Treatment method for recycling oxadiazon etherifying salt waste

A treatment method, the technology of oxadiazon ether, is applied in the field of waste salt slag reuse treatment, and can solve the problems of no effective and reasonable industrialized treatment method, difficult direct treatment, and high treatment cost, achieve significant social benefits, solve treatment problems, Simple to use effects

Active Publication Date: 2015-03-25
ANHUI KELIHUA CHEM
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0005] The waste salt slag contains a variety of inorganic substances and a variety of organic components. The treatment cost is high, the method is complicated, and i

Method used

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  • Treatment method for recycling oxadiazon etherifying salt waste

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Comparison scheme
Effect test

Embodiment 1

[0024] Take 300g of waste salt residue and add it to a 1000mL three-necked flask with electric stirring, then add 300g of water and 60g of toluene, stir for 30min to fully dissolve, pour the mixture into a 1000mL pear-shaped separating funnel and let it stand for 30min before layering , Separate the upper layer toluene extract, weighing 66.3g, for recycling, when the content of 2,4-dichloro-5-isopropoxynitrobenzene in the toluene extract reaches 30%, it will be used for the production of oxadiazone.

[0025] The separated lower aqueous solution was transferred to a 1000mL three-neck flask equipped with a thermometer, an electric stirring device and a dropping funnel, and hydrochloric acid was added dropwise to adjust the pH to 3.5. After stirring for 30 minutes to fully dissolve, the pH was re-measured to 3.5, and chlorine gas was passed. The outlet pressure of chlorine gas is controlled at 0.45 MPa ~ 0.5 MPa. When the chlorine distribution rate is 110%, the chlorine gas...

Embodiment 2

[0027] Take 300g of waste salt residue and add it to a 1000mL three-necked flask with electric stirring, then add 300g of water and 60g of toluene, stir for 30 minutes, pour the mixture into a 1000mL pear-shaped separating funnel and let it stand for 30min before layering. Separate the upper strata toluene extract, weigh 66.3g, and recycle, when the 2,4-dichloro-5-isopropoxynitrobenzene content in the toluene extract reaches 30%, it will be used for the production of oxadiazone.

[0028] The separated lower aqueous solution was transferred to a 1000mL three-neck flask equipped with a thermometer, an electric stirring device and a dropping funnel, and hydrochloric acid was added dropwise to adjust the pH to 2.5. After stirring for 30 minutes to fully dissolve, the pH was re-measured to 2.5, and chlorine gas was passed. The outlet pressure of chlorine gas is controlled at 0.45 MPa ~ 0.5 MPa. When the chlorine distribution rate is 130%, the chlorine flow is completed. At this ...

Embodiment 3

[0030] Take 300g of waste salt residue and add it to a 1000mL three-necked flask with electric stirring, then add 300g of water and 60g of toluene, stir for 30 minutes, pour the mixture into a 1000mL pear-shaped separating funnel and let it stand for 30min before layering. Separate the upper strata toluene extract, weigh 66.3g, and recycle, when the 2,4-dichloro-5-isopropoxynitrobenzene content in the toluene extract reaches 30%, it will be used for the production of oxadiazone.

[0031] The separated lower aqueous solution was transferred to a 1000mL three-necked flask equipped with a thermometer, an electric stirring device and a dropping funnel, and hydrochloric acid was added dropwise to adjust the pH to 3.0. After stirring for 30 minutes to fully dissolve, the pH was re-measured to 3.0, and chlorine gas was passed. The outlet pressure of chlorine gas is controlled at 0.45 MPa ~ 0.5 MPa. When the chlorine distribution rate is 120%, the chlorine flow is completed. At thi...

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Abstract

The invention discloses a treatment method for recycling oxadiazon etherifying salt waste. The treatment method is characterized by comprising the following treatment steps: adding water to dissolve salt waste; extracting with methylbenzene; preparing bromine employing an acid process; and concentrating and extracting KCl, so as to obtain industrial bromine and crude KCl products, wherein a methylbenzene extracting liquid containing 2,4-dichloro-5-nitro-isopropoxybenzene is used for producing oxadiazon. The problem in treatment of the oxadiazon etherifying salt waste is solved. The method is scientific, reasonable, simple to operate, significant in economic benefits and social benefits and suitable for application in industrial production.

Description

technical field [0001] The invention belongs to the technical field of waste salt slag reuse treatment, and relates to waste salt slag produced in the synthesis process of 2,4-dichloro-5-isopropoxynitrobenzene, an intermediate of oxadiazone, and recovering usable components. Achieving re-use of processing methods. Background technique [0002] 2,4-dichloro-5-isopropoxynitrobenzene is an important intermediate in the synthesis of oxadiazone, which is generally prepared from 2,4-dichloro-5-nitrophenol through etherification have to. Synthetic 2, the reaction formula of 4-dichloro-5-isopropoxynitrobenzene is as follows: [0003] [0004] The realization of this process will produce a large amount of waste salt slag. The composition of this kind of salt slag is complex. After analysis, the main components and the percentage of each component of the salt slag are roughly as follows: KBr 40-60%, KHCO 3 30-50%, K 2 CO 3 2~6%, 2,4-dichloro-5-isopropoxynitrobenzene 0.5~3%, ...

Claims

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Application Information

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IPC IPC(8): C07C205/37C07C201/16C01B7/09C01D3/04
Inventor 王春王多余刘改玲魏晓明朱海峰
Owner ANHUI KELIHUA CHEM
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