CN103204823A - Method for purifying 1, 2-benzisothiazole-3-ketone - Google Patents
Method for purifying 1, 2-benzisothiazole-3-ketone Download PDFInfo
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- CN103204823A CN103204823A CN2013100847757A CN201310084775A CN103204823A CN 103204823 A CN103204823 A CN 103204823A CN 2013100847757 A CN2013100847757 A CN 2013100847757A CN 201310084775 A CN201310084775 A CN 201310084775A CN 103204823 A CN103204823 A CN 103204823A
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Abstract
The invention belongs to the field of fine chemicals, and relates to a method for purifying 1, 2-benzisothiazole-3-ketone (BIT). Water-soluble polar proton solvents and water are mixed to form solvents to be re-crystallized so as to obtain snow-white granular 1, 2-benzisothiazole-3-ketone. The method particularly includes steps of mixing the water-soluble polar proton solvents with the water to obtain the solvents; mixing the obtained solvents with the 1, 2-benzisothiazole-3-ketone; heating a mixture of the solvents and the 1, 2-benzisothiazole-3-ketone until the mixture is dissolved completely; decoloring and filtering the mixture to obtain filter liquor; cooling the obtained filter liquor; filtering the filter liquor to obtain 1, 2-benzisothiazole-3-ketone crystals; and drying the obtained crystals. The method has the advantages that consumption of acid, alkali and a large quantity of water is omitted, pollution is greatly reduced, and the obtained products are high in quality and content, contain few impurities and are granular; as BIT has a severe irritation effect on respiratory ducts of human bodies and a BIT powder layer can be prevented from being inhaled by the human bodies, operation conditions are greatly improved; and the granular products are easy to dry, and production processes needing anhydrous BIT can be greatly facilitated as the granular products do not contain crystallization water.
Description
[technical field]
The invention belongs to field of fine chemical, relate to the method for purification of compound, specifically a kind of 1, the method for purification of 2-benzisothiazole-3-ketone.
[background technology]
1,2-benzisothiazole-3-ketone (BIT, formula I) is widely used in sterilant, sanitas, and its traditional method of purification is to adopt acid-base method, is solvent with big water gaging, with the liquid caustic soda dissolving, then separates out with hydrochloric acid earlier, obtains 1.2-benzisothiazole-3-ketone powder.Yet this method of purification has the following disadvantages: not only can produce a large amount of brine wastes, quality product is low, and dust is many, and operational condition is poor.
Therefore, if a kind of avoid using soda acid and big water gaging can be provided, reduce and pollute, and good product quality, the content height greatly improves 1 of operational condition, and 2-benzisothiazole-3-ketone method of purification will have very important significance.
[summary of the invention]
Purpose of the present invention is exactly will solve above-mentioned deficiency and provide a kind of 1, and the method for purification of 2-benzisothiazole-3-ketone has not only been avoided use soda acid and big water gaging, greatly reduced pollution, and the products obtained therefrom quality is good, the content height, impurity is few, has greatly improved condition.
Design a kind ofly 1 for achieving the above object, the method for purification of 2-benzisothiazole-3-ketone may further comprise the steps:
1) water-soluble polar aprotic solvent is mixed with water make solvent, gained solvent and 1,2-benzisothiazole-3-ketone are mixed, be warming up to moltenly entirely, decolorization filtering gets filtrate;
2) gained filtrate is cooled, filter 1,2-benzisothiazole-3-ketone crystal, and dry gained crystal.
In some embodiments of the present invention, described water-soluble polar aprotic solvent is one or more the combination in methyl alcohol, ethanol, acetic acid, acetone, propyl alcohol, butanols, acetonitrile, the formic acid, is preferably methyl alcohol.
In some embodiments of the present invention, in the step 1) 1,2-benzisothiazole-3-ketone and water-soluble polar aprotic solvent mass ratio are 1.5-4.5, are preferably 2-3, and water and 1,2-benzisothiazole-3-ketone mass ratio is 0-2, is preferably 0.5-1.5.
In certain preferred embodiments of the present invention, in the step 1) 1,2-benzisothiazole-3-ketone and dissolution with solvents temperature are 40-120 ℃, are preferably 60-80 ℃.
In certain preferred embodiments of the present invention, step 2) cooling temperature is 0-35 ℃ in, is preferably 10-25 ℃.
In certain preferred embodiments of the present invention, step 2) time of cooling is 1.5-8h in, is preferably 1-3h.
When cooling in some embodiments of the present invention, step 2), filtrate is stirred, stirring velocity is 25-55RPM, is preferably 30-40RPM.
The present invention compares with prior art, has following beneficial effect: make solvent recrystallization owing to adopt water-soluble polar aprotic solvent to mix with water, obtained snow-white particulate state 1,2-benzisothiazole-3-ketone, avoid use soda acid and big water gaging, greatly reduced pollution; And on the one hand, the products obtained therefrom quality is good, the content height, and impurity is few, can satisfy some special purposes; On the other hand, products obtained therefrom is particulate state, can prevent that the BIT bisque from being sucked by human body, because the people's of BIT respiratory tract has serious hormesis, thereby has greatly improved operational condition; In addition, granular product is dry easily, be not with crystal water after, will have very big benefit to the production technique of the BIT that needs anhydrous state.
[description of drawings]
Fig. 1 is that the HPLC of 1,2-benzisothiazole-3-ketone standard substance detects data;
Fig. 2 is that the HPLC of embodiment 1 products therefrom detects data.
[embodiment]
Further specify below doing below in conjunction with the present invention of embodiment:
Experimental example 1
Throw 1,2-benzisothiazole-3-ketone 160g, methyl alcohol 450g, water 130g, be warming up to 65 ℃ complete molten, add the 1.5g gac, insulation 30min filters gained filtrate, transfer slowly and stir, slowly be cooled to 20 ℃, need 1h approximately, filter, the 100g cold water washing, dry the snow-white particle 1 of 145g, 2-benzisothiazole-3-ketone (HPLC〉99.85%), yield 90.6%.
