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Process for producing 2- methyl group -3- phenylbenzene methanol cleanly

A technology of phenylbenzyl alcohol and clean production, applied in hydrolysis preparation, organic chemistry, etc., can solve problems such as difficult water purification, no application value, difficult separation by biochemical or physical and chemical methods, and achieve the effect of eliminating emissions

Active Publication Date: 2008-02-27
盐城市大丰区生产力促进中心
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The tetrahydrofuran solvent separated in the production process generally contains about 5% water, and it is difficult to remove water by general distillation methods, so the currently recovered tetrahydrofuran can only be used for other purposes and cannot be used in the system; the hydrolysis process wastewater in production Contains a large amount of magnesium chloride and magnesium bromide, and the mixed salt obtained by dehydration recovery is difficult to separate by biochemical or physical and chemical methods, forming pollutants with no application value

Method used

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  • Process for producing 2- methyl group -3- phenylbenzene methanol cleanly
  • Process for producing 2- methyl group -3- phenylbenzene methanol cleanly

Examples

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Embodiment Construction

[0034] The present invention is further illustrated below by way of examples.

[0035] (1) Add 1050Kg of tetrahydrofuran, 120Kg of magnesium powder, and 10Kg of ethyl bromide into the reaction kettle, and stir. After the reaction is triggered, add 2,6-dichlorotoluene dropwise under reflux to a total of 750Kg. After the Grignard reaction is completed, keep the temperature below 60°C for 2 hours , get the first grignard material, and transfer it to the header tank.

[0036] Add 750Kg of bromobenzene, 2.5kg of catalyst, and 40Kg of tetrahydrofuran into the coupling reaction kettle, stir, add the first Grignard material dropwise under reflux at 110-120°C, and drop it in 3-5 hours to obtain the coupling material, adjust it with hydrobromic acid To pH2-3, hydrolysis reaction, then gradually increase the temperature to 90-110°C, recover the distilled tetrahydrofuran, cool down the feed liquid, add 300Kg water, separate the water phase and the oil phase, separate the oil layer, wash w...

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Abstract

The invention relates to a cleaning production technique of 2-methyl-3-phenyl benzenemethanol, which comprises the following steps: using 2, 6-dichlorotoluene as raw material and tetrahydrofuran as dissolvent; reacting bromobenzene to be 2- methyl-3-chlorine biphenyl after one step Grignard reaction; reacting dimethyl formamide to produce 2-methyl-3- benzaldehyde through tow-step Grignard reaction after hydrolytic decomposition and using potassium borohydride to deacidize to be product; dewatering recycled tetrahydrofuran firstly with solid caustic soda then returning system to use after hydrolytic decomposition with ethyl magnesium bromide again. The invention utilizes chlorine to deal system waste water to make bromide ion convert bromine and to be bromobenzene, bromoethane and bromide hydracids arranging for coupling material, Grignard reaction initiator and hydrolytic decomposition acid respectively and dissociates magnesium chloride in the waste water to be industrial salt, which achieves cleaning production through recycling waste liquid and water reasonably to reduce producing cost.

Description

technical field [0001] The present invention relates to the production method of 2-methyl-3-phenylbenzyl alcohol containing 2-step Grignard reaction using 2,6-dichlorotoluene as raw material, especially relates to the synthesis of tetrahydrofuran solvent and waste water discharged from the production system clean production process. Background technique [0002] 2-Methyl-3-phenylbenzyl alcohol is mainly used in the production of the pesticide bifenthrin and as a raw material for the synthesis of other pharmaceutical products. [0003] Molecular formula: C 14 h 14 o [0004] Structural formula: [0005] [0006] 2-Methyl-3-phenylbenzyl alcohol is a white crystal with a special smell of alcohol, soluble in toluene, methanol, ethyl acetate, acetone and other organic solvents; insoluble in water; [0007] At present, there are two kinds of preparation methods of 2-methyl-3-phenylbenzyl alcohol: one is to use 2,6-dichlorotoluene as raw material, tetrahydrofuran as solvent...

Claims

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Application Information

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IPC IPC(8): C07C33/24C07C29/09
Inventor 杨茂生王菁
Owner 盐城市大丰区生产力促进中心
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