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Supported solid acid catalyst and its application in the preparation of ester fragrances

A solid acid catalyst and supported technology, which is applied in the preparation of carboxylic acid esters, chemical instruments and methods, and the preparation of organic compounds. It can solve the problems of complex purification, side reactions, and corrosive equipment, and achieve good catalytic effects. High activity and good product quality

Active Publication Date: 2015-08-26
APPLE FLAVOR & FRAGRANCE GRP
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

For example: there are side reactions, which make the purification more complicated; the discharge of acid-containing wastewater causes environmental pollution; the acid consumption is large, and the equipment is easy to corrode

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0018] A. The preparation method of supported solid acid catalyst supported type:

[0019] This example is γ-Al 2 o 3 - Preparation of 0.5% P carrier:

[0020] Take 16.13 mL of 1 mol / L phosphoric acid solution and dilute it to 200 mL with deionized water. Weigh the γ-Al calcined at 500°C for 2 hours 2 o 3 100g. γ-Al to be weighed 2 o 3 Mix and impregnate with diluted 200mL phosphoric acid solution for 4 hours, the volume of diluted phosphoric acid solution is equal to that of γ-Al 2 o 3 The mass ratio is 2.0mL / g, and the impregnation process adopts ultrasonic to enhance the impregnation effect. Then stir in a sand bath at 110°C until dry. The γ-Al 2 o 3 -0.5% P carrier.

[0021] B. 20%SiW 12 / γ-Al 2 o 3 - Preparation of 0.5% P catalyst

[0022] Weigh 4.6g of silicotungstic acid H with keggin structure 4 SiW 12 o 40 24 hours 2 O was dissolved to 32 mL with deionized water to obtain a silicotungstic acid solution. Weigh 16g of the γ-Al obtained in the above...

Embodiment 2

[0027] 30%SiW 12 / γ-Al 2 o 3 - Preparation of 0.5% P catalyst

[0028] Weigh 6.9g of silicotungstic acid H with keggin structure 4 SiW 12 o 40 24 hours 2 O, dissolved to 28mL with deionized water to obtain silicotungstic acid solution. Weigh 14g γ-Al 2 o 3 -0.5% P mixed with the above 28mL silicotungstic acid solution for impregnation. The liquid-solid ratio of the volume of the impregnating solvent and the mass of the carrier is 2.0mL / g. The rest of the processing conditions are the same as the steps of Example 1 B, and 30% SiW can be obtained 12 / γ-Al 2 o 3 -0.5% P catalyst.

Embodiment 3

[0030] 40%SiW 12 / γ-Al 2 o 3 - Preparation of 0.5% P catalyst

[0031] Weigh 9.2g of silicotungstic acid H with keggin structure 4 SiW 12 o 40 24 hours 2 O was dissolved to 24 mL with deionized water to obtain a silicotungstic acid solution. Weigh 12g γ-Al 2 o 3 -0.5% P mixed with the above 24mL silicotungstic acid solution for impregnation. The liquid-solid ratio of the volume of the impregnating solvent and the mass of the carrier is 2.0mL / g. The rest of the treatment conditions are the same as the steps in Example 1 B, and 40% SiW can be obtained 12 / γ-Al 2 o 3 -0.5% P catalyst.

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PUM

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Abstract

The invention relates to a supported solid acid catalyst, and a method for preparing ester perfumes through applying it. The novel supported heteropoly acid catalyst is obtained through loading heteropoly acid on an SAPO-34 molecular sieve molecular sieve support, or a P and B modified gamma-Al2O3 support, or a mixed support of the above two supports, the catalyst has a good catalytic effect on an esterification reaction, and allows various ester perfumes to be efficiently synthesized. The method adopting the supported solid acid as a catalyst has the advantages of avoiding of problems comprising complex post-treatment technology, equipment corrosion, and influences of byproducts to the fragrances of the ester perfumes and caused by the adoption of sulfuric acid as a catalyst, high esterification reaction activity, good product quality, and recovery and recycle of the catalyst in the invention.

Description

technical field [0001] The invention relates to a method for preparing ester fragrances, in particular to a method for preparing ester fragrances by using a loaded solid acid catalyst. Background technique [0002] Organic ester compounds are widely used in organic synthesis industries such as flavors and fragrances, cosmetics, medicine, solvents, and coatings. Therefore, the esterification reaction has become an important way to synthesize raw materials and intermediates. [0003] The esterification reaction is a typical acid-catalyzed reaction, and the catalyst is the key factor affecting the reaction rate and yield. In the traditional process of esterification reaction, concentrated sulfuric acid is usually used as a catalyst. But it has many deficiencies. For example: there are side reactions, which make the purification more complicated; the discharge of acid-containing wastewater causes environmental pollution; the acid consumption is large, and the equipment is eas...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): B01J31/26C07C67/08C07C69/24C07C69/618C07C69/06C07C69/614C07C69/157
CPCY02P20/584
Inventor 王冠石铭亮冯黎
Owner APPLE FLAVOR & FRAGRANCE GRP
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