Experimental example 2
Throw 90% solid content 1,2-benzisothiazole-3-ketone 178g, methyl alcohol 450g, water 110g, be warming up to 66 ℃ complete molten, add the 1.5g gac, insulation 30min filters gained filtrate, transfer slowly and stir, slowly be cooled to 20 ℃, need 1h approximately, filter, the 100g cold water washing, dry the snow-white particle 1 of 143g, 2-benzisothiazole-3-ketone (HPLC〉99.85%), yield 89.3%.
Experimental example 3
Throw 1,2-benzisothiazole-3-ketone 160g, ethanol 420g, water 135g, be warming up to 70 ℃ complete molten, add the 1.5g gac, insulation 30min filters gained filtrate, transfer slowly and stir, slowly be cooled to 20 ℃, need 1h approximately, filter, the 100g cold water washing, dry the snow-white particle 1 of 140g, 2-benzisothiazole-3-ketone (HPLC〉99.85%), yield 87.5%.
Should be understood that; the present invention is not subjected to the restriction of above-mentioned embodiment; other any do not deviate from change, the modification done under spirit of the present invention and the principle, substitutes, combination, simplify, and all should be the substitute mode of equivalence, is included within protection scope of the present invention.
Claims (7)
1. the method for purification of 2-benzisothiazole-3-ketone is characterized in that, may further comprise the steps:
1) water-soluble polar aprotic solvent is mixed with water make solvent, gained solvent and 1,2-benzisothiazole-3-ketone are mixed, be warming up to moltenly entirely, decolorization filtering gets filtrate;
2) gained filtrate is cooled, filter 1,2-benzisothiazole-3-ketone crystal, and dry gained crystal.
2. the method for claim 1 is characterized in that: described water-soluble polar aprotic solvent is one or more the combination in methyl alcohol, ethanol, acetic acid, acetone, propyl alcohol, butanols, acetonitrile, the formic acid, is preferably methyl alcohol.
3. method as claimed in claim 1 or 2 is characterized in that: in the step 1) 1,2-benzisothiazole-3-ketone and water-soluble polar aprotic solvent mass ratio are 1.5-4.5, be preferably 2-3, water and 1,2-benzisothiazole-3-ketone mass ratio is 0-2, is preferably 0.5-1.5.
4. method as claimed in claim 3 is characterized in that: in the step 1) 1,2-benzisothiazole-3-ketone and dissolution with solvents temperature are 40-120 ℃, are preferably 60-80 ℃.
5. method as claimed in claim 4 is characterized in that: step 2) in cooling temperature be 0-35 ℃, be preferably 10-25 ℃.
6. method as claimed in claim 5 is characterized in that: step 2) in the time of cooling be 1.5-8h, be preferably 1-3h.
7. method as claimed in claim 6 is characterized in that: step 2) in when cooling, filtrate is stirred, stirring velocity is 25-55RPM, is preferably 30-40RPM.
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105753805A (en) * | 2016-03-31 | 2016-07-13 | 寿光新泰精细化工有限公司 | Method for purifying 1,2-benzisothiazole-3-ketone |
| CN105801516A (en) * | 2016-04-28 | 2016-07-27 | 大丰跃龙化学有限公司 | Purification process of 1,2-benzisothiazolin-3-ketone |
| CN108794424A (en) * | 2018-07-16 | 2018-11-13 | 连云港市三联化工有限公司 | A kind of method for refining solvent of BIT |
| CN109970677A (en) * | 2019-04-23 | 2019-07-05 | 中国烟草总公司郑州烟草研究院 | A kind of method of purification of 1,2-benzisothiazolin-3-one |
| CN111559986A (en) * | 2020-06-22 | 2020-08-21 | 大连百傲化学股份有限公司 | Purification method of 1, 2-benzisothiazolin-3-ketone |
| CN114181124A (en) * | 2021-12-13 | 2022-03-15 | 大连百傲化学股份有限公司 | Recycling treatment method of 1, 2-benzisothiazolin-3-one chlorination process wastewater |
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Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105753805A (en) * | 2016-03-31 | 2016-07-13 | 寿光新泰精细化工有限公司 | Method for purifying 1,2-benzisothiazole-3-ketone |
| CN105801516A (en) * | 2016-04-28 | 2016-07-27 | 大丰跃龙化学有限公司 | Purification process of 1,2-benzisothiazolin-3-ketone |
| CN105801516B (en) * | 2016-04-28 | 2018-05-04 | 大丰跃龙化学有限公司 | A kind of 1,2- benzisothiazole-3-ketones purifying technique |
| CN108794424A (en) * | 2018-07-16 | 2018-11-13 | 连云港市三联化工有限公司 | A kind of method for refining solvent of BIT |
| CN109970677A (en) * | 2019-04-23 | 2019-07-05 | 中国烟草总公司郑州烟草研究院 | A kind of method of purification of 1,2-benzisothiazolin-3-one |
| CN111559986A (en) * | 2020-06-22 | 2020-08-21 | 大连百傲化学股份有限公司 | Purification method of 1, 2-benzisothiazolin-3-ketone |
| CN114181124A (en) * | 2021-12-13 | 2022-03-15 | 大连百傲化学股份有限公司 | Recycling treatment method of 1, 2-benzisothiazolin-3-one chlorination process wastewater |
| CN114181124B (en) * | 2021-12-13 | 2024-01-26 | 大连百傲化学股份有限公司 | Recycling treatment method of 1, 2-benzisothiazolin-3-one chlorination process wastewater |
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