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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 of the product. The jasronal product has more impurities and cannot improve the jasronal higher. Therefore, it cannot effectively make the aroma and fragrance of jasminal more pure and lasting

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0015] In the high-purity jasmonal production process of this embodiment, the crude jasmonal is formed through the steps of isomerization, oxidation and water washing and reduction, and the crude jasmonal is refined and purified through fractionation, crystallization, centrifugation and drying steps in turn;

[0016] The crystallization step adopts the staged cooling and cooling crystallization process:

[0017] a. Mix jasmonal with alcohol and put it into the crystallization kettle. The temperature in the crystallization kettle is 35°C-40°C. After the jasmonal is completely dissolved in alcohol, keep warm for 20 minutes; in this embodiment, the heat preservation time of this step adopts 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 conducive to improving production efficiency.

[0018] b. Start to freeze and crystallize, and cool down the tem...

Embodiment 2

[0026] In the high-purity jasmonal production process of this embodiment, the crude jasmonal is formed through the steps of isomerization, oxidation and water washing and reduction, and the crude jasmonal is refined and purified through fractionation, crystallization, centrifugation and drying steps in turn;

[0027] The crystallization step adopts the staged cooling and cooling crystallization process:

[0028] a. Mix the jasmonal with alcohol and put it into the crystallization kettle. The temperature in the crystallization kettle is 35°C-40°C. After the jasmonal is completely dissolved in the alcohol, keep it warm for 40 minutes;

[0029] b. Start to freeze and crystallize, and cool down the temperature in the crystallization tank at a cooling rate of 3°C-5°C / h. After the temperature in the crystallization tank drops to 8°C, keep the mixture of jasmonal and alcohol under stirring for 2 hours and then enter the centrifugal separation step.

[0030] In this embodiment, the d...

Embodiment 3

[0033] In the high-purity jasmonal production process of this embodiment, the crude jasmonal is formed through the steps of isomerization and oxidation, and the crude jasmonal is refined and purified by washing, fractional distillation, crystallization, centrifugation and drying in sequence;

[0034] The crystallization step adopts the staged cooling and cooling crystallization process:

[0035] a. Mix jasmonal with alcohol and put it into a crystallization kettle. The temperature in the crystallization kettle is 35°C-40°C. After the jasmonal is completely dissolved in alcohol, keep warm for 20 minutes;

[0036] b. Start to freeze and crystallize, and cool down the temperature in the crystallization tank at a cooling rate of 3°C-5°C / h. After the temperature in the crystallization tank drops to 10°C, keep the mixture of jasmonal and alcohol under stirring for 2 hours and then enter into centrifugation. step.

[0037] In this embodiment, the drying step adopts a rotary vacuum d...

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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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