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Method for recovering phenyltrimethylammonium tribromide from phenyltrimethylammonium tribromide centrifugal mother liquor

A technology of phenyltrimethylammonium tribromide and centrifugal mother liquor, which is applied in the fields of medicine and chemical industry, can solve the problems of unfavorable environmental protection enterprise sustainable development, reduced utilization rate of raw materials, increased difficulty in waste water treatment, etc. The effect of sustainable development

Pending Publication Date: 2022-06-07
江苏八巨药业有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0007] When D,L-naproxen is brominated, phenyltrimethylammonium tribromide is used as bromination reagent for bromination reaction, but in the synthesis process of phenyltrimethylammonium tribromide, phenyltrimethylammonium tribromide is used Methyl ammonium bromide, hydrobromic acid, and hydrogen peroxide are used as raw materials. Due to the incomplete reaction of phenyltrimethylammonium bromide, there is a large amount of phenyltrimethylammonium bromide in the centrifugal mother liquor of phenyltrimethylammonium tribromide. Ammonium chloride and hydrobromic acid increase the difficulty of wastewater treatment, reduce the utilization rate of raw materials, waste useful resources, and are not conducive to environmental protection and sustainable development of enterprises

Method used

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  • Method for recovering phenyltrimethylammonium tribromide from phenyltrimethylammonium tribromide centrifugal mother liquor

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0016] Embodiment 1 Preparation of centrifugal mother liquor of phenyltrimethylammonium tribromide

[0017] In a clean and dry 1000mL three-necked flask, put 129.6g of phenyltrimethylammonium bromide, 220g of hydrobromic acid with a mass concentration of 48%, 420g of water, 36g of 98% concentrated sulfuric acid, start stirring, and slowly dropwise add 90g 27.5% After the hydrogen peroxide was added dropwise, the reaction was continued for 1 hour, and orange-yellow crystals were gradually formed. After standing for 1 hour, centrifugation was performed to obtain the centrifugal mother liquor of phenyltrimethylammonium tribromide and phenyltrimethylammonium tribromide. The weight of phenyltrimethylammonium tribromide is 205.2g, the content is 99.2%, and the yield is 91%; the weight of the centrifugal mother liquor of phenyltrimethylammonium tribromide is 645g, and the content of phenyltrimethylammonium bromide in the mother liquor is 1.75%.

Embodiment 2

[0018] Embodiment 2 reclaims phenyl trimethyl ammonium tribromide

[0019] Take 215 g of the centrifugal mother liquor of phenyltrimethyl ammonium tribromide in Example 1, add 4 g of activated carbon, stir and decolorize for 1 hour, and filter to obtain the decolorized phenyltrimethylammonium tribromide centrifugal mother liquor.

[0020] The centrifugal mother liquor decolorization solution of phenyltrimethylammonium tribromide was cooled to 10°C, and 17 g of sodium hypochlorite solution with a mass concentration of 10% was slowly added dropwise. After the dropwise addition, the oxidation reaction and the perbromination reaction were continued for 2 hours. Crystals gradually formed, and the amount of orange-yellow crystals no longer increased, that is, the reaction was complete. After standing for 1 hour, filter to obtain 6.17 g of phenyltrimethylammonium tribromide with a content of 99%.

Embodiment 3

[0021] Embodiment 3 reclaims phenyl trimethyl ammonium tribromide

[0022] Take 215 g of the centrifugal mother liquor of phenyltrimethyl ammonium tribromide in Example 1, add 4 g of activated carbon, stir and decolorize for 1 hour, and filter to obtain the decolorized phenyltrimethylammonium tribromide centrifugal mother liquor.

[0023] The centrifugal mother liquor decolorization solution of phenyltrimethylammonium tribromide was obtained and cooled to 10° C., and 8 g of sodium chlorate solution with a mass concentration of 10% was slowly added dropwise, and the oxidation reaction and the perbromination reaction were continued for 2 hours after the dropwise addition. Orange-yellow crystals were gradually formed, and the reaction was complete if the amount of orange-yellow crystals no longer increased. After standing for 1 hour, filtration was performed to obtain 6.05 g of phenyltrimethylammonium tribromide with a content of 99.2%.

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Abstract

In the prior art, when phenyltrimethylammonium bromide, hydrobromic acid and hydrogen peroxide are used as raw materials to synthesize phenyltrimethylammonium bromide, because the reaction of phenyltrimethylammonium bromide is incomplete, a large amount of phenyltrimethylammonium bromide and hydrobromic acid exist in the centrifugal mother liquor of phenyltrimethylammonium tribromide, so that the wastewater treatment difficulty is increased, and the reaction time is shortened. In order to solve the technical problems in the prior art that the concentration of phenyltrimethylammonium tribromide is reduced, the utilization rate of raw materials is reduced, useful resources are wasted, and environmental protection and sustainable development of enterprises are not facilitated, the invention provides the method for recovering phenyltrimethylammonium tribromide from the phenyltrimethylammonium tribromide centrifugal mother liquor, which comprises the following steps: adding activated carbon into the phenyltrimethylammonium tribromide centrifugal mother liquor for decoloration; dropwise adding a strong oxidant into the decolorized phenyltrimethylammonium tribromide centrifugal mother liquor, continuously reacting until the reaction is complete after dropwise adding, standing and filtering to obtain phenyltrimethylammonium tribromide. The problem of difficulty in wastewater treatment is solved, and phenyltrimethylammonium bromide in the centrifugal mother liquor is recycled.

Description

technical field [0001] The invention belongs to the technical field of medicine and chemical industry, and particularly relates to a method for recovering phenyltrimethylammonium tribromide from centrifugal mother liquor of phenyltrimethylammonium tribromide. Background technique [0002] Chemical name: Phenyltrimethylammonium tribromide, referred to as PTT, English name Phenyltrimethylammoniumtribromide, the structural formula is as follows. [0003] [0004] It is an important raw material for naproxen drugs. [0005] Because naproxen is an antipyretic, anti-inflammatory and analgesic drug, its anti-inflammatory, antipyretic and analgesic effects are good, and the adverse reactions are small. It has been widely used in the world and has become one of the world's major antipyretic analgesics and one of the best-selling over-the-counter drugs. [0006] At present, the industrial synthesis process of D,L-naproxen generally takes propionyl naphthoyl ether as the starting ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C209/84C07C211/64
CPCC07C209/84C07C211/64
Inventor 程焕达张进福晏显兵张岱任敏刘振益
Owner 江苏八巨药业有限公司