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A kind of purification method of 2-methyl-4-isothiazolin-3-one

A technology of isothiazoline and purification method, applied in the direction of organic chemistry, etc., can solve the problem of low purity of MIT

Active Publication Date: 2021-10-01
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 U.S. patent document with the application number US08220763 discloses a preparation method of a 3-isothiazolinone biofungicide, the main technical scheme of which is to dissociate the mixture of MIT and CMI by heating the selective dissociation hydrochloride to decompose the CMI MIT is isolated and dissolved in a solvent, and MIT is separated separately in the form of hydrochloride. Although this method can realize the separation of MIT and CMI, the purity of MIT obtained is low

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  • A kind of purification method of 2-methyl-4-isothiazolin-3-one

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Embodiment 1

[0035] The purification method of the 2-methyl-4-isothiazolin-3-one of the present embodiment comprises the following steps:

[0036] 25g MIT reagent (purity is 95%, Aladdin reagent company) is dissolved in 50mL ethyl acetate, then pours into the funnel of sand core that is connected with water pump and carries out suction filtration, then washes funnel of sand core with ethyl acetate again, obtains Primary filtrate; add 3g of anhydrous sodium sulfate in primary filtrate and dry 1h, remove the moisture in primary filtrate and remove anhydrous sodium sulfate by suction again to obtain secondary filtrate, then wash anhydrous sodium sulfate with ethyl acetate to obtain washing liquid, Then the secondary filtrate and washing liquid were collected in a 250mL round-bottomed flask and evaporated with a rotary evaporator to remove the volatile solvent ethyl acetate to obtain a white solid. The white solid was washed with petroleum ether and filtered to obtain a solid (repeat 3 times, ...

Embodiment 2

[0039] The purification method of the 2-methyl-4-isothiazolin-3-one of the present embodiment comprises the following steps:

[0040]20g MIT reagent (purity is 95%, Aladdin Reagent Company) is dissolved in 40mL ethyl acetate, then pours into the funnel of sand core that is connected with water pump and carries out suction filtration, then washes funnel of sand core with ethyl acetate, Obtain the primary filtrate; add 2 g of anhydrous sodium sulfate to the primary filtrate and dry for 1 h, remove the moisture in the primary filtrate and then filter again to remove the anhydrous sodium sulfate to obtain the secondary filtrate, then wash the anhydrous sodium sulfate with ethyl acetate to obtain the washing liquid , and then the secondary filtrate and washing liquid were collected in a 250mL round bottom flask and carried out rotary evaporation with a rotary evaporator, and the volatile solvent ethyl acetate was removed to obtain a white solid. The white solid was washed with petr...

Embodiment 3

[0043] The purification method of the 2-methyl-4-isothiazolin-3-one of the present embodiment comprises the following steps:

[0044] 10g of MIT reagent (purity is 95%, Bailingwei Technology Co., Ltd.) was dissolved in 25mL ethyl acetate, then poured into the sand core funnel connected with the water pump for suction filtration, and then the sand core funnel was washed with ethyl acetate to obtain Primary filtrate; add 2g of anhydrous sodium sulfate to the primary filtrate and dry for 1h, remove the moisture in the primary filtrate by suction filtration again to remove anhydrous sodium sulfate to obtain the secondary filtrate, then wash the anhydrous sodium sulfate with ethyl acetate to obtain the washing liquid, Then the secondary filtrate and washing liquid were collected in a 250mL round-bottomed flask and evaporated with a rotary evaporator to remove the volatile solvent ethyl acetate to obtain a white solid. The white solid was washed with petroleum ether and filtered to ...

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Abstract

The invention belongs to the technical field of organic matter purification, in particular to a method for purifying 2-methyl-4-isothiazoline-3-one. The purification method of 2-methyl-4-isothiazoline-3-ketone of the present invention comprises the following steps: dissolving the crude product of 2-methyl-4-isothiazoline-3-ketone in an organic solvent, and then filtering to obtain the filtrate ; Remove the organic solvent in the filtrate to obtain a solid, and then wash the solid and recrystallize the mixed solvent. The purity of the 2-methyl-4-isothiazolin-3-one purified by the purification method of the present invention reaches 99.9%, which effectively improves the purity of the crude 2-methyl-4-isothiazolin-3-one.

Description

technical field [0001] The invention belongs to the technical field of organic matter purification, and in particular relates to a method for purifying 2-methyl-4-isothiazolin-3-one. Background technique [0002] 2-Methyl-4-isothiazolin-3-one (MIT) is a fungicide with high efficiency, good spectrum and good compatibility, which is widely used in pulp and paper making, cosmetics, personal care products, coatings, adhesives, inks Anticorrosion and sterilization of products in industries such as tanning and tanning. MIT is a kind of sensitizer, which will cause allergy or dermatitis and other symptoms in contact with the skin, and has certain cytotoxicity and neurotoxicity. There are strict restrictions on the use of isothiazolinone fungicides in food contact materials, toys, cosmetics and other daily necessities at home and abroad, and the mass percentage of MIT shall not exceed 0.01%. At present, the purity of MIT reagents provided by domestic reagent companies is 95%. Ther...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07D275/03
CPCC07D275/03
Inventor 叶长文闫晓宇范黎贺琛蒋锦锋苗芊张勍陈连芳李青常王佟曹瑞曾波
Owner ZHENGZHOU TOBACCO RES INST OF CNTC
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