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Spherical mesoporous sepiolite composite carrier, catalyst and preparation method and application thereof and preparation method of ethyl acetate

A composite carrier, sepiolite technology, applied in the preparation of organic compounds, catalyst carriers, chemical instruments and methods, etc., can solve the problems of complex product separation, many side reactions, large equipment investment, etc., to broaden the application field, reduce The effect of production costs

Active Publication Date: 2014-12-31
CHINA PETROLEUM & CHEM CORP +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] At present, concentrated sulfuric acid is usually used as a catalyst in the industry to synthesize ethyl acetate, which has defects such as large equipment investment, many side reactions, complicated product separation, and difficult waste liquid treatment. Therefore, in order to overcome the above defects, a new esterification method has been developed. Reaction catalyst to replace concentrated sulfuric acid, people have carried out a lot of research
Among them, solid acid, solid superacid and cation exchange resin are all relatively successful explorations as catalysts for esterification reactions. These catalysts all have high catalytic activity, but there are also some shortcomings, such as more by-products, etc.

Method used

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  • Spherical mesoporous sepiolite composite carrier, catalyst and preparation method and application thereof and preparation method of ethyl acetate
  • Spherical mesoporous sepiolite composite carrier, catalyst and preparation method and application thereof and preparation method of ethyl acetate
  • Spherical mesoporous sepiolite composite carrier, catalyst and preparation method and application thereof and preparation method of ethyl acetate

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preparation example Construction

[0031] The preparation method of spherical mesoporous sepiolite composite carrier provided by the invention comprises the following steps:

[0032] (1) In the presence of a template, trimethylpentane and ethanol, tetramethoxysilane is first contacted with an acid agent, and the product obtained after the first contact is crystallized and filtered to obtain No. 1 medium Porous material filter cake; second contacting cetyltrimethylammonium bromide, tetraethylorthosilicate and ammonia water, and filtering the product after the second contacting, to obtain No. 2 mesoporous material filter cake;

[0033] (2) performing a third contact with water glass and inorganic acid, and filtering the product obtained after the third contact to obtain a silica gel filter cake;

[0034] (3) Mix the No. 1 mesoporous material filter cake, No. 2 mesoporous material filter cake, silica gel filter cake and sepiolite evenly and ball mill, and the solid powder obtained after ball milling is slurried wi...

Embodiment 1

[0072] This example is used to illustrate the spherical mesoporous sepiolite composite carrier and catalyst provided by the present invention and the preparation method thereof.

[0073] (1) Preparation of spherical mesoporous sepiolite composite support:

[0074] Add 1.0 g of triblock copolymer P123 and 1.69 g (0.037 mol) of ethanol to 28 mL of a buffer solution of acetic acid and sodium acetate with a pH value of 4, stir at 15 °C until P123 is completely dissolved, and then add 6 g (0.053 mol) of trimethylpentane, and stirred at 15°C for 8 hours, then added 2.13 g (0.014mol) of tetramethoxysilane, then stirred at 15°C and pH 4.5 for 20 hours, and The solution was transferred to a polytetrafluoroethylene-lined reactor, and oven-crystallized at 60° C. for 24 hours. The obtained crystallized product was suction-filtered and washed four times with distilled water to obtain No. 1 mesoporous material filter cake.

[0075] At 80°C, cetyltrimethylammonium bromide and ethyl orthosil...

Embodiment 2

[0098] This example is used to illustrate the spherical mesoporous sepiolite composite carrier and catalyst provided by the present invention and the preparation method thereof.

[0099] (1) Preparation of spherical mesoporous sepiolite composite support:

[0100] Add 1.0 g of triblock copolymer P123 and 3.69 g (0.08 mol) of ethanol to 28 mL of a buffer solution of acetic acid and sodium acetate with a pH value of 5, stir at 60 °C until P123 is completely dissolved, and then add 9.14 g ( 0.08mol) of trimethylpentane, and stirred at 60°C for 1 hour, then added 4.68 grams (0.03mol) of tetramethoxysilane, then stirred at 60°C and pH value of 5.5 for 10 hours, and The solution was transferred to a polytetrafluoroethylene-lined reactor, and oven crystallized at 30° C. for 72 hours. The obtained crystallized product was suction-filtered and washed four times with distilled water to obtain No. 1 mesoporous material filter cake.

[0101] At 100°C, cetyltrimethylammonium bromide and e...

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Abstract

The invention discloses a spherical mesoporous sepiolite composite carrier, a preparation method thereof, and the spherical mesoporous sepiolite composite carrier prepared by the preparation method, a phosphate supported type catalyst, a preparation method thereof, and application of the phosphate supported type catalyst in esterification, and a preparation method of ethyl acetate. The spherical mesoporous sepiolite composite carrier contains sepiolite and a mesoporous molecular sieve material, the average grain diameter of the spherical mesoporous sepiolite composite carrier is 10-50 microns, the specific surface area of the spherical mesoporous sepiolite composite carrier is 150-600 m<2> / g, the pore volume of the spherical mesoporous sepiolite composite carrier is 0.5-1.5 ml / g, the pore size distribution is three peak distribution, and most probable apertures corresponding to three peaks are respectively 2-5 nm, 5-15 nm and 10 nm-40 nm. The phosphate supported type catalyst not only has high photocatalytic activity, but also can be used repeatedly..

Description

technical field [0001] The invention relates to a spherical mesoporous sepiolite composite carrier, a method for preparing a spherical mesoporous sepiolite composite carrier, a spherical mesoporous sepiolite composite carrier prepared by the method, a loaded phosphoric acid catalyst, A preparation method of a supported phosphoric acid catalyst, an application of the supported phosphoric acid catalyst in esterification and a preparation method of ethyl acetate. Background technique [0002] In 1992, Mobile Company synthesized mesoporous materials. The mesoporous material has high specific surface area, regular pore structure and narrow pore size distribution, which makes its application in catalysis, separation, medicine and other fields have attracted great attention. In 1998, Zhao Dongyuan and others synthesized a new type of mesoporous material SBA-15 (D.Y.Zhao, J.L.Feng, Q.S.Huo, et al Science279(1998), 548-550), which has highly ordered cubic unit Mesoporous material p...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J32/00B01J35/08B01J27/182C07C67/08C07C69/14
Inventor 亢宇张明森王洪涛
Owner CHINA PETROLEUM & CHEM CORP
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