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

A montmorillonite-mediated and composite carrier technology is applied in the preparation of organic compounds, organic compound/hydride/coordination complex catalysts, catalyst carriers, etc., which can solve the problems of low conversion rate of reaction raw materials and reduce production costs. , The effect of high conversion rate of reaction raw materials and less side reactions

Active Publication Date: 2014-12-31
CHINA PETROLEUM & CHEM CORP +1
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  • 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 montmorillonite mesoporous composite carrier, a A preparation method of a spherical montmorillonite mesoporous composite carrier, a spherical montmorillonite 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 montmorillonite mesoporous composite carrier, supported catalyst, preparation methods of spherical montmorillonite mesoporous composite carrier and supported catalyst, use of supported catalyst and preparation method of ethyl acetate
  • Spherical montmorillonite mesoporous composite carrier, supported catalyst, preparation methods of spherical montmorillonite mesoporous composite carrier and supported catalyst, use of supported catalyst and preparation method of ethyl acetate
  • Spherical montmorillonite mesoporous composite carrier, supported catalyst, preparation methods of spherical montmorillonite 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 montmorillonite mesoporous composite carrier, the 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 material with a three-dimensional cubic pore structure, the silica gel filter cake and montmorillonite evenly and ball mill, and the solid powder obtained after the ball mill is slurryed with water and then spray-dried, and then The template agent in the product obtained after spray drying is removed.

[0039] In the preparation process of the above-mentione...

Embodiment 1

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

[0077] (1) Preparation of spherical montmorillonite mesoporous composite support

[0078] Dissolve 6 g (0.001 mol) of triblock copolymer polyethylene glycol-polyglycerol-polyethylene glycol (P123) in 10 mL of hydrochloric acid aqueous solution with a pH value of 4 and 220 mL of deionized aqueous solution, and stir at 15 °C for 4 h 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, add 12.9g (0.062mol) ethyl orthosilicate The ester was slowly added dropwise to the solution, the temperature was kept at 40°C and the pH value was 4.5, stirred for 24h, and then hydrothermally treated at 100°C for 24h, followed by filtration and repeated wa...

Embodiment 2

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

[0104] (1) Preparation of spherical montmorillonite mesoporous composite support

[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 45°C, and 10.4g (0.05mol) tetraethyl orthosilicate was slowly added dropwise to the solution, keeping the temperature at 45°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 filt...

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Abstract

The invention discloses a spherical montmorillonite 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 montmorillonite mesoporous composite carrier contains montmorillonite and a mesoporous molecular sieve material having a three-dimensional tunnel structure. The spherical montmorillonite 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 2-8nm and 20-50nm 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 montmorillonite mesoporous composite carrier, a preparation method of a spherical montmorillonite mesoporous composite carrier, a spherical montmorillonite 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] Montmorillonite is one of the most widely distributed clay minerals on the surface of the earth. It has nano-micron particle size, large specific surface area, exchangeability of interlayer ions and other physical and chemical properties. Some ions or molecules with special functional groups are inserted between layers or grafted on the surface to achieve surface modification and performance regulation. Acidification can increase the effective pores and bro...

Claims

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Application Information

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IPC IPC(8): B01J32/00B01J35/10B01J31/02C07C69/14C07C67/08
Inventor 亢宇张明森王洪涛
Owner CHINA PETROLEUM & CHEM CORP
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