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Spherical montmorillonite mesoporous composite carrier, supported catalyst and preparation method and application thereof, and ethyl acetate preparation method

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. , does not corrode the instrument, the effect of expanding the application field

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 the existing mesoporous molecular sieve material is used for the lower conversion rate of the reaction raw material 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 and preparation method and application thereof, and ethyl acetate preparation method
  • Spherical montmorillonite mesoporous composite carrier, supported catalyst and preparation method and application thereof, and ethyl acetate preparation method
  • Spherical montmorillonite mesoporous composite carrier, supported catalyst and preparation method and application thereof, and ethyl acetate preparation method

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preparation example Construction

[0033] The invention also provides a method for preparing the spherical smectite mesoporous composite carrier, which includes the following steps:

[0034] (1) In the presence of templating agent, trimethylpentane and ethanol, tetramethoxysilane is contacted with acid agent, and the product obtained after contact is crystallized and filtered to obtain No. 1 mesoporous material filter cake ; Cetyltrimethylammonium bromide, ethyl orthosilicate and ammonia water are contacted, and the contacted product is filtered to obtain No. 2 mesoporous material filter cake;

[0035] (2) Contact water glass with inorganic acid, and filter the product obtained after contact to obtain silica gel filter cake;

[0036] (3) Mixing the No. 1 mesoporous material filter cake, No. 2 mesoporous material filter cake, silica gel filter cake and montmorillonite uniformly and ball milling, and slurrying the solid powder obtained after ball milling with water and then spray drying, The templating agent in the obt...

Embodiment 1

[0074] This example is used to illustrate the spherical smectite mesoporous composite carrier and the supported benzene sulfonic acid catalyst provided by the present invention and the preparation method thereof.

[0075] (1) Preparation of spherical smectite mesoporous composite carrier

[0076] 1.0g (0.0001mol) triblock copolymer polyethylene glycol-polyglycerol-polyethylene glycol (P123) and 1.69g (0.037mol) ethanol were added to 28mL, pH 4 acetic acid and sodium acetate In the buffer solution, stir at 15°C until P123 is completely dissolved, then add 3.43g (0.03mol) of trimethylpentane to the above solution, and stir at 15°C for 8 hours, then add 2.28g (0.015 mol) Tetramethoxysilane, then stirred for 20 hours at 15°C and pH 4.5, and the resulting solution was transferred to a polytetrafluoroethylene-lined reactor, and crystallized in an oven at 60°C for 24 hours After hours, the obtained crystalline product was suction filtered and washed with distilled water four times to obt...

Embodiment 2

[0100] This example is used to illustrate the spherical smectite mesoporous composite carrier and the supported benzene sulfonic acid catalyst provided by the present invention and the preparation method thereof.

[0101] (1) Preparation of spherical smectite mesoporous composite carrier

[0102] Add 1.0 g of triblock copolymer P123 and 0.92 g of ethanol (0.02 mol) to 28 mL of a buffer solution of acetic acid and sodium acetate with a pH of 5, stir at 20°C until P123 is completely dissolved, and then 2.86 g (0.025mol) trimethylpentane was added to the above solution, and after stirring for 1 hour at 20°C, 1.07g (0.007mol) of tetramethoxysilane was added, and then the pH was 5.5 at 20°C Stir for 30 hours under the conditions of, and transfer the resulting solution to a polytetrafluoroethylene lined reactor, crystallize in an oven at 40°C for 40 hours, and filter the resulting crystallized product and wash it with distilled water four times. Obtain No. 1 mesoporous material filter c...

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Abstract

The invention discloses a spherical montmorillonite mesoporous composite carrier and a preparation method thereof, a supported benzenesulfonic acid catalyst and a preparation method thereof, an application of the 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, average particle size of the spherical montmorillonite mesoporous composite carrier is 30-60 micrometers, the specific surface area is 150-600 square meters / gram, pore volume is 0.5-1.5 milliliters / gram, aperture distribution is trimodal distribution, most probable apertures corresponding to three peaks are 2-4 nanometers, 5-15 nanometers and 10-40 nanometers respectively. The provided supported benzenesulfonic acid catalyst has the advantages of high catalytic activity and repeated usage.

Description

Technical field [0001] The invention relates to a spherical montmorillonite mesoporous composite carrier, a method for preparing a spherical montmorillonite mesoporous composite carrier, a spherical montmorillonite mesoporous composite carrier prepared by the method, and a supported benzenesulfonate An acid catalyst, a preparation method of a supported benzenesulfonic acid catalyst, application of the supported benzenesulfonic acid catalyst in an esterification reaction, and a preparation method of ethyl acetate. Background technique [0002] Montmorillonite is one of the most widely distributed clay minerals on the surface. It has nano-micron particle size, large specific surface area, interlayer ion exchangeability and other physical and chemical properties. Therefore, it can be used in Insert or graft some ions or molecules with special functional groups on the surface to realize the modification and performance control of the surface. Acidification can increase the effective...

Claims

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Application Information

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