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Refining method of coumarin crude product

A purification method and technology for coumarin, applied in the direction of organic chemistry, etc., can solve the problems of low processing efficiency and cumbersome processing method, and achieve the effect of improving processing efficiency, saving personnel and ensuring rectification.

Inactive Publication Date: 2017-06-20
成都建中香料香精有限公司
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Problems solved by technology

[0008] For the post-treatment method of the crude coumarin obtained through the Perkin reaction, the coumarin is often extracted by rectification in industry. Phenyl esters, finished products and post-distillation; and these processes are all batch-type treatment processes, the treatment methods are cumbersome, and the treatment efficiency is low

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  • Refining method of coumarin crude product
  • Refining method of coumarin crude product
  • Refining method of coumarin crude product

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Embodiment 1

[0044] According to attached figure 1 Coumarin is purified using the process described in figure 1 For the process flow diagram of the purification method of coumarin provided by the present invention; Wherein, the process parameter of each step operation is as shown in table 1:

[0045] Table 1

[0046]

[0047]

[0048]

[0049]

[0050] Experimental results show that the coumarin purification method provided by the invention, through four sets of continuous towers (dehydration, dephenylesterification, removal of fore distillation, finished product) through the coumarin crude product, two sets of intermittent towers (finish dehydration, rear distillation) ). The crystallization process adopts a total of two sets of dynamic crystallization, four sets of one time and four sets of two times; the purification of the crude coumarin is realized by the main continuous and partly intermittent process; the distillation yield is 98.5-99.5%, and the coumarin content is 97...

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Abstract

The invention provides a refining method of a coumarin crude product. The refining method comprises the following steps of first mixing the coumarin crude product prepared through a perkin reaction and water, so as to obtain a water-containing coumarin crude product; afterwards, subjecting the water-containing coumarin crude product to a coarse water removal process, a phenyl ester removal process, before-removal rectification process and a finished product outputting process in sequence through continuous rectification, so as to obtain a coumarin pure product. According to the refining method, through controlling process conditions in the coarse water removal process, the phenyl ester removal process, the before-removal rectification process and the finished product outputting process, a purification method provided by the invention can be used for realizing the continuous rectification; not only are the quality and the yield of a coumarin rectified product guaranteed, but also the high efficiency and the energy conservation of the rectification are guaranteed.

Description

technical field [0001] The invention relates to the field of organic matter purification, in particular to a method for purifying crude coumarin. Background technique [0002] Coumarin (coumarin), the scientific name is o-hydroxylauric acid lactone, also known as coumarin, and its molecular formula is C 9 h 6 o 2 , relative molecular mass 146.15, its structural formula is as shown in formula (I), [0003] [0004] Coumarin is a white crystal or crystalline powder with a strong aroma of tonka bean and chocolate, bitter in taste and capable of sublimation. The melting point is 68-70°C, and the boiling point is 297-299°C. Insoluble in cold water, soluble in hot water, ethanol, ether and chloroform. It is an important spice, often used as a fixative, used to prepare violet, lavender, orchid and other flavors, and also used as a flavor enhancer for beverages, food, cigarettes, rubber products, plastic products, etc. Used as a brightener in the electroplating industry. C...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D311/10
CPCC07D311/10
Inventor 李良龙蒲勇曾林久马妙玲陈军
Owner 成都建中香料香精有限公司
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