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Method for treating and recycling process waste water generated during production of 1,2-Benzisothiazolin-3-One

A technology for benzisothiazole and production process is applied in the field of treatment and resource utilization of 1,2-benzisothiazol-3-one production process wastewater, which can solve the problems of waste, high treatment cost and high energy consumption, and achieves the Achieving the effect of recycling waste

Inactive Publication Date: 2015-10-21
YANCHENG TEACHERS UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Each ton of product will produce 20~22m of waste water 3 , the wastewater is reddish brown, CODc r 23000-24000mg / L, of which 1,2-benzisothiazol-3-one content is 6100-6600mg / L, and sodium chloride content is 100-130g / L. Due to the high salt content in wastewater, now The treatment method is mainly to concentrate the process wastewater and treat it as hazardous solid waste, which not only costs a lot, but also wastes the expensive 1,2-benzisothiazol-3-one and sodium chloride; or use Ethyl acetate extraction method recovery, the recovery rate is only about 63%, and because ethyl acetate is volatile and has a certain solubility in water, so the consumption is relatively large, and the energy consumption is high, so there is no economical and effective treatment of the process wastewater. method

Method used

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  • Method for treating and recycling process waste water generated during production of 1,2-Benzisothiazolin-3-One

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0018] Pack 20mL of NDA150 resin with a dry weight of about 15g into two adsorption columns (Φ20×250mm) in the first adsorption column and the second adsorption column with insulation jackets.

[0019] Take 1000mL of reddish-brown 1,2-benzisothiazol-3-one production process wastewater and filter, add 0.5ml of 1% liquid caustic soda dropwise, and put the column liquid COD Cr 23420mg / L, 1,2-benzisothiazol-3-one content is 6240mg / L, at 35±5℃, 400ml upper column solution is passed through the NDA150 resin column at a flow rate of 40mL / h, and the primary effluent is yellow. The water output from the second adsorption column is light yellow, and the content of 1,2-benzisothiazol-3-one in the secondary adsorption water is 222.6mg / L, COD Cr Reduced to 1292mg / L, the water is distilled to recover 44.6g of crude sodium chloride salt after drying, and the effluent can reach the national first-class discharge standard after aerobic biochemical treatment.

[0020] The adsorbed NDA150 resin...

Embodiment 2

[0022] Pack 300mL of ZH124 resin with a dry weight of about 225g into two first and second adsorption columns (Φ35×500mm) with insulation jackets respectively.

[0023] Take 10L of reddish-brown 1,2-benzisothiazol-3-one production process wastewater and filter it, add 5ml of 1% liquid alkali dropwise, and put the column liquid COD Cr The content of 1,2-benzisothiazol-3-one is 6117mg / L. At 5±5℃, 6600ml of the upper column liquid is passed through the ZH124 resin column at a flow rate of 300mL / h, and the primary effluent is yellow. The water output from the second adsorption column is light yellow, and the content of 1,2-benzisothiazol-3-one in the secondary adsorption water is 116.8g / L, COD Cr Reduced to 1067mg / L, the water is distilled to recover 694.8g of crude sodium chloride salt after drying, and the effluent can reach the national first-level discharge standard after aerobic biochemical treatment.

[0024] The adsorbed ZH124 resin is desorbed and regenerated with 900mL o...

Embodiment 3

[0026] The adsorbents in Examples 1 and 2 in Examples 1 and 2 were changed to FZH11, ZH01, ZH33, JX101, CHA111 resins and American AmberLiteXAD-4, XAD-2, XAD-7 resins respectively, and other operating conditions remained unchanged , the results are basically the same except that the volume of each batch and the amount of recovery are changed.

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Abstract

The invention provides a method for treating and recycling process waste water generated during the production of 1,2-Benzisothiazolin-3-One. The production of 1,2-Benzisothiazolin-3-One is as follows: dithio-salicylic acid is used as a raw material and is subjected to acylating chlorination, chloro-substitution, distillation, alkaline hydrolysis using ammonia, bleaching, acidification and refining. The method for treating and recycling the process waste water includes the following steps: adjusting the pH of the process waste water to be about 8, carrying out two-level serially connected preferential adsorption on 1,2-Benzisothiazolin-3-One using ultra-high cross-linked polystyrene-divinylbenzene polymeric adsorbent bed layer, the effluent after the second level of adsorption is subjected to triple effect evaporation, a part of the distillation effluent returns to the original production process for being used indiscriminately, and another part of the distillation effluent is subjected to aerobic biological treatment, and the treated effluent can reach national first-level discharge standards; the residual after distillation is subjected to cooling, crystallization and centrifugation, and then crude sodium chloride is recycled; the polymeric adsorbent used dilute sodium hydroxide solution is regenerated through desorption; all levels of resins can be used repeatedly; the desorption solution can be directly applied to the bleaching process of the original production process; recycling of organic matters is realized while the waste water is treated by using the method.

Description

technical field [0001] The present invention relates to the treatment and treatment of process wastewater produced by obtaining 1,2-benzisothiazol-3-one from dithiodibenzoic acid as a raw material through acid chlorination, chlorination, distillation, aqueous ammonia alkali hydrolysis, decolorization, and acidification. Resource method. Background technique [0002] 1,2-Benzisothiazol-3-one is also called 1,2-benzisothiazolin-3-one. The synthetic route applicable to this method is to use dithiodibenzoic acid as a raw material to obtain 1,2-benzisothiazole-3 - Ketone sodium salt, after being decolorized by activated carbon, acidified and refined with hydrochloric acid to obtain 1,2-benzisothiazol-3-one, the main principle is as follows: [0003] [0004] Using the above production process, one stream of waste water will be produced after acidification with hydrochloric acid and centrifugation, and another stream of waste water will be produced after washing with water. B...

Claims

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Application Information

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IPC IPC(8): C02F9/10C02F103/36
Inventor 费正皓李万鑫柯长忠施卫忠李振兴邢蓉刘总堂方洁杨珊珊
Owner YANCHENG TEACHERS UNIV
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