Method for synthesizing tricyclodecenyl propionate perfume by adopting loaded solid acid catalyst

A technology of tricyclodecenyl propionate and solid acid catalyst is applied in the field of preparation of organic synthetic fragrances, and can solve the problems of low content, insufficient isomer ratio to satisfy fragrance quality, product fragrance with sour taste and the like

Active Publication Date: 2014-10-15
ANHUI HYEA AROMAS
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  • Abstract
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AI Technical Summary

Problems solved by technology

[0009] The binary compound acid of perchloric acid-phosphoric acid is used as a catalyst for the acetylation reaction. Compared with perchloric acid as a catalyst, the reaction conditions are optimized, the production cost is reduced, and the yield of the synthesis reaction is relatively improved. However, high-strength acid is harmful to equipment. The corrosion problem of TCDA is relatively serious, and the isomer ratio of the prepared TCDA cannot meet the requirements of aroma quality, and the product has a floral-fruity sweet tricyclic [5,2,1,0 2.6 The content of ]-3-decen-9-ol propionate is low, resulting in a sour aroma and affecting product quality
[0010] Boron trifluoride or b

Method used

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  • Method for synthesizing tricyclodecenyl propionate perfume by adopting loaded solid acid catalyst

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0037] a) Pump the material in the dicyclopentadiene insulation tank 1 into the dicyclopentadiene high-level tank 2, and add dicyclopentadiene from the dicyclopentadiene high-level tank 2 to the 500 L esterification reactor 5 Pentadiene 260 kg, add propionic anhydride 2.5 kg from propionic anhydride header tank 3 to esterification reactor 5, after the feed finishes, add propionic acid 140 kg from propionic acid header tank 4, from esterification reactor 5 hand holes 52 Add 2 kg of catalyst zeolite loaded phosphotungstic acid, start the mixer 53 and mix evenly;

[0038] b) Open the steam valve, heat up the esterification reaction kettle 5, and control the reaction temperature to 95~98°C;

[0039] c) After 4 hours of reaction, take samples for gas chromatography detection, and then take samples for detection at intervals of 2 hours. When the dicyclopentadiene content is less than 2%, maintain the temperature and continue the reaction for 2 hours, then cool down to terminate the ...

Embodiment 2

[0049] a) Add 1300 kg of dicyclopentadiene and 13 kg of propionic anhydride to the 2500 L esterification reactor 5. After the feeding is completed, add 700 kg of propionic acid from the propionic acid head tank 4, and add 700 kg of propionic acid from the esterification reactor 5 Add catalyst zeolite-loaded phosphotungstic acid 8 kg into hole 52, start the mixer and mix evenly;

[0050] b) Open the steam valve, heat up the esterification reaction kettle 5, and control the reaction temperature to 95-100°C;

[0051] c) After 4 hours of reaction time, take samples for gas chromatography detection, and then take samples for detection at intervals of 2 hours. When the dicyclopentadiene content is less than 2%, maintain the temperature and continue the reaction for 2 hours, then cool down to terminate the reaction, and add 30 kg of clear water, continue to stir, and propionic anhydride is hydrolyzed into propionic acid;

[0052] d) The reaction solution in step c) is sent to the pr...

Embodiment 3

[0059] a) Add 260 kg of dicyclopentadiene and 3 kg of propionic anhydride to the esterification reactor 5. After the feed is completed, add 130 kg of propionic acid from the propionic acid head tank 4, and add it from the hand hole 52 of the esterification reactor 5 Catalyst zeolite loaded phosphotungstic acid 1.5 kg, turn on the mixer 53 and mix evenly;

[0060] b) Open the steam valve, heat up the esterification reaction kettle 5, and control the reaction temperature to 98~100°C;

[0061] c) After 4 hours of reaction time, take samples for gas chromatography detection, and then take samples for detection at intervals of 2 hours. When the dicyclopentadiene content is less than 2%, maintain the temperature and continue the reaction for 2 hours, then cool down to terminate the reaction, and add 6 kg of clear water, continue to stir, and propionic anhydride is hydrolyzed into propionic acid;

[0062] d) The reaction solution in step c) is sent to the precision filter 7 with nit...

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Abstract

The invention discloses a synthesis method of a tricyclodecenyl propionate perfume. Petroleum coking byproducts dicyclopentadiene and propionic acid are used as the raw materials, under the catalysis of loaded solid acid, the raw materials directly have acetylation through electrophilic addition to prepare crude tricyclodecenyl propionate at one step, and meanwhile, a small amount of a propionic anhydride guard catalyst is added to prevent the crude tricyclodecenyl propionate from having hydrolysis reaction with a small amount of moisture in the material; then, propionic acid is recycled for applied mechanically, and the finished tricyclodecenyl propionate product is obtained through neutralizing, washing and rectification. According to the synthesis method, the petroleum coking byproducts used as the raw materials are easily available, the reaction condition is moderate, the reaction conversion rate is high, the technology is easier to implement, the discharge capacity of three wastes generated in the production process is low, the product yield is greatly increased, and the synthesis method belongs to technology of cleaner production. In addition, the content of tricyclo[5, 2, 1, 0<2.6>]-3-decene-9-yl acetate with delicate fragrance and fragrance and sweetness of anise is more than 92%, and the product green wood is pure, fine and mild in fragrance. The invention further provides a synthesis device special for the synthesis method of a tricyclodecenyl propionate perfume.

Description

technical field [0001] The invention relates to the technical field of fine chemical synthesis, in particular to a method for preparing organically synthesized spices. Background technique [0002] Tricyclodecenyl propionate is widely used in various flavor formulas in daily chemical flavors. It is commonly found in surface cleaners, shampoos, deodorants, detergents, soaps and other flavors. It has a sweet fruity aroma Floral fragrance, accompanied by the aroma of jasmine and anise, is an important synthetic fragrance in the cycloalkene family. The aroma is softer than tricyclodecenyl acetate. It is suitable for use with other cycloalkene family fragrances. The dosage can be adjusted Reaching within 10%, IFRA has not made restrictions on the use. [0003] Tricyclodecenyl Propionate has a woody and herbaceous aroma with floral and fruity aromas and woody notes. Appearance is colorless to light yellow transparent liquid, tricyclodecenyl propionate is a mixture of four isomer...

Claims

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Application Information

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IPC IPC(8): C07C69/24C07C67/04
CPCC07C67/04C07C69/24
Inventor 王天义汪洋汪民富徐基龙董金龙
Owner ANHUI HYEA AROMAS
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