homogeneous catalyst of concentrated sulfuric acid, the loaded phosphoric acid catalyst has better catalytic performance, less side reactions, and does not cause corrosion to equipment.

Description

technical field [0001] The invention relates to a supported phosphoric acid catalyst and a preparation method thereof, and also relates to a preparation method of n-butyl acetate using the catalyst. Background technique [0002] N-Butyl Acetate is a colorless transparent liquid with a strong banana-like aroma and can be used as a food flavoring according to the national regulations of GB2760-86. At the same time, n-butyl acetate can also be used as a solvent for natural rubber and synthetic resins. In addition, n-butyl acetate can also be used as an extractant in petroleum processing. [0003] The traditional synthesis method of n-butyl acetate is under the catalysis of homogeneous catalyst (sulfuric acid), synthesizes by esterification method, but the shortcoming that this method exists is that sulfuric acid corrodes equipment seriously, side reaction is many, and waste liquid discharge amount Big and other shortcomings. [0004] Therefore, developing a novel catalyst for...

Claims

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Application Information

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IPC IPC(8): B01J27/182C07C69/14C07C67/08
Inventor 亢宇谢伦嘉郭顺王彦强赵思源姜健准田宇凌永泰
Owner CHINA PETROLEUM & CHEM CORP