Solid waste reutilization technique in BIT (1,2-benzoisothiazolyl-3-one) production

A process and solid technology, applied in the field of solid waste recycling process in BIT production, can solve the problems of affecting economic effects, backward technical level, high cost, increase economic benefits, solve the problem of three wastes, and realize the effect of reuse

Inactive Publication Date: 2015-11-11
DAFENG YUELONG CHEM
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0006] 1,2-Benzisothiazol-3-one (BIT) is a new type of anti-mold, anti-corrosion and anti-bacterial material. The current technical level of its synthesis research is still relatively backward, which is mainly reflected in the high production cost and low reaction conversion rate in the preparation process. Low, the quality and purity of the product are not high enough, which directly affects the economic effect
Currently, for the waste liquid after the reaction, only the solvent inside is distilled and recycled for reuse. For every ton of product produced, 150 kg of waste residue will be produced after recycling the solvent
However, in the prior art, the waste residue generated after solvent recovery can only be treated as solid waste, and the waste residue will undoubtedly cause a certain degree of pollution to the environment during the solid waste treatment process.
Waste residue is a mixture of several by-products produced in the BIT production process. If you want to separate them one by one, it is not only technically difficult, but also expensive. For enterprises, the input and output are negative and have no actual economic value. , therefore, the prior art lacks a treatment plan for having a variety of solid by-products

Method used

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  • Solid waste reutilization technique in BIT (1,2-benzoisothiazolyl-3-one) production

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0027] Mix 150kg of waste with 300kg of solvent chlorobenzene, dissolve completely, add 99kg of solid light at 40°C while keeping warm, there is no obvious heat release, and the gas is continuously released. The reaction is detected by HPLC, and the active ingredient content in the mixture is less than 0.5%. The temperature was raised to 60°C, 64Kg of ammonium chloride was added, and the temperature was raised to reflux. After the reaction is complete, add 10Kg of water, feed chlorine gas, analyze and monitor with HPLC during the process, the raw material disappears, raise the temperature to 80°C, filter the solid, distill the filtrate to recover the solvent, dissolve the solid with liquid alkali, adjust the pH to 12, the solid is completely dissolved, add Stir the activated carbon, filter the activated carbon, add hydrochloric acid to the filtrate to adjust PH=5, precipitate solids, cool to 20°C, filter to obtain 114Kg solids, and the yield reaches 95% (based on the effective...

Embodiment 2

[0029] Mix 150Kg of waste with 450Kg of solvent toluene, dissolve completely, add 125Kg of thionyl chloride at 30°C, no obvious heat release, and continuous release of gas. The reaction is detected by HPLC, and the active ingredient content in the mixture is less than 0.5%. The temperature was raised to 50°C, and 127Kg of 20% ammonia water was added until the pH=9. Introduce chlorine gas, analyze and monitor with HPLC during the process, the raw material disappears, raise the temperature to 70°C, filter the solid, distill the filtrate to recover the solvent, dissolve the solid with liquid caustic soda, adjust the pH to 11-12, and dissolve all the solid, add activated carbon and stir, filter the activated carbon solid , the filtrate was added hydrochloric acid to adjust PH=4, and the solid was precipitated, cooled to 20° C., filtered to obtain 114Kg solid, and the yield reached 95% (based on the effective content in solid waste).

Embodiment 3

[0031] Mix 150Kg of waste with 300Kg of solvent chlorobenzene, dissolve completely, add 125Kg of thionyl chloride at 20°C, no obvious exotherm is seen, and the gas is continuously released. The reaction is detected by HPLC, and the active ingredient content in the mixture is less than 0.5%. The temperature was raised to 80°C, and ammonia gas was introduced until PH=9. Add 40Kg of water, feed chlorine gas, analyze and monitor with HPLC during the process, the raw materials disappear, raise the temperature to 80°C, filter the solid, distill the filtrate to recover the solvent, dissolve the solid with liquid caustic soda, adjust the pH to 10, dissolve all the solid, add activated carbon to stir, filter Activated carbon was solid, and hydrochloric acid was added to the filtrate to adjust PH=3, and the solid was precipitated, cooled to 10° C., filtered to obtain 114Kg solid, and the yield reached 95% (based on the effective content in solid waste).

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Abstract

The invention discloses a solid waste reutilization technique in BIT (1,2-benzoisothiazolyl-3-one) production, which comprises the following steps: mixing solid waste in BIT product with a solvent, and adding an acylation reagent while keeping the temperature at 0-60 DEG C to continuously release gas; while keeping the temperature at 20-30 DEG C, adding ammonia gas, ammonia water or ammonium chloride until the pH value is 9, and keeping the temperature at 30-80 DEG C for 3 hours; and adding water, introducing chlorine gas, heating to 50-90 DEG C, filtering out the solid, distilling the filtrate to recover the solvent, dissolving the solid in alkali, adding activated carbon for decolorization, filtering, regulating the pH value to 2-5 with hydrochloric acid, precipitating the solid, and centrifuging to obtain the solid. The technique analyzes the variety of byproducts in the solid residue and the specific chemical structure of each coproduct after the final solvent recovery in the existing BIT production technique, calculates the main components in all the byproducts, and provides a synthesis route according to the main components.

Description

technical field [0001] The invention belongs to the technical field of chemical industry, and more specifically, the invention relates to a solid waste recycling process in BIT production. Background technique [0002] 1,2-benzisothiazol-3-one (BIT) product appearance is light yellow crystal, molecular formula is: [0003] [0004] At present, it is divided into two categories: qualified products and refined products, the content of qualified products is 98.5%, and the content of refined products is more than 99%. The growth in the medium has a prominent effect, and it solves a series of problems such as mold, fermentation, deterioration, demulsification, and odor of organic products caused by the growth of microorganisms. And the toxicity is very small, it will not cause cancer and mutation, and basically has no harm to the human body. It is a green and environmentally friendly product, mainly used for anti-mildew of high-grade paints and coatings, and sterilization of ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D275/04
CPCC07D275/04
Inventor 江以桦李艳军陶友善
Owner DAFENG YUELONG CHEM
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