Method for preparing solid acid catalyst by microwave solid phase method and application thereof

A solid acid catalyst, solid-phase method technology, applied in molecular sieve catalysts, chemical instruments and methods, catalyst activation/preparation and other directions, can solve the problems of increasing the isoamyl acetate treatment process, long reaction time, and many side reactions, etc. Easy to use repeatedly, simplify the post-processing process, and synthesize the effect of the simple method

Inactive Publication Date: 2010-05-12
GUANGDONG UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

At present, most of the synthetic catalysts used in industry are concentrated sulfuric acid as the catalyst, but this method has a series of problems such as long reaction time, many side reactions, serious equipment corrosion and three waste pollution.
[0004] Chloride is also one of the commonly used catalysts, but because it is not immobilized, it is very cumbersome to separate it from reactants and liquid products, and the post-treatment process for the synthesis of isoamyl acetate is added.

Method used

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  • Method for preparing solid acid catalyst by microwave solid phase method and application thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0014] Example 1: Weigh tin chloride and carrier OMS-2 according to the ratio of 0.001mmol: 1g carrier OMS-2, mix and grind them, then put them into a microwave oven and heat them for 4 minutes under 600w power to obtain OMS-2 loaded chloride Tin solid acid catalyst. The esterification reaction conditions are: the amount of catalyst used is 3.35% of the total mass of acetic acid and isoamyl alcohol, the molar ratio of acetic acid and isoamyl alcohol is 1:1.5, the reaction temperature is controlled at 110-120°C, and after the reaction, the solid-liquid separation and separation The solid catalyst can be used for the reaction again, and the separated liquid is washed with water, distilled and other further processes to obtain isoamyl acetate with an ester yield of 74%.

Embodiment 2

[0015] Embodiment 2: Take by weighing tin chloride and carrier OMS-2 according to the ratio of 0.009mmol: 1g carrier OMS-2, mix and grind, then put into microwave oven and heat under 600w power for 4 minutes to obtain the chlorine loaded on OMS-2 Tin oxide solid acid catalyst. The esterification reaction conditions are: the amount of catalyst used is 3.35% of the total mass of acetic acid and isoamyl alcohol, the molar ratio of acetic acid and isoamyl alcohol is 1:1.5, the reaction temperature is controlled at 110-120°C, and after the reaction, the solid-liquid separation and separation The solid catalyst can be used for the reaction again, and the separated liquid is washed with water, distilled and other further processes to obtain isoamyl acetate, and the ester yield is 76%.

Embodiment 3

[0016] Embodiment 3: Weigh tin chloride and carrier OMS-2 according to the ratio of 0.005mmol: 1g carrier OMS-2, mix and grind, then put into microwave oven and heat under 600w power for 4 minutes, namely obtain the chloride of OMS-2 load. Tin solid acid catalyst. The esterification reaction conditions are: the amount of catalyst used is 3.35% of the total mass of acetic acid and isoamyl alcohol, the molar ratio of acetic acid and isoamyl alcohol is 1:1.5, the reaction temperature is controlled at 110-120°C, and after the reaction, the solid-liquid separation and separation The solid catalyst can be used for the reaction again, and the separated liquid is washed with water, distilled and other further processes to obtain isoamyl acetate with an ester yield of 85%. The catalyst is reused three times, and its ester yield remains above 80%.

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Abstract

The invention discloses a method for preparing a solid acid catalyst by a microwave solid phase method and application thereof. A catalyst is synthesized into the solid acid catalyst by using a manganese oxide octahedral molecular sieve as a carrier, using tin tetrachloride or ferric chloride as an active component and adopting the microwave solid phase method. The method efficiently implements even solid load of the active component on the surface of the carrier; the method used in a reaction for synthesizing iso-amyl acetate can implement the separation of a solid catalyst, a liquid reactant and a product more easily, and simplify the post treatment process for synthesizing the iso-amyl acetate; and the yield of ester can reach 85 percent at most.

Description

technical field [0001] The invention relates to a method for preparing a solid acid catalyst by a microwave solid-phase method and its application. Background technique [0002] Isoamyl acetate is a colorless and transparent liquid and an important spice in the food industry. It has a strong fresh fruity aroma, slightly sweet, and has an odor similar to ripe bananas, raw pears, and apples. It is often used in the preparation of edible fruit flavors, candy products, and non-alcoholic beverages. It is also used in appropriate amounts in flavors for cigarettes and daily cosmetics. Isoamyl acetate is also a very useful organic solvent in leather, rubber, and paint industries. It can be used as a solvent for neoprene, nitrocellulose, celluloid, camphor, ink, paint, spray paint, varnish, etc. It is a widely used organic chemical product. [0003] The method for preparing isoamyl acetate is a lot, and the method for traditionally preparing isoamyl acetate has sulfuric acid cataly...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J37/34B01J29/00C07C69/14C07C67/08
Inventor 孙明余林余倩郝志峰刁贵强李永峰郑育英
Owner GUANGDONG UNIV OF TECH
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