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Method for catalytically synthesizing 4,4'-bischloromethylbiphenyl by using silicon dioxide-loaded phosphotungstic acid

A technology of dichloromethyl biphenyl and silicon dioxide is applied in chemical instruments and methods, physical/chemical process catalysts, organic chemistry, etc., and can solve the problems of complex reaction process, high production cost, hazardous raw material toxicity and the like, Achieve the effect of high catalytic activity, good stability and inhibition of side reactions

Active Publication Date: 2016-04-20
RIANLON
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Although the Chinese patent CN103708530 describes the method of producing zinc compounds from the wastewater discharged from the synthesis of biphenyl dichlorobenzyl, its production cost is still very high
[0005] Chinese patent CN104860792 invented the chlorination reaction between 4,4'-dimethylbiphenyl and chlorination reagent under the action of initiator and free radical scavenger. After the reaction is complete, the 4,4 '-dichloromethylbiphenyl, the chlorination reagent is trichloroisocyanuric acid, sulfonyl chloride, chlorine, etc., and the initiator is organic peroxide or azobisisobutyronitrile and azobis Isoheptanonitrile, the reaction process is more complicated, and the raw materials are more toxic and dangerous

Method used

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0020] The preparation process of the silica-supported phosphotungstic acid catalyst is as follows: add 60 g of phosphotungstic acid (CAS number: 12067-99-1) to 200 ml of distilled water, stir until it is completely dissolved, and add 20 g of ultrafine silica (3000 mesh). ), soaked for 48 hours at room temperature, then filtered, the filter cake was rinsed with distilled water, dried at 110-120 °C for 2 hours, and then calcined at 200 °C for activation for 3 hours to obtain a silica-supported phosphotungstic acid catalyst.

Embodiment 2

[0022] The preparation process of the silica-supported phosphotungstic acid catalyst is as follows: add 30 g of phosphotungstic acid (CAS number: 12067-99-1) to 200 ml of distilled water, stir until it is completely dissolved, add 60 g of ultrafine silica (1000 mesh ), soaked for 48 hours at room temperature, then filtered, the filter cake was rinsed with distilled water, dried at 110-120 °C for 2 hours, and then calcined at 200 °C for activation for 3 hours to obtain a silica-supported phosphotungstic acid catalyst.

Embodiment 3

[0024] The preparation process of the silica-supported phosphotungstic acid catalyst is as follows: add 50 g of phosphotungstic acid (CAS number: 12067-99-1) to 200 ml of distilled water, stir until it is completely dissolved, add 30 g of ultrafine silica (2000 mesh) ), soaked for 48 hours at room temperature, then filtered, the filter cake was rinsed with distilled water, dried at 110-120 °C for 2 hours, and then calcined at 200 °C for activation for 3 hours to obtain a silica-supported phosphotungstic acid catalyst.

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Abstract

The invention relates to a method for catalytically synthesizing 4,4'-bischloromethylbiphenyl by using silicon dioxide-loaded phosphotungstic acid, which comprises the steps: charging biphenyl, 30-37% hydrochloric acid and paraformaldehyde into a reactor according to a molar ratio of 1:(2-8):(3-4), adding the silicon dioxide-loaded phosphotungstic acid catalyst, then adding an organic solvent, heating to 50-80 DEG C, introducing HCl gas, reacting for 10-20h, and performing posttreatment and crude product recrystallization on the reaction solution to obtain a target product 4,4'-bischloromethylbiphenyl. The method has the advantages that the catalyst can be repeatedly used and regenerated and an acid phase is used indiscriminately, a conversion rate of the 4,4'-bischloromethylbiphenyl is obviously improved, a yield after refinement is 89%, content is 99% or above, emission of three wastes is reduced, clean and circulation production is realized and the method is an environment-friendly preparation method.

Description

technical field [0001] The invention relates to a method for the catalytic synthesis of 4,4'-dichloromethylbiphenyl supported by silica-supported phosphotungstic acid, and belongs to the technical field of chemical synthesis. Background technique [0002] 4,4'-Dichloromethylbiphenyl (English name 4,4'-bis(chloromethyl)biphenyl, referred to as BCMB), referred to as biphenyl dichlorobenzyl, is an important organic synthesis intermediate, is the synthesis of fluorescence enhancer. The key intermediate of whitening agent FP and stilbene biphenyl type fluorescent whitening agent CBS. Fluorescent whitening agent is widely used in the whitening of plastics, fibers, coatings, etc., and its whitening and brightening effects are very obvious; at the same time, it has excellent resistance to oxygen bleaching, chlorine bleaching, strong acid and alkali resistance and excellent perspiration fastness. Spend. Moreover, its whiteness is very stable, the loss during washing, dyeing and dry...

Claims

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Application Information

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IPC IPC(8): C07C17/32C07C22/04B01J27/188
CPCB01J27/188C07C17/32C07C22/04
Inventor 云会霞孙春光范小鹏汤翠祥李海平徐丁
Owner RIANLON