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Method for synthesizing isolongifolene by catalytically isomerizing longifolene with solid acid

A solid acid catalyzed, isolongifolene technology, applied in the direction of isomerization hydrocarbon production, organic chemistry, chemical recovery, etc., can solve the problems of pollution, high production costs, etc., to reduce corrosion, save labor and provide competitiveness Effect

Inactive Publication Date: 2013-12-11
WUZHOU SONGHUA AROMATIC CHEM
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] The invention provides a solid acid-catalyzed method for synthesizing isolongifolene from isolongifolene to solve the problems of high production cost and serious pollution of isolongifolene or isolongifolene

Method used

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  • Method for synthesizing isolongifolene by catalytically isomerizing longifolene with solid acid

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Effect test

Embodiment 1

[0009] The method for the synthesis of isolongifolene by solid acid catalyzed isomerization of longifolene, the small test feed is 100 grams of longifolene / pot: 20 grams of macroporous strong acid cation exchange resin D72 catalyst is added to a 500ml three-necked flask, and then 100 grams of 65% longifolene and 80 grams of glacial acetic acid are mixed and added to the reaction flask, stirring is started to heat, and the isomerization reaction is carried out in the reaction kettle. For the content of leafene, take samples every 0.5-1 hour until the content of isolongifolene no longer increases or increases very slowly or even falls back, then stop adding and start cooling down to below 40 degrees. The reaction lasts for about 4 hours, and then sequentially Filtration was carried out, the catalyst was recovered, and finally the filtrate was subjected to atmospheric distillation to recover the solvent, and the analysis results of the crude isolongifolene obtained were: the conte...

Embodiment 2

[0012] The method for the synthesis of isolongifolene by solid acid catalyzed isomerization of longifolene, enlarged test 10000 grams of longifolene / pot: 3000 grams of macroporous strong acid cation exchange resin D72 catalyst is added in a 30L reactor, and then 10000 Gram 65% longifolene and 12000 grams of glacial acetic acid are added respectively to the reaction kettle, start stirring, heating, carry out isomerization reaction in the reaction kettle, the temperature in the reaction kettle is 90 ℃, after 3 hours, sampling analysis isolongifolene content , sampling once every 0.5-1 hour, until the content of isolongifolene no longer increases or increases very slowly or even falls back, stop adding and start to cool down, cool down to below 40 degrees, react for a total of about 5 hours, and then filter in turn, The catalyst was recovered, and finally the filtrate was subjected to atmospheric distillation to recover the solvent, and the analysis results of the crude isolongifo...

Embodiment 3

[0015] The method for synthesizing isolongifolene by solid acid catalyzed isomerization longifolene, pilot test 100kg longifolene / pot, 10kg of macroporous strong acid cation exchange resin D72 catalyst is added in the pilot test reactor, and then 100kg65% longifolene Folene and 60kg of glacial acetic acid are added to the reactor respectively, start stirring and heating, and carry out isomerization reaction in the reactor. Sampling once every 1 hour, until the isolongifolene content no longer increases or increases very slowly or even drops back down, stop adding and start to cool down, cool down to below 40 degrees, and react for about 6 hours in total, then filter in turn, recover the catalyst, and finally put The filtrate was subjected to atmospheric distillation to recover the solvent, and the analysis results of the crude isolongifolene obtained were: the content of isolongifolene was 59.838%, and the content of longifolene was 2.9%. The crude isolongifolene is distilled ...

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Abstract

The invention discloses a method for synthesizing isolongifolene by catalytically isomerizing longifolene with solid acid. The method comprises the following steps: mixing longifolene and glacial acetic acid; putting the mixture into a reaction container; adding a catalyst to perform an isomerization reaction; filtering after the reaction is finished; recycling the catalyst; distilling to recycle a solvent; rectifying to obtain an isolongifolene finished product. The method is characterized in that the catalyst is solid acid D72 macroporous strong acid ion exchange resin; the weight ratio of the longifolene to the glacial acetic acid to the catalyst is 1:(0.4-1.2):(0.1-0.3); the temperature in the reaction container is 60-110 DEG C, and the reaction time is 4-6 hours. The method can solve the existing problems of high cost and severe pollution for producing isolongifolene or isolongifolenone.

Description

technical field [0001] The invention relates to the technical field of chemical pine resin deep processing, in particular to a method for synthesizing isolongifolene using longifolene isomerization. Background technique [0002] At present, sulfuric acid is commonly used as a catalyst in the reaction process of synthesizing isolongifolene from longifolene through isomerization. Due to the strong corrosiveness of sulfuric acid, the inner wall of the reaction kettle and the inner wall of the pipeline and other equipment are subject to strong corrosion, which reduces the service life of the equipment; and sulfuric acid is a dangerous chemical that has certain harm to the human body. Danger, after the isomerization reaction, it is necessary to add a washing process to remove the sulfuric acid left over from the reaction, which consumes more solvent and water resources, increases manpower and material resources, and increases production costs; in addition, sulfuric acid is used i...

Claims

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Application Information

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IPC IPC(8): C07C5/29C07C13/72
CPCY02P20/584
Inventor 陈键泉陈伟强杨振洲梁利诚苏炳连黄宇平李杰鹏冯玲廖军
Owner WUZHOU SONGHUA AROMATIC CHEM
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