Method for re-extracting materials from wastewater of pyridine salt alcoholization section
A pyridinium salt and waste water technology, applied in chemical instruments and methods, water/sewage multi-stage treatment, heating water/sewage treatment, etc., can solve the problems of material waste, no material analysis and extraction, etc., to achieve a simple process, easy for employees Simple operation and processing method
Inactive Publication Date: 2019-04-02
ANHUI JINGHE IND
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Problems solved by technology
Due to the lack of in-depth research and scientific analysis, the wastewater generated in this section has been directly sent to the sewage station for treatment, and the dissolved materials in the wastewater have not been further analyzed and extracted, resulting in a small part of the dissolved materials in the wastewater. Discharged with waste water, resulting in waste of materials
Method used
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Experimental program
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Effect test
Embodiment Construction
[0018] 1) The alcohol chemical section uses 700KG of 4-chloro-3-methoxy-2-methylpyridine-N-oxide produced in the previous section, and 2.8T methanol and 325KG solid sodium hydroxide at 68-72°C for 6 hours to produce Alcoholation reaction generates 3,4-dimethyl-2-methylpyridine-N-oxide, and then recovers excess methanol through filtration and decompression, and then adds 1.5 m³ of water; adds 2.4 m³ of dichloromethane in three times Methane is extracted and separated, and the separated dichloromethane extract is sent to the extract storage tank, and about 2 m³ of the generated waste water is sent to the waste water decompression recovery kettle.
[0019] 2) Turn on the vacuum pump to bring negative pressure (0.09~0.1MP) to the decompression recovery kettle, open the steam valve to heat the decompression recovery kettle to steam out excess water in the kettle, control the temperature during the whole distillation process to 70-80°C, and the distilled water enters Water storage t...
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The invention discloses a method for re-extracting materials from wastewater of an alcoholization section of pyridine salt production. The method comprises the following steps: 1) carrying out a qualified alcoholization reaction, then adding wastewater generated after reduced-pressure recovery of methanol and wastewater generated after extraction separation are completely into a reduced-pressure recovery kettle at one time; 2) heating the reduced-pressure recovery kettle to distill out residual water in the kettle under a negative pressure state, wherein the temperature in the whole distillingprocess is controlled to be 70-80 DEG C, and the distilled water enters a water storage tank; 3) adjusting the pH value of the wastewater in the reduced-pressure recovery kettle to be 9, filtering out waste salt in the system through a filter press, and feeding the filtrate into an extraction layering kettle; and 4) adding dichloromethane into the extraction layering kettle for extraction and separation, so as to obtain the product of the section in the wastewater, and feeding the product into a next section. According to the method disclosed by the invention, materials dissolved in the wastewater can be separated and extracted again, so that the yield of the section can be greatly improved, and the overall yield is improved by 5% compared with the yield in the prior art.
Description
technical field [0001] The invention relates to a method for re-extracting materials from waste water in the alcohol chemical industry section of raw material pyridine hydrochloride. Background technique [0002] Pyridine hydrochloride is the raw material for the production of stomach medicine pantoprazole, and its full name is 2-chloromethyl-3,4-dimethoxypyridine hydrochloride. [0003] For the production of pyridine hydrochloride, manufacturers at home and abroad mainly use methyl maltol through methyl esterification, ammoniation, chlorination, oxidation, alcoholization, anhydrideization and salt refining. The production process is methyl maltol through Dimethyl sulfate, after esterification, ammoniation with ammonia water, then add phosphorus oxychloride for chlorination, then add hydrogen peroxide dropwise for oxidation, add methanol for alcoholization, add acetic anhydride for oxidation, add thionyl chloride to form a salt, and then add absolute ethanol Refined finishe...
Claims
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IPC IPC(8): C02F9/10
CPCC02F1/001C02F1/04C02F1/26C02F9/00
Inventor 耿庆保陈永旭
Owner ANHUI JINGHE IND