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Production method of m-bromophonol and production device thereof

A production method and m-bromophenol technology are applied in the production of m-bromophenol and the field of its production equipment, which can solve the problems of difficult operation, high equipment requirements, and low product yield, so as to avoid side reactions, shorten reaction time, The effect of reducing production costs

Active Publication Date: 2007-07-18
江西扬帆新材料有限公司 +1
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  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] The defect of existing preparation method is: what adopt is the method that diazonium salt is replaced by halogen, have used concentrated hydrobromic acid and cuprous bromide to react, not only operation difficulty is big, and equipment requirement is high, also will discharge a large amount of waste water, And the use of tank reactors is prone to side reactions, low product yields, and long reaction times

Method used

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  • Production method of m-bromophonol and production device thereof
  • Production method of m-bromophonol and production device thereof
  • Production method of m-bromophonol and production device thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0023] Embodiment 1: a kind of production method of m-bromophenol, carries out following steps successively:

[0024] 1), diazotization reaction: a typical method is as follows (Preparation of m-bromophenol, C.FrederickKoelsch, Journal of the American Chemical Society (1939), 61, 969): 10g m-bromoaniline is dissolved in boiling 300ml water and 50ml sulfuric acid solution, the mixture was cooled to 10°C and diazotized with 4.0 g of sodium nitrite. 300 ml of the obtained m-bromoaniline diazosulfate aqueous solution (containing 0.0578 mol of m-bromoaniline diazosulfate).

[0025] 2), hydrolysis reaction: after the above-mentioned m-bromoaniline diazosulfate aqueous solution passes through the flow pump 3, it enters the pipeline reactor 4 with a flow rate of 100ml / hr to carry out the hydrolysis reaction. The hydrolysis temperature is 120°C, and the residence time is 10 minutes.

[0026] 3), extraction (this is as a kind of prior art): the reaction liquid is all collected after p...

Embodiment 2

[0029] Embodiment 2: a kind of production method of m-bromophenol, carries out following steps successively:

[0030] 1), diazotization reaction: with embodiment 1.

[0031] 2), hydrolysis reaction: after the above-mentioned m-bromoaniline diazosulfate aqueous solution passes through the flow pump 3, it enters the pipeline reactor 4 with a flow rate of 60ml / hr to carry out the hydrolysis reaction. The hydrolysis temperature is 120°C, and the residence time is 15 minutes.

[0032] 3), extraction: 150ml of normal hexane is placed in the extract container 70, and the extraction time is 2 hours; all the other are the same as in Example 1.

[0033] 4), product refining: take the extracted organic phase and rectify under reduced pressure, vacuum degree 30mmHg, distill out n-hexane at 22-24°C, collect fractions at 138-140°C, detect purity 98.8% by chromatography, and obtain 8.7g m-bromine phenol.

Embodiment 3

[0034] Embodiment 3: a kind of production method of m-bromophenol, carries out following steps successively:

[0035] 1), diazotization reaction: with embodiment 1.

[0036] 2), hydrolysis reaction: after the above-mentioned m-bromoaniline diazosulfate aqueous solution passes through the flow pump 3, it enters the pipeline reactor 4 with a flow rate of 160ml / hr to carry out the hydrolysis reaction. The hydrolysis temperature is 70°C, and the residence time is 3 minutes.

[0037] 3), extraction: 150ml ether is placed in the extract container 70, and the extraction time is 2.5 hours; all the other are the same as in Example 1.

[0038]4), product refinement: get the diethyl ether phase vacuum rectification that has been extracted, vacuum tightness 30mmHg, collect 138~140 ℃ fraction, through chromatographic detection purity 99%, obtain 8.5g m-bromophenol.

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Abstract

This invention relates to a production methods of inter-Br-phenol. It includes diazotization reaction, also includes the following steps: 1. hydrolysis reaction: put the aqueous solution of inter-hypotyl heavy nitrogen sulfate that generate from diazotization in pipe reactor for hydrolysis; 2. Extraction: put the liquid generated form hydrolysis reaction into continuous extraction apparatus for extraction, until the water layer clarification; make the separation of the organic layer through vacuum distillation to obtain inter-Br-phenol. The invention also opens the device for the realization of the production: Liquid Storage Tank flow through the pump, then connect with temperature control device's pipeline reactor, outlet of pipeline reactor and continuous extraction unit Linked; Liquid Storage Tank with insulation kits.

Description

technical field [0001] The invention relates to a production method of m-bromophenol and a production device thereof. Background technique [0002] M-bromophenol is an organic synthesis intermediate, a raw material for pesticides and medicines, and can be used to synthesize m-bromoanisole; it is also the main intermediate for the synthesis of anticancer sedative analgesic drug trimidol, and can be used for other medicines , dyes and organic synthesis. The industrial synthesis method of m-bromophenol is generally to use m-aminophenol as raw material, in the presence of concentrated sulfuric acid, carry out diazotization reaction with sodium nitrite at 5°C to generate diazonium salt, and then react with bromine in hydrobromic acid It is obtained by reaction of cuprous chloride. which is: [0003] [0004] The defect of existing preparation method is: what adopt is the method that diazonium salt is replaced by halogen, have used concentrated hydrobromic acid and cuprous b...

Claims

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Application Information

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IPC IPC(8): C07C37/62C07C37/72C07C39/02
Inventor 樊培仁樊彬朱俊飞陈新志李银革刘伟
Owner 江西扬帆新材料有限公司
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