Purification process of 1,2-benzisothiazolin-3-ketone
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A benzisothiazoline and process technology, which is applied in the field of 1,2-benzisothiazoline-3-one purification technology, can solve the problems of allergy, easy drift, low yield and the like of staff, and achieves less allergic, The effect of not easy to drift and high yield
Active Publication Date: 2016-07-27
DAFENG YUELONG CHEM
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Problems solved by technology
[0002] In the prior art, 1,2-benzisothiazolin-3-one is mostly purified by acid-base purification, which will produce a large amount of high-salt wastewater; a mixed system of protic alcohol and water is used for recrystallization , the yield will be low due to the high solubility of the product in the system, not only that, but also the recovery of mixed solvents cannot be industrialized; using activated carbon for decolorization, not only the site is messy, but also a large amount of product is adsorbed in the filtered activated carbon , an average of 2-3kg of products can be adsorbed per kilogram of activated carbon, resulting in a large amount of solid waste
More importantly, the products produced by the prior art are in the form of powder, which is easy to drift and cause allergies to the staff
Method used
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Embodiment 1
[0045]Mix 100g of 1,2-benzisothiazolin-3-one with 297g of butyl acetate, 3g of N,N-dimethylformamide, and 0.5g of nickel chloride, then raise the temperature to 110°C, keep it warm for 2 hours, then cool down to 80°C ℃, filter, the filtrate is stirred and crystallized, the stirring speed is controlled at 20 rpm, the temperature is lowered to 0-5 ℃, 1,2-benzisothiazolin-3-one crystals are precipitated, filtered, washed with water, and dried to obtain 97.8gBIT, content 99.7%, yield 97.8%.
Embodiment 2
[0047] Mix 100g of 1,2-benzisothiazolin-3-one with 280g of xylene, 20g of N,N-diethylbenzamide, and 1.5g of copper nitrate, then heat it up to 120°C, keep it warm for 2 hours, then cool it down to 90°C , filtered, the filtrate was stirred and crystallized, the stirring speed was controlled at 20 rpm, the temperature was lowered to 0-5°C, 1,2-benzisothiazolin-3-one crystals were precipitated, filtered, washed with water, and dried to obtain 97.0g BIT with a content of 99.7 %, yield 97.0%.
Embodiment 3
[0049] Mix 100g of 1,2-benzisothiazolin-3-one with 290g of chlorobenzene, 10g of N-methylpyrrolidone, and 1g of zinc nitrate, then heat up to 120°C, keep warm for 2 hours, cool down to 85°C, filter, and the filtrate is stirred and crystallized , the stirring speed was controlled at 20 rpm, and the temperature was lowered to 0-5°C to precipitate 1,2-benzisothiazolin-3-one crystals, filtered, washed with water, and dried to obtain 96.8g of BIT, with a content of 99.8% and a yield of 96.8% .
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Abstract
The invention discloses a purification process of 1,2-benzisothiazolin-3-ketone. The method comprises the following steps of (1) mixing a coarse product of 1,2-benzisothiazolin-3-ketone, an aprotic solvent, an auxiliary reaction type solvent and solid metal salt; then, raising the temperature to 60 to 120 DEG C; performing heat insulation for 2 hours to form a mixed solution with solid undissolved substance impurities; (2) controlling the temperature of the mixed solution; filtering the solid undissolved substance impurities, and remaining filter liquid; (3) lowering the temperature of the filter liquid to 10 DEG C to 20 DEG C to form materials with crystals; (4) performing centrifugal filtration on the materials to obtain flaky 1,2-benzisothiazolin-3-ketone crystals; performing vacuum drying to obtain the 1,2-benzisothiazolin-3-ketone product. The method has the advantages that the product obtained through crystallization is in flaky and colorless solid with metal luster; the specific gravity is great; drifting cannot easily occur; operators cannot easily generate allergy.
Description
technical field [0001] The invention relates to a 1,2-benzisothiazolin-3-one purification process. Background technique [0002] In the prior art, 1,2-benzisothiazolin-3-one is mostly purified by acid-base purification, which will produce a large amount of high-salt wastewater; a mixed system of protic alcohol and water is used for recrystallization , the yield will be low due to the high solubility of the product in the system, not only that, but also the recovery of mixed solvents cannot be industrialized; using activated carbon for decolorization, not only the site is messy, but also a large amount of product is adsorbed in the filtered activated carbon , On average, every kilogram of activated carbon can adsorb 2-3kg of products, resulting in a large amount of solid waste. What's more, the products produced by the prior art are in the form of powder, which is very easy to drift and cause allergies to the staff. Contents of the invention [0003] The purpose of the pr...
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