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Preparation process for improving phloroglucinol by membrane method

A technology for phloroglucinol and preparation process, which is applied in the preparation of organic compounds, chemical instruments and methods, and hydrocarbon production from halogen-containing organic compounds, etc., can solve the problems of long process, difficult disposal of waste salt, generation of by-products, etc. , to achieve the effect of simple reaction process, satisfying recycling and high relative efficiency

Pending Publication Date: 2020-11-13
HANGZHOU BLUETEC ENVIRONMENTAL TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] The purpose of the present invention is to overcome the defects in the prior art, solve the problems of lengthy process, generation of by-products and difficult disposal of waste salt in the preparation process of phloroglucinol, and provide an improved membrane method with economic and resource advantages The preparation technology of phloroglucinol

Method used

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  • Preparation process for improving phloroglucinol by membrane method
  • Preparation process for improving phloroglucinol by membrane method

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0040] Adopt method of the present invention to prepare phloroglucinol, concrete technological process is as follows:

[0041] S1. Select cumene, an inert solvent with a density lower than water, immiscible with water and capable of azeotroping, to dissolve the reaction substrate 2,6-dichlorophenol to obtain solution A. Mix solution A and potassium hydroxide solution at a molar ratio of 1:10, then add water, and finally add hydrochloric acid solution to acidify to prepare a mixed solution of phloroglucinol and potassium chloride.

[0042] S2. The mixed solution of phloroglucinol and potassium chloride is firstly pretreated by precision filtration with a 0.5 μm filter membrane to remove suspended solids and macromolecular phloroglucinol crystals. Then the filtered mixed solution is passed into an electrodialysis system to obtain crude phloroglucinol and potassium chloride solution respectively. During the electrodialysis process, water needs to be added to the dilute chamber r...

Embodiment 2

[0045] Adopt method of the present invention to prepare phloroglucinol, concrete technological process is as follows:

[0046] S1. Select cumene, an inert solvent with a density lower than water, immiscible with water and capable of azeotroping, to dissolve the reaction substrate 2,6-dichlorophenol to obtain solution A. Mix solution A and potassium hydroxide solution at a molar ratio of 1:10, then add water, and finally add hydrochloric acid solution to acidify to prepare a mixed solution of phloroglucinol and potassium chloride.

[0047] S2. The mixed solution of phloroglucinol and potassium chloride is pretreated by precision filtration with a filter membrane of 1 μm, so as to remove suspended solids and macromolecular phloroglucinol crystals. Then the filtered mixed solution is passed into an electrodialysis system to obtain crude phloroglucinol and potassium chloride solution respectively. During the electrodialysis process, water needs to be added to the dilute chamber r...

Embodiment 3

[0050] This embodiment is used as a comparative example of Example 1 to explore the effectiveness of two-step electrodialysis in the present invention. The specific practices of this embodiment are as follows:

[0051] S1. Select cumene, an inert solvent with a density lower than water, immiscible with water and capable of azeotroping, to dissolve the reaction substrate 2,6-dichlorophenol to obtain solution A. Mix solution A and potassium hydroxide solution at a molar ratio of 1:10, then add water, and finally add hydrochloric acid solution to acidify to prepare a mixed solution of phloroglucinol and potassium chloride.

[0052] S2. The mixed solution of phloroglucinol and potassium chloride is firstly pretreated by precision filtration with a 0.5 μm filter membrane to remove suspended solids and macromolecular phloroglucinol crystals. Then, the filtered mixed solution is separated by electrodialysis, and the operation process of the system and the difference of the obtained p...

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Abstract

The invention discloses a preparation process for improving phloroglucinol by a membrane method. The preparation process comprises the following steps: S1, dissolving 2,6-dichlorophenol or 2,4-dichlorophenol served as a reaction substrate in an inert solvent, adding a potassium hydroxide solution to eliminate dimolecular hydrogen chloride, carrying out addition with water to generate a phloroglucinol potassium salt solution, and acidifying the phloroglucinol potassium salt solution with a hydrochloric acid solution to obtain a mixed solution of phloroglucinol and potassium chloride; S2, filtering the mixed solution, and separating through an electrodialysis system to respectively obtain a phloroglucinol crude product and a potassium chloride solution; S3, introducing the potassium chloridesolution into a three-compartment bipolar membrane electrodialysis system to respectively obtain a potassium hydroxide solution and a hydrochloric acid solution; and respectively refluxing the potassium hydroxide solution and the hydrochloric acid solution into the potassium hydroxide solution and the hydrochloric acid solution in S1. The method has the advantages of simple operation, no generation of by-products and process wastewater, high realization of resource utilization, high automation degree, great reduction of the production cost, and good industrial application prospect.

Description

technical field [0001] The invention relates to the field of drug synthesis, in particular to a preparation process for improving phloroglucinol by a membrane method. Background technique [0002] Phloroglucinol (1,3,5-trihydroxybenzene) is an important organic synthesis intermediate and fine chemical product. Phloroglucinol injection is a smooth muscle antispasmodic drug, which is clinically used to treat digestive system and biliary tract Acute spastic pain caused by dysfunction, acute spastic urethra, bladder, renal colic and gynecological spastic pain, phloroglucinol will not produce a series of anticholinergic side effects, and will not cause hypotension, increased heart rate, heart rhythm Symptoms such as abnormalities have no effect on cardiovascular function; at the same time, it can be used for the synthesis of flavonoid isoflavone antineoplastic drugs. In addition, phloroglucinol can be used as raw materials such as dye coupling agent, tire tackifier and azo compo...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C39/10C07C37/00
CPCC07C37/00C07C1/30C07C39/10C07C15/04
Inventor 张笑维潘云辉张楠楠楼永通俞树新
Owner HANGZHOU BLUETEC ENVIRONMENTAL TECH
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