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Spherical attapulgite mesoporous composite carrier, supported catalyst, preparation methods of spherical attapulgite mesoporous composite carrier and supported catalyst, use of supported catalyst and preparation method of ethyl acetate

A technology of composite carrier and attapulgite, which is applied in the preparation of organic compounds, organic compound/hydride/coordination complex catalysts, catalyst carriers, etc., can solve the problem of low conversion rate of reaction raw materials, and reduce production costs. Does not corrode equipment and has less side effects

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

[0005] The purpose of the present invention is to overcome the defect that the supported catalyst made of existing mesoporous molecular sieve material is used for the low conversion rate of reaction raw materials in the process of esterification, and to provide a spherical attapulgite mesoporous composite carrier, a A preparation method of a spherical attapulgite mesoporous composite carrier, a spherical attapulgite mesoporous composite carrier prepared by the method, a loaded benzenesulfonic acid catalyst, a preparation method of a loaded benzenesulfonic acid catalyst, the Application of supported benzenesulfonic acid catalyst in esterification and a preparation method of ethyl acetate

Method used

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  • Spherical attapulgite mesoporous composite carrier, supported catalyst, preparation methods of spherical attapulgite mesoporous composite carrier and supported catalyst, use of supported catalyst and preparation method of ethyl acetate
  • Spherical attapulgite mesoporous composite carrier, supported catalyst, preparation methods of spherical attapulgite mesoporous composite carrier and supported catalyst, use of supported catalyst and preparation method of ethyl acetate
  • Spherical attapulgite mesoporous composite carrier, supported catalyst, preparation methods of spherical attapulgite mesoporous composite carrier and supported catalyst, use of supported catalyst and preparation method of ethyl acetate

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preparation example Construction

[0035] The present invention also provides a method for preparing a spherical attapulgite mesoporous composite carrier, the preparation method comprising the following steps:

[0036] (1) In the presence of a template and butanol, contact ethyl orthosilicate with an acid agent, and crystallize and filter the contacted product to obtain a filter material of a mesoporous molecular sieve material with a three-dimensional cubic pore structure. cake;

[0037] (2) Contact water glass with inorganic acid, and filter the product obtained after contact to obtain a silica gel filter cake;

[0038] (3) Mix the filter cake of the mesoporous molecular sieve material having a three-dimensional cubic pore structure, the silica gel filter cake and attapulgite evenly and ball mill, and the solid powder obtained after ball milling is slurried with water and then spray-dried, The template agent in the product obtained after spray drying is removed.

[0039] In the preparation process of the sp...

Embodiment 1

[0076] This example is used to illustrate the spherical attapulgite mesoporous composite carrier and supported benzenesulfonic acid catalyst provided by the present invention and the preparation method thereof.

[0077] (1) Preparation of spherical attapulgite mesoporous composite carrier

[0078] Dissolve 6g (0.001mol) triblock copolymer polyethylene glycol-polyglycerol-polyethylene glycol (P123) in 10mL aqueous hydrochloric acid solution with a pH value of 4 and 220mL deionized aqueous solution, stir for 4h until P123 dissolves , to form a transparent solution, then add 6g (0.08mol) n-butanol to the transparent solution and stir for 1h, then place the solution in a water bath at 40°C, slowly drop 12.9g (0.062mol) ethyl orthosilicate Add it into the solution, keep the temperature at 40°C and the pH value of 4.5 and stir for 24h, then hydrothermally treat at 100°C for 24h, then filter and wash 4 times with deionized water, and then suction filter to get Mesoporous molecular s...

Embodiment 2

[0103] This example is used to illustrate the spherical attapulgite mesoporous composite carrier and supported benzenesulfonic acid catalyst provided by the present invention and the preparation method thereof.

[0104] (1) Preparation of spherical attapulgite mesoporous composite carrier

[0105] Dissolve 6g (0.001mol) of triblock copolymer P123 in 10mL of hydrochloric acid aqueous solution with a pH value of 5 and 220mL of deionized aqueous solution, stir for 4 hours until P123 dissolves to form a transparent solution, and then add 4.5g of (0.06mol) n-butanol was stirred for 1 hour, then the solution was placed in a water bath at 60°C, and 10.4g (0.05mol) tetraethyl orthosilicate was slowly added dropwise to the solution, keeping the temperature at 60°C and pH Stir for 48 hours at a value of 5.5, then hydrothermally treat at 80°C for 20 hours, then filter and wash with deionized water four times, and then suction filter to obtain a mesoporous molecular sieve filter cake with...

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Abstract

The invention discloses a spherical attapulgite mesoporous composite carrier and its preparation method, a supported benzenesulfonic acid catalyst and its preparation method, a use of the supported benzenesulfonic acid catalyst in an esterification reaction, and a preparation method of ethyl acetate. The spherical attapulgite mesoporous composite carrier contains attapulgite and a mesoporous molecular sieve material having a three-dimensional tunnel structure. The spherical attapulgite mesoporous composite carrier has the average particle size of 20-50 microns, a specific surface area of 150-600 m<2> / g and a pore volume of 0.5-1.5ml / g, and has a bimodal pore diameter distribution mode and most probable pore diameters of 2-10nm and 20-40nm corresponding to two peaks. The supported benzenesulfonic acid catalyst has high catalytic activity and can be recycled.

Description

technical field [0001] The invention relates to a spherical attapulgite mesoporous composite carrier, a preparation method of a spherical attapulgite mesoporous composite carrier, a spherical attapulgite mesoporous composite carrier prepared by the method, and a loaded benzenesulfonic acid Catalyst, a preparation method of a loaded benzenesulfonic acid catalyst, an application of the loaded benzenesulfonic acid catalyst in esterification and a preparation method of ethyl acetate. Background technique [0002] Attapulgite clay (abbreviated as attapulgite) is a hydrous magnesium-rich aluminum silicate crystal mineral. Its basic structural unit is a unit layer composed of two layers of silicon-oxygen tetrahedron sandwiching a layer of magnesium-oxygen octahedron. In each 2: In layer 1, the corners of the tetrahedral sheets are reversed at a certain distance to form a layer chain structure, and channels parallel to the c-axis direction are formed between the tetrahedral strips, ...

Claims

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Application Information

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IPC IPC(8): B01J32/00B01J35/08B01J31/26C07C69/14C07C67/08
Inventor 亢宇张明森王洪涛
Owner CHINA PETROLEUM & CHEM CORP
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