High-purity piperonal production process

A technology for the production of jasronal, which is applied in the field of high-purity jasronal production technology, and can solve the problem that the aroma and type of jasronal are not pure and long-lasting, and the purity of jasronal and crystals of jasronal cannot be improved. Poor shape and other problems, to achieve the effect of automatic control transformation of the process, mellow aroma, and longer-lasting aroma

Inactive Publication Date: 2010-04-14
重庆德馨香料植物开发有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The production technology of the prior art jasronal generally focuses on solving the problems such as the poor crystal form of jasronal, uneven particle size distribution, and easy coalescence

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Example Embodiment

[0014] Example 1

[0015] In the production process of high-purity jasmine aldehyde of the present embodiment, the crude jasmine aldehyde product is formed through the steps of isomerization, oxidation and water-washing reduction, and the crude product of jasmine aldehyde is purified and purified successively through the steps of fractionation, crystallization, centrifugal separation and drying;

[0016] The crystallization step adopts subsection cooling and cooling crystallization process:

[0017] a. After mixing the jasmonaldehyde and alcohol, put it in the crystallization kettle, the temperature in the crystallization kettle is 35 ℃-40 ℃, after all the jasmonaldehyde is dissolved in the alcohol, the temperature is kept for 20 minutes; 20 minutes can not only meet the process requirements, but also save energy and reduce costs; of course, the holding time can be extended, but the holding time in this embodiment is beneficial to improve production efficiency.

[0018] b. St...

Example Embodiment

[0025] Embodiment 2

[0026] In the production process of high-purity jasmine aldehyde of the present embodiment, the crude jasmine aldehyde product is formed through the steps of isomerization, oxidation and water-washing reduction, and the crude product of jasmine aldehyde is purified and purified successively through the steps of fractionation, crystallization, centrifugal separation and drying;

[0027] The crystallization step adopts subsection cooling and cooling crystallization process:

[0028] a. After mixing the jasmonaldehyde and alcohol, put it in the crystallization kettle, the temperature in the crystallization kettle is 35 ℃-40 ℃, after the jasmonaldehyde is completely dissolved in the alcohol, the temperature is kept for 40 minutes;

[0029] b. Start freezing and crystallization. The temperature in the crystallization kettle is lowered at a cooling rate of 3 °C-5 °C / h. After the temperature in the crystallization kettle is lowered to 8 °C, the mixture of jasmon...

Example Embodiment

[0032] Embodiment 3

[0033] The high-purity jasmine aldehyde production process of the present embodiment forms a crude jasmine aldehyde product through isomerization and oxidation steps, and the crude jasmine aldehyde product is successively purified and purified through the steps of washing, fractional distillation, crystallization, centrifugation and drying;

[0034] The crystallization step adopts subsection cooling and cooling crystallization process:

[0035] a. Mix the jasmonaldehyde with alcohol and place it in the crystallization kettle. The temperature in the crystallization kettle is 35°C-40°C. After the jasmonaldehyde is completely dissolved in the alcohol, the temperature is kept for 20 minutes;

[0036] b. Start freezing and crystallization. The temperature in the crystallization kettle is lowered at a cooling rate of 3 °C-5 °C / h. After the temperature in the crystallization kettle is lowered to 10 °C, the mixture of jasmonal and alcohol is kept under stirring f...

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PUM

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Abstract

The invention discloses a high-purity piperonal production process. Crude piperonal is formed after steps of isomerism, oxidation, washing and reduction and is refined and purified sequentially through steps of fractionation, crystallization, centrifugal separation and drying, wherein the step of crystallization adopts stage cooling temperature reduction crystallization process. The piperonal product of the invention improves obviously in quality and has the purity up to 99.9 percent, stronger and more lasting sweet smell, mellow odor type and sweeter and crisper aftertaste. By adopting kettle type segmentation temperature reduction crystallization process, the process of temperature reduction is relatively moderate, thus avoiding the simultaneous crystallization of impurities and piperonal to the maximum degree, reducing the content of impurities in the piperonal to the minimum degree and further abating the influence of impurities on the sweet smell of piperonal to the minimum degree. Therefore, the sweet smell of the high-purity piperonal is superior to that of common granular piperonal. The product is in the form of powder, has excellent mobility after being mixed with alcohol and is beneficial to the automation control transformation of the process.

Description

technical field [0001] The invention relates to a production process of jasmonal, in particular to a production process of high-purity jasmonal. Background technique [0002] Jasmonal is an important fine chemical and organic synthesis intermediate, which is widely used in food, daily chemical, fine chemical, pharmaceutical and other industries. With jasmonal as raw material, dozens of derivative fine chemical products can be developed, such as jasmonal, piperonyl acetone, jasmonol, jasmononitrile, etc., which can be used as fragrances for soap, perfume, and cosmetic production. In addition, the use of jasmonal can also be used to develop intermediate sesamol for drug production and synthesis of high-grade anti-mold and antibacterial synergists, synergist methylenedioxyphenyl alkyl ether for pesticide pyrethrins, anti-tumor And downstream deep processing derivative products such as drug intermediates and alkaloids for the prevention and treatment of hypertension. [0003] ...

Claims

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Application Information

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IPC IPC(8): C07D317/54
Inventor 刘松何渊
Owner 重庆德馨香料植物开发有限公司
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