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Purification method of 2-methyl-4-isothiazolin-3-ketone

A technology of isothiazoline and purification method, which is applied in organic chemistry and other fields, and can solve problems such as low purity

Active Publication Date: 2019-06-21
ZHENGZHOU TOBACCO RES INST OF CNTC +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

The process or method in the prior art can obtain MIT with relatively low purity. Through inquiries on websites such as Bailingwei Technology Co., Ltd., Aladdin Reagent, Shanghai Merrill Chemical Technology Co., Ltd., and Sinopharm Chemical Reagent Co., Ltd., domestic reagent companies can only Provides analytically pure MIT with a purity of 95%, and MIT with higher purity has not been reported yet

Method used

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  • Purification method of 2-methyl-4-isothiazolin-3-ketone
  • Purification method of 2-methyl-4-isothiazolin-3-ketone

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Embodiment 1

[0024] The purification method of the present embodiment 2-methyl-4-isothiazolin-3-one comprises the following steps:

[0025] (1) Mix 25g of 2-methyl-4-isothiazolin-3-one reagent (purity is 95%, purchased from Aladdin Company) with 10mL acetone (chromatographically pure 99.8%, purchased from Merck Company), and heat up to 40°C, stirred until completely dissolved, kept warm for 10 minutes, and filtered to obtain the mixed solution.

[0026] (2) Place the mixed solution in an environment of 25° C. to cool naturally for 3 hours, and then place it in an environment of 4° C. to cool for 5 hours, and then perform suction filtration to obtain crystals.

[0027] (3) The crystals were washed 3 times with petroleum ether.

[0028] The above steps (1), (2) and (3) are all completed in an inert gas glove box, and the inert gas is nitrogen.

[0029] (4) The washed crystals were subjected to vacuum freeze-drying at a temperature of -80° C., a vacuum degree of <0.12 Mbar, and a drying tim...

Embodiment 2

[0031] The purification method of the present embodiment 2-methyl-4-isothiazolin-3-one comprises the following steps:

[0032] (1) 25g of 2-methyl-4-isothiazolin-3-one reagent (purity is 95%, Bailingwei Technology Co., Ltd.) is mixed with 25mL ethyl acetate (chromatographically pure 99.9%, purchased from Merck Co.), and the temperature is raised to 50°C, stir until completely dissolved, keep warm for 20 minutes, and filter to obtain the mixture.

[0033] (2) Place the mixed solution in an environment of 20° C. to cool naturally for 3 hours, and then place it in an environment of 8° C. to cool for 5 hours, and then perform suction filtration to obtain crystals.

[0034] (3) The crystals were washed 3 times with petroleum ether.

[0035] The above steps (1), (2) and (3) are all completed in an inert gas glove box, and the inert gas is argon.

[0036] (4) The washed crystals were subjected to vacuum freeze-drying at a temperature of -40° C., a vacuum degree of <0.12 Mbar, and a...

Embodiment 3

[0038] The purification method of the present embodiment 2-methyl-4-isothiazolin-3-one comprises the following steps:

[0039] (1) 25g of 2-methyl-4-isothiazolin-3-one reagent (purity is 95%, Bailingwei Technology Co., Ltd.) is mixed with 25mL ethyl acetate (chromatographically pure 99.9%, purchased from Merck Co.), and the temperature is raised to 45°C, stirred until completely dissolved, kept warm for 15 minutes, and filtered to obtain the mixture.

[0040] (2) The mixture was naturally cooled at 23°C for 3 hours, then cooled at 0°C for 5 hours, and suction filtered to obtain crystals.

[0041] (3) The crystals were washed 3 times with petroleum ether.

[0042] The above steps (1), (2) and (3) are all completed in an inert gas glove box, and the inert gas is nitrogen.

[0043] (4) The washed crystals were subjected to vacuum freeze-drying at a temperature of -80° C., a vacuum degree of <0.12 Mbar, and a drying time of 4 days, and finally 21.2 g of snow-white crystals were ...

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Abstract

The invention relates to a purification method of 2-methyl-4-isothiazolin-3-ketone, and belongs to the technical field of organic matter purification and separation. The purification method comprisesthe following steps: (1) mixing 2-methyl-4- isothiazolin-3-ketone with an organic solvent, heating the mixture to 40 to 50 DEG C, and performing solid-liquid separation to obtain a mixed solution, wherein the organic solvent is acetone or ethyl acetate; (2) cooling the liquid mixture after the solid-liquid separation in step (1) to 0 to 10 DEG C, and performing crystallization and solid-liquid separation to obtain a solid; (3) performing vacuum freeze-drying on the solid obtained after solid-liquid separation in step (2), to obtain 2-methyl-4-isothiazolin-3-ketone. The 2-methyl-4-isothiazoline-3-one obtained according to this method has high purity, less impurities, and extremely low moisture content (mass percentage less than 0.1%), and can be used as a candidate for a purity standard substance.

Description

technical field [0001] The invention relates to a method for purifying 2-methyl-4-isothiazolin-3-one, which belongs to the technical field of organic matter purification and separation. Background technique [0002] 2-Methyl-4-isothiazolin-3-one (MIT) is a high-efficiency, broad-spectrum, and good compatibility fungicide, which is widely used in pulp and paper, cosmetics, personal care products, coatings, adhesives, Anticorrosion and sterilization of industrial products such as ink and leather. MIT is usually used in combination with 5-chloro-2-methyl-4-isothiazolin-3-one (CMI) at a mass ratio of 1:3, and its trade name is Kathon or Kathon (CG). The fungicide MIT is a kind of sensitizer, it will cause allergy or dermatitis and other symptoms in contact with the skin, and it has certain cytotoxicity and neurotoxicity. There are strict restrictions on the use of related isothiazolinone fungicides in food contact materials, toys, cosmetics and other daily necessities at home ...

Claims

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Application Information

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IPC IPC(8): C07D275/03
Inventor 范黎叶长文黄世杰贺琛周芸韦康邹林陈志燕陈宸陈连芳李小兰李青常
Owner ZHENGZHOU TOBACCO RES INST OF CNTC
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