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Method for recovering methoxyamine from furan ammonium salt wastewater

A technology of furan ammonium salt and methoxyamine, applied in the field of medicine and chemical industry, can solve the problems such as difficulty in recycling and separation, and achieve the effects of high recovery rate, reduction of distillation waste residue, and reduction of production cost.

Active Publication Date: 2019-07-12
SHANDONG JINCHENG PHARMACCUTICAL CHEM CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The current production process of furan ammonium salt is mainly to obtain furanone acid by oxidation of 2-acetylfuran as raw material. Furanone acid and methoxyamine react in aqueous solution, and the ammonium furan salt is obtained through extraction into salt. During the production process, there will be A large amount of waste water contains 300-350kg of sodium chloride, 50-52kg of methoxyamine hydrochloride, and 90-95kg of phosphoric acid per ton of waste water, and its pH value is less than or equal to 0.5. The traditional process is neutralized by liquid caustic soda and distilled. Wastewater, finally get a mixture of sodium chloride, sodium phosphate and methoxyamine hydrochloride, the mixture is difficult to separate, so it is difficult to realize the recycling of each substance

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0036] A kind of furyl ammonium salt waste water: contain 320kg sodium chloride in 1 ton of waste water, 50kg methoxylamine hydrochloride, 90kg phosphoric acid, its pH value<0.5; The method for reclaiming methoxylamine from furyl ammonium salt waste water, step is as follows:

[0037] (1) Slowly add 5kg of calcium carbonate to the reaction kettle equipped with 100kg ammonium furan salt waste water, then add dropwise liquid caustic soda to adjust pH to 3.0, stir 1.5h, obtain calcium hydrogen phosphate salt emulsion;

[0038] (2) Control the temperature at 42 ± 3° C., stirring speed 150 rpm, slowly add 0.4 kg mass fraction of 5% flocculant polyacrylamide aqueous solution to carry out flocculation and sedimentation in the calcium hydrogen phosphate salt emulsion obtained in step (1), It took 15 minutes to complete the addition, stirred for 15 minutes, filtered and washed with water to obtain a solid calcium hydrogen phosphate salt, dissolved the solid calcium hydrogen phosphate sa...

Embodiment 2

[0042]A kind of furyl ammonium salt waste water: contain 300kg sodium chloride in 1 ton of waste water, 52kg methoxylamine hydrochloride, 95kg phosphoric acid, its pH value<0.5; The method for reclaiming methoxylamine from furyl ammonium salt waste water, step is as follows:

[0043] (1) Slowly add 6kg of calcium carbonate to the reaction kettle equipped with 100kg ammonium furan salt waste water, then add dropwise liquid caustic soda to adjust pH to 3.5, stir 1h, obtain calcium hydrogen phosphate salt emulsion;

[0044] (2) Control temperature 44 ± 3 ℃, stirring speed 180rpm, in step (1) obtained calcium hydrogen phosphate salt emulsion, slowly add 0.5kg mass fraction is the flocculant polyacrylamide aqueous solution of 10% to carry out flocculation and sedimentation, with time After 18 minutes of adding, stir for 12 minutes, filter and wash to obtain calcium hydrogen phosphate solid, dissolve the calcium hydrogen phosphate solid with 30% sulfuric acid solution to adjust pH to...

Embodiment 3

[0048] A kind of furyl ammonium salt waste water: contain 320kg sodium chloride in 1 ton of waste water, 50kg methoxylamine hydrochloride, 90kg phosphoric acid, its pH value<0.5; The method for reclaiming methoxylamine from furyl ammonium salt waste water, step is as follows:

[0049] (1) Slowly add 6 kg of calcium carbonate to the reaction kettle equipped with 100 kg of ammonium furan salt waste water, then add dropwise liquid caustic soda to adjust the pH to 3.2, stir for 1.2 h, and obtain calcium phosphate salt emulsion;

[0050] (2) Control the temperature at 42±3°C and the stirring speed at 120rpm, and slowly add 0.4kg of 10% flocculant polyacrylamide aqueous solution to the calcium phosphate emulsion obtained in step (1) for flocculation and sedimentation, which takes 12 minutes After the addition is complete, stir for 18 minutes, filter and wash with water to obtain a calcium phosphate solid, dissolve the calcium phosphate solid with a sulfuric acid solution with a mass ...

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Abstract

The invention belongs to the technical field of medical chemical industry, and particularly relates to a method for recovering methoxyamine from furan ammonium salt wastewater. The method comprises the following steps of: adding calcium carbonate into the furan ammonium salt wastewater, and regulating pH to 3.0-3.5 to obtain calcium hydrogen phosphate salt emulsion; adding a flocculant into the obtained calcium hydrogen phosphate salt emulsion for flocculation sedimentation; filtering to obtain calcium hydrogen phosphate salt solid and filtrate; concentrating the filtrate under reduced pressure to evaporate water; filtering to remove precipitated sodium chloride to obtain the filtrate; regulating the pH of the filtrate to 12-14; raising the temperature; introducing nitrogen into the filtrate; carrying out nitrogen purge distillation; and receiving steam carried by the nitrogen to obtain a methoxamine aqueous solution. By the adoption of the method for recovering the methoxyamine from the furan ammonium salt wastewater, three salts in the furan ammonium salt wastewater can be effectively separated, recycling of three raw materials of methoxyamine, phosphoric acid and sodium chloridefor producing the furan ammonium salt is achieved, production cost of the furan ammonium salt is further reduced, distillation waste residue is reduced and economic benefit is improved.

Description

technical field [0001] The invention belongs to the technical field of medicine and chemical industry, and in particular relates to a method for recovering methoxyamine from furan ammonium salt wastewater. Background technique [0002] Methoxyamine is an important chemical raw material for the production of antibiotics such as cefuroxime acid (ester) and phenoxystrobin fungicides; methoxyamine is also a kind of drug, which is often used in surgery to maintain or restore arteries Pressure, especially suitable for the reduction of blood pressure caused by spinal anesthesia. [0003] Furan ammonium salt is an important intermediate for preparing cefuroxime acid (ester), and methoxyamine is a key intermediate for preparing furan ammonium salt. The current production process of furan ammonium salt is mainly to obtain furanone acid by oxidation of 2-acetylfuran as raw material. Furanone acid and methoxyamine react in aqueous solution, and the ammonium furan salt is obtained throu...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C239/20
CPCC07C239/20
Inventor 付凯蔡会敏阴华栋张希诚侯乐伟翟琦磊时泽来
Owner SHANDONG JINCHENG PHARMACCUTICAL CHEM CO LTD
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