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A kind of modified cation exchange resin catalyst and its preparation method and application

A technology of cation exchange and resin exchange, which is applied in the direction of chemical instruments and methods, preparation of organic compounds, physical/chemical process catalysts, etc., can solve the problems of low conversion rate, catalyst corrosion, easy deactivation, etc., and achieve good dispersion, No equipment corrosion and long service life

Active Publication Date: 2015-09-02
CHINA PETROLEUM & CHEM CORP +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] Aiming at the deficiencies of the prior art, the present invention provides a solid superacid-modified cation exchange resin catalyst and its preparation method and application, which solves the deficiencies of the prior art catalysts such as corrosion of equipment, low conversion rate and easy deactivation

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0019] 1. Preparation of solid super acid-modified ion exchange resin catalyst: a: Wash 50 grams of hydrogen-type styrene-based strong acid cation exchange resin with deionized water for 5 times, 20 minutes each time, and dry it in a vacuum drying box at 100°C 24 hours; b: mix the dried hydrogen-type strong acid cation exchange resin with 200 g of 3.9% Zn (NO 3 ) 2 The aqueous solution was immersed for 8 hours, titrated to neutrality with ammonia water, washed and dried in a vacuum drying oven at 90 ° C for 20 hours; c: The dried hydrogen cation exchange resin was treated with 15% (NH 4 ) 2 SO 4 300 g of the aqueous solution was impregnated in excess for 8 hours; d: after filtration, put it in a vacuum drying oven at 100°C to dry for 20 hours, and then calcined at 210°C for 8 hours to obtain a solid superacid-modified ion-exchange resin catalyst.

[0020] 2. This catalyst was used in the reaction of acetic acid and 1-butene to synthesize sec-butyl acetate. The reaction was ...

Embodiment 3

[0022] 1. Preparation of solid super acid-modified ion exchange resin catalyst: a: Wash 70 grams of hydrogen-type styrene-based strong acid cation exchange resin with deionized water for 5 times, 20 minutes each time, and dry in a vacuum drying box at 100°C 24 hours; b: mix the dried hydrogen-type strong acid cation exchange resin with 200 g of 2.9% Zn (NO 3 ) 2 The aqueous solution was immersed for 8 hours, titrated to neutrality with ammonia water, washed and dried in a vacuum drying oven at 90 ° C for 20 hours; c: The dried hydrogen cation exchange resin was treated with 15% (NH 4 ) 2 SO 4 300 g of the aqueous solution was soaked in excess for 8 hours; d: after filtration, put it in a vacuum drying oven for 16 hours at 100°C, and then calcined at 220°C for 9 hours to obtain a solid superacid-modified ion-exchange resin catalyst.

[0023] 2. This catalyst was used in the reaction of acetic acid and 1-butene to synthesize sec-butyl acetate. The reaction was carried out on ...

Embodiment 4

[0025] 1. Preparation of solid super acid-modified ion exchange resin catalyst: a: Wash 90 grams of hydrogen-type styrene-based strong acid cation exchange resin with deionized water for 5 times, 20 minutes each time, and dry in a vacuum drying box at 100°C 24 hours; b: mix the dried hydrogen-type strong acid cation exchange resin with 300 g of 7.1% Zn (NO 3 ) 2 The aqueous solution was immersed for 8 hours, titrated to neutrality with ammonia water, washed and dried in a vacuum drying oven at 90 ° C for 20 hours; c: The dried hydrogen cation exchange resin was treated with 15% (NH 4 ) 2 SO 4 300 g of the aqueous solution was impregnated in excess for 8 hours; d: after filtration, put it in a vacuum drying oven at 100°C to dry for 18 hours, and then calcined at 230°C for 10 hours to obtain a solid superacid-modified ion exchange resin catalyst.

[0026]2. This catalyst is used in the reaction of acetic acid and 1-butene to synthesize sec-butyl acetate. The reaction is carri...

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PUM

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Abstract

The invention discloses a modified cation exchange resin catalyst, solid super acid SO4<2-> / ZnO is used as a modifier, taking the weight of cation exchange resin as a carrier as the base, the modifier solid super acid SO4<2-> / ZnO accounts for 1%-10%, by Zn, of the mass of the catalyst, the exchange capacity of the matrix cation exchange resin is 4.4-5.3mol / kg, the mass content of the water is 45%-50%, the wet apparent density is 0.80-0.95g / ml, and the wet true density is 1.1-1.3g / ml. The catalyst is used in the reaction process for sec-butyl acetate synthesis, and is high in esterification efficiency, good in selective stability and free of equipment corrosion and environmental pollution problems.

Description

technical field [0001] The invention relates to a cation exchange resin catalyst modified by a solid super acid, a preparation method of the catalyst and an application in the synthesis reaction of sec-butyl acetate. Background technique [0002] Sec-butyl acetate is one of the four isomers of butyl acetate. It is a colorless, flammable, fruit-flavored liquid, insoluble in water, and miscible with ethanol and ether. Sec-butyl acetate is widely used in nitrocellulose, coatings, artificial leather, medicine, paints, fragrances, inks, and plastics industries. At the same time, it can also be used as extracting agent, dehydrating agent and metal cleaning agent. CN1844076A uses sulfuric acid as a catalyst to produce butyl acetate by reactive distillation. Using sulfuric acid as a catalyst will inevitably cause corrosion to the equipment, and discharge a large amount of acid-containing wastewater, causing serious environmental pollution problems. CN184187C discloses super acid S...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): B01J31/26C07C69/14C07C67/04
Inventor 刘野霍稳周吕清林李花伊魏晓霞田丹
Owner CHINA PETROLEUM & CHEM CORP