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Post-treatment method of isopulegol reaction liquid

A technology of isopulegol and reaction solution, which is applied in chemical instruments and methods, preparation of organic compounds, separation/purification of hydroxyl compounds, etc., can solve the problem of unstable operation of separation system, complicated quenching process and low quenching efficiency And other issues

Active Publication Date: 2022-04-15
WANHUA CHEM GRP CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0008] The purpose of the present invention is to provide a post-treatment method of isopulegol reaction solution, which can solve the problems of low quenching efficiency, complex quenching process and unstable operation of the separation system in the quenching process

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0030] Take 0.6g of L-valinol into 1000g of unquenched isopulegol reaction solution 1, stir evenly to obtain a reaction solution mixture, control the reaction temperature of the reaction solution mixture to 50°C, and the reaction time for 0.5h to obtain the quenched Isopulegol reaction solution. The quenching effect evaluation experiment was further carried out, and the quenched reaction solution was heated to 100° C., kept for 24 hours, and the loss rate of isopulegol was 0.51% by gas phase detection. The quenched reaction liquid is subjected to distillation and separation. During the distillation process, the absolute pressure of the operation is 5mbar, the temperature of the tower bottom is controlled to be 150°C, and the temperature of the tower top is 80°C to obtain the top product rich in isopulegol and remove isopulegol. The bottom product of pulegitol, the content of isopulegol in the top product obtained through gas chromatography analysis is 99.8wt%, and the yield of...

Embodiment 2

[0032] Take 0.2g of D-phenylglycinol into 1000g of unquenched isopulegol reaction solution 1, stir evenly to obtain a reaction solution mixture, control the reaction temperature of the reaction solution mixture to 100°C, and the reaction time for 1.5h, that is, after quenching isopulegol reaction solution. The quenching effect evaluation experiment was further carried out, and the quenched reaction solution was heated to 100° C., kept for 24 hours, and the loss rate of isopulegol was 0.38% by gas phase detection. The quenched reaction liquid is subjected to distillation and separation. During the distillation process, the absolute pressure of the operation is 5mbar, the temperature of the tower bottom is controlled to be 150°C, and the temperature of the tower top is 80°C to obtain the top product rich in isopulegol and remove isopulegol. The bottom product of pulegitol is analyzed by gas chromatography to obtain that the content of isopulegol in the top product is 99.7wt%, an...

Embodiment 3

[0034] Take 1g of L-phenylalaninol into 1000g of unquenched isopulegol reaction solution 1, stir evenly to obtain a reaction solution mixture, control the reaction temperature of the reaction solution mixture to 80°C, and react for 2 hours to obtain the quenched isopulegol. Pulverized alcohol reaction solution. The quenching effect evaluation experiment was further carried out, and the quenched reaction solution was heated to 100° C., kept for 24 hours, and the loss rate of isopulegol was 0.44% by gas phase detection. The quenched reaction liquid is subjected to distillation and separation. During the distillation process, the absolute pressure of the operation is 5mbar, the temperature of the tower bottom is controlled to be 150°C, and the temperature of the tower top is 80°C to obtain the top product rich in isopulegol and remove isopulegol. The bottom product of pulegitol is analyzed by gas chromatography to obtain that the content of isopulegol in the top product is 99.7wt...

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Abstract

The invention relates to a post-treatment method of an isopulegol reaction solution. The method comprises the following specific steps: quenching the residual active catalyst in the isopulegol reaction liquid by using an amino alcohol compound as a quenching agent, and finally separating and recycling. The quenching mode is adopted for post-treatment, the product stability is good, the impurity increase phenomenon is avoided, the production cost is reduced, stable and continuous operation can be achieved, and the industrial value is achieved.

Description

technical field [0001] The invention belongs to the field of post-treatment of chemical industry, and in particular relates to a post-treatment method of isopulegol reaction liquid. [0002] technical background [0003] Isopulegol is an important intermediate for obtaining different aroma compounds, such as menthol, thymol, etc. Among them, menthol, as one of the most sold spices in the world, is widely used in the food industry, daily fine chemicals and medicine and hygiene And other fields, with huge market demand. [0004] Isopulegol is an important intermediate in the production of menthol. The current traditional preparation method is to use citronellal under the catalysis of Lewis acid-base pair to prepare by cyclization reaction, and usually obtain the form of a mixture of four enantiomers , namely isopulegol, iso-isopulegol, neo-isopulegol, new iso-isopulegol. [0005] CN 107188781 discloses a method for preparing isopulegol by using the cyclization reaction of cit...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C29/74C07C29/88C07C29/80C07C35/17
CPCY02P20/584
Inventor 王亚新董菁张永振黎源
Owner WANHUA CHEM GRP CO LTD
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