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Preparation method of high-quality 1, 3-cyclohexanedione product

A cyclohexanedione, high-quality technology, applied in the field of chemical synthesis, can solve the problems of difficult storage, low overall content, 1,3-cyclohexanedione appearance, quality problems, etc., and achieve the effect of not easy to change color

Active Publication Date: 2021-03-30
浙江清和新材料科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, the appearance and quality of the 1,3-cyclohexanedione obtained by this method have relatively large problems.
The overall content of 1,3-cyclohexanedione in the finished product obtained in this way is not high (the content of inorganic salt is about 1%), the finished product is easy to change color and agglomerate, and is not easy to store
Simultaneously, because 1,3-cyclohexanedione has better solubility in water, uncontrolled crystallization process often leads to the yield of final product 1,3-cyclohexanedione being only about 90%

Method used

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  • Preparation method of high-quality 1, 3-cyclohexanedione product
  • Preparation method of high-quality 1, 3-cyclohexanedione product

Examples

Experimental program
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Effect test

experiment example 1

[0030] Preparation of high-quality seed crystals: 400kg of 1,3-cyclohexanedione solid (i.e., for example, the 1,3-cyclohexanedione solid prepared in Comparative Example 1 of the present invention) and 1000kg of toluene were added to a 1500L enamel kettle, and stirred Heat to 40°C, after all dissolves, cool down to 0-5°C, solids slowly precipitate out, continue to stir for 2 hours, discharge the feed liquid into a three-in-one filter to filter dry, and discharge the feed into a dryer after drying. Material, obtain the white powdery crystal of moisture content about 0.08%. The purity is 99.97% (HPLC purity, the same below), the yield is 98.11%, and the inorganic salt content is 0.21%. The obtained product was placed in a constant temperature and humidity chamber (temperature 35° C., humidity 40%) for 3 months without discoloration, caking and the like. Carry out powder XRD analysis to described white powdery crystal, the result sees figure 1 . The white powder crystal is the ...

experiment example 2

[0033]Preparation of high-quality 1,3-cyclohexanedione product: Add 300kg of water into a 3000L enamel crystallization kettle, add 60kg of high-quality 1,3-cyclohexanedione crystal seeds under stirring conditions, and prepare the high-quality crystal seeds The method is consistent with the preparation method of high-quality seed crystals in Example 1, and the temperature is controlled at 5-10 ° C; at the same time, 1500 kg of hydrogenation reaction solution and 450 kg of industrial hydrochloric acid with a concentration of 31% are pumped into the crystallization kettle, the feeding time is controlled at 2 hours, and the temperature is controlled At 5-10°C. After the reaction is completed, when the temperature is lowered to -5 ~ 0°C, the feed liquid enters the centrifuge to dry, and after drying, the material is discharged into the dryer, and the material is discharged after drying to obtain a white powder crystal with a moisture content of about 0.30%. The purity is 99.96%, th...

experiment example 3

[0035] Preparation of high-quality 1,3-cyclohexanedione product: Add 300kg of water into a 3000L enamel crystallization kettle, and leave 50kg of the high-quality 1,3-cyclohexanedione product prepared in Example 2 in the enamel crystallization kettle as For seed crystals, the temperature is controlled at 5-10°C; at the same time, 1500kg of hydrogenation reaction solution and 450kg of 31% industrial hydrochloric acid are pumped into the crystallization tank, the feeding time is controlled at 2h, and the temperature is controlled at 5-10°C. After the reaction is completed, when the temperature is lowered to -5 ~ 0°C, the feed liquid enters the centrifuge to dry, and after drying, the material is discharged into the dryer, and the material is discharged after drying to obtain a white powder crystal with a moisture content of about 0.32%. The purity is 99.94%, the yield is 95.86%, and the inorganic salt content is 0.27%. The obtained product was placed in a constant temperature an...

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Abstract

The invention provides a preparation method of a high-quality 1, 3-cyclohexanedione product, which comprises the following steps: carrying out hydrogenation reaction on resorcinol and strong base in the presence of hydrogen and a solid catalyst, and carrying out solid-liquid separation to remove the solid catalyst after the reaction is completed, thereby obtaining a hydrogenation reaction solution; and simultaneously adding a hydrogenation reaction solution and hydrochloric acid in the presence of the high-quality seed crystal and water, carrying out acidification reaction, cooling, crystallizing, and drying the obtained crystal to obtain the high-quality 1, 3-cyclohexanedione product. The high-quality seed crystal is a high-quality 1, 3-cyclohexanedione seed crystal obtained by dissolvinga 1, 3-cyclohexanedione solid in an organic solvent and then carrying out cooling crystallization. The obtained high-quality 1, 3-cyclohexanedione product is a white crystal, recrystallization purification is not needed, the inorganic salt content of the product is as low as 0.5% or below, the purity of the product is higher than 99.9%, refrigeration is not needed in the transportation and storage process, and the phenomena of discoloration, caking and the like are not likely to happen even in the international sea transportation process.

Description

technical field [0001] The invention belongs to the technical field of chemical synthesis, and in particular relates to a method for preparing a high-quality 1,3-cyclohexanedione product. Background technique [0002] 1,3-Cyclohexanedione is an organic compound with a wide range of uses. It is not only the synthetic clinical specific analgesic drug mebutamol, the specific drug carvedilol for the protection of cardiovascular and cerebrovascular, and the treatment of high blood pressure, but also an antiemetic drug. The intermediate of ondansetron is also the necessary intermediate for the synthesis of pesticides such as mesotrione and mesotrione, which are highly effective corn herbicides. [0003] Generally, the reduction method is used to synthesize 1,3-cyclohexanedione, that is, resorcinol is used as raw material, water is used as solvent, after adding caustic soda to form phenoxide, the benzene ring is hydrogenated and reduced using a metal catalyst, and after the hydroge...

Claims

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Application Information

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IPC IPC(8): C07C49/403C07C45/81C07C45/00C07C49/713
CPCC07C45/81C07C45/00C07C45/006C07C2601/14C07C49/403C07C49/713Y02P20/584
Inventor 洪俊杰范占成杨荣强王凌云符建琼
Owner 浙江清和新材料科技有限公司
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