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Cleaner production process of 2‑cyano‑4′‑methylbiphenyl

A technology of methyl biphenyl and production process, which is applied in the purification/separation of carboxylic acid nitrile, magnesium chloride, magnesium halide, etc., which can solve the problems of high solvent recovery cost and inability to discharge waste water, and achieve resource utilization and reduce treatment costs , Improve the effect of recycling efficiency

Active Publication Date: 2017-02-01
ZHEJIANG APELOA JIAYUAN PHARMA +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0006] In the context of continuous expansion of production capacity and increasing pressure on environmental protection, conventional treatment methods face problems such as the inability to discharge waste water and the high cost of solvent recovery.

Method used

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  • Cleaner production process of 2‑cyano‑4′‑methylbiphenyl

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0024] (1) Preparation of crude magnesium chloride: 20Kg content of 30% p-methylphenylmagnesium chloride tetrahydrofuran solution is slowly added dropwise at 0~10°C to a mixture containing 5.5Kg o-chlorobenzonitrile, 50g anhydrous ferric chloride and 14.5Kg tetrahydrofuran The solution was incubated for 3 hours to obtain a Grignard coupling reaction solution. Slowly add 2Kg tap water dropwise to the reaction solution at 20-25°C (apply the reclaimed aqueous tetrahydrofuran and tap water in batches, and ensure that the total amount of water added is 2Kg). Kilograms of magnesium chloride crude product and 36Kg filtrate.

[0025] (2) Purification of crude magnesium chloride: add 3 kg of tap water and 300 g of concentrated hydrochloric acid to 6 kg of crude magnesium chloride, adjust the pH to 6-7, and heat up to 60-70°C to dissolve all the solids. 2Kg of toluene was added to carry out extraction and layering to obtain about 2.3Kg of toluene solution in the upper layer. Concentra...

Embodiment 2

[0030] (1) Preparation of crude magnesium chloride: 20Kg content of 30% p-methylphenylmagnesium chloride tetrahydrofuran solution is slowly added dropwise at 0~10°C to a mixture containing 5.5Kg o-chlorobenzonitrile, 50g anhydrous ferric chloride and 14.5Kg tetrahydrofuran The solution was incubated for 3 hours to obtain a Grignard coupling reaction solution. Slowly add 3Kg tap water dropwise to the reaction solution at 20~25°C (apply the reclaimed aqueous tetrahydrofuran and tap water in batches, and ensure that the total amount of water added is 3Kg). Kilograms of magnesium chloride crude product and 36Kg filtrate.

[0031] (2) Purification of crude magnesium chloride: add 2 kg of tap water and 300 g of concentrated hydrochloric acid to 7 kg of crude magnesium chloride, adjust the pH to 6-7, and heat up to 60-70°C to dissolve all the solids. 2Kg of toluene was added to carry out extraction and layering to obtain about 2.3Kg of toluene solution in the upper layer. Concentra...

Embodiment 3

[0036](1) Preparation of crude magnesium chloride: 20Kg content of 24.3% p-methylphenylmagnesium chloride tetrahydrofuran solution is slowly added dropwise to a mixture containing 4.5Kg o-chlorobenzonitrile, 40g anhydrous ferric chloride and 14.5Kg tetrahydrofuran at 0-10°C. The solution was incubated for 4 hours to obtain a Grignard coupling reaction solution. Slowly add 1.75Kg tap water dropwise to the reaction solution at 20-25°C (apply the recovered aqueous tetrahydrofuran and tap water in batches, and ensure that the total amount of water added is 1.75Kg). Obtained 4.8 kg of magnesium chloride crude product and 36Kg of filtrate.

[0037] (2) Purification of crude magnesium chloride: add 1.6 kg of tap water and 240 g of concentrated hydrochloric acid to 4.8 kg of crude magnesium chloride, adjust the pH to 6-7, and heat up to 60-70°C to dissolve all the solids. Add 1.6Kg of toluene to carry out extraction and stratification to obtain about 1.8Kg of upper layer toluene solu...

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Abstract

The invention discloses a clean production technology of 2-cyan-4'-methyl diphenyl. The production technology comprises the following steps: adding water or aqueous tetrahydrofuran to coupling reaction liquid, destroying complexing of tetrahydrofuran and magnesium chloride; forming magnesium chloride containing crystal water and separating out in a solid manner; removing magnesium chloride through a filtering method; and directly distilling filtered filtrate to recycle tetrahydrofuran. According to the production technology, zero release of the wastewater is achieved, the magnesium chloride is extracted as a byproduct, solid waste is avoided, the solvent recovery procedure is simplified, the recovery efficiency of the solvent is improved, and the recovery cost of the solvent is reduced. Due to these results, the competitiveness of the product is improved, and clean production and sustainable development of the 2-cyan-4'-methyl diphenyl product are achieved.

Description

technical field [0001] The invention relates to a new clean production process of Grignard coupling reaction, in particular to a new clean production process of 2-cyano-4'-methylbiphenyl, belonging to the field of organic synthesis. Background technique [0002] Grignard reagent is an important intermediate widely used in fine chemical industry, medicine, agriculture and other chemical fields. Among the types of reactions that Grignard reagents participate in in industrial production, the common nucleophilic addition reactions with compounds with electron-deficient centers such as aldehydes and ketones, and the coupling reactions with halogenated hydrocarbons under the action of catalysts. [0003] The Grignard reaction generally uses anhydrous tetrahydrofuran as the reaction solvent. In the post-treatment stage of the reaction, the operation of acidification, extraction and stratification is usually adopted, which produces a large amount of acidic wastewater containing hig...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C255/50C07C253/34C01F5/30
Inventor 庄程翰唐武期李晓黎叶素斌陈淑娟徐健周雄飞
Owner ZHEJIANG APELOA JIAYUAN PHARMA
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