A kind of preparation method of synthetic dimethoxycarbonic acid bisphenol A diester catalyst

A technology of dimethoxycarbonate bisphenol and catalyst is applied in the field of preparation of catalyst for synthesizing dimethoxycarbonate bisphenol A diester, and can solve the problems of no inhibition of alkylation products, no catalytic activity, low catalytic activity and the like , to achieve the effect of solving difficult separation and improving selectivity

Active Publication Date: 2016-04-06
TIANJIN POLYTECHNIC UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0008] Studies have shown that pure layered cross-MFI molecular sieves have no catalytic activity; pure layered cross-H-MFI molecular sieves have very low catalytic activity and have no inhibitory effect on alkylation products.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0022] (1) Take 15gC 22 h 45 Add Br into the 192mL toluene and acetonitrile mixed solution in the beaker (the volume ratio of toluene and acetonitrile is 1:1), stir and dissolve, put it in a constant pressure dropping funnel, and set it aside. Add 24.8mL of N,N,N',N'-tetramethyl-1,6-hexanediamine into the three-necked flask. Reflux reaction at 82°C, slowly drop the liquid in the constant pressure dropping funnel, react for 10h, filter and dry to obtain C 22 h 45 N(CH 3 ) 2 (CH 2 ) 6 N(CH 3 ) 2 Br.

[0023] (2) Take 20gC 22 h 45 N(CH 3 ) 2 (CH 2 ) 6 N(CH 3 ) 2 Br, dissolved in 107mL acetonitrile solution, then take 10mL 6 h 13 Br was added to the three-necked flask respectively, refluxed at 82°C for 10 hours, filtered, and dried to obtain C 22 h 45 N(CH 3 ) 2 (CH 2 ) 6 N(CH 3 ) 2 C 6 h 13 Br 2 .

[0024] (3) First dissolve 4g NaOH in 56.25g water, then add 8.18gC 22 h 45 N(CH 3 ) 2 (CH 2 ) 6 N(CH 3 ) 2 C 6 h 13 Br 2 , heated and stirred...

Embodiment 2

[0031] Catalyst preparation method is the same as example 1, just changes the butane bromide in step (7) into benzyl chloride, prepares catalyst: MFI-TiO 2 -(CH 2 ) 3 -SnO-CH 2 -Ph.

[0032] 0.3gMFI-TiO 2 -(CH 2 ) 3 -SnO-CH 2 -Ph catalyst was added to a 50mL three-necked flask, weighed 5.7g of BPA and added to the three-necked flask, first raised the temperature to 160°C, then slowly added DMC dropwise, the system temperature was controlled at 160°C, the steam temperature was guaranteed not to exceed 90°C, reacted for 8 hours, filtered, That is, the polycarbonate intermediate dimethoxycarbonic bisphenol A diester was obtained, and the yield was 82%.

Embodiment 3

[0034] Catalyst preparation method is the same as embodiment 1, just changes the bromobutane in step (7) into bromocyclohexane, prepares catalyst: MFI-TiO 2 -(CH 2 ) 3 -SnO-C 6 h 12 .

[0035] 0.3gMFI-TiO 2 -(CH 2 ) 3 -SnO-C 6 h 12 Add the catalyst into a 50mL three-neck flask, weigh 5.7g of BPA and add it into the three-necked flask, first raise the temperature to 160°C, then slowly add DMC dropwise, control the system temperature at 160°C, ensure that the steam temperature does not exceed 90°C, react for 8 hours, and filter to obtain The polycarbonate intermediate dimethoxycarbonic acid bisphenol A diester, the yield is 86%.

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PUM

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Abstract

The invention discloses a preparation method for synthesizing a dimethoxy bisphenol A carbonate catalyst. According to the preparation method for the catalyst, layered cross MFI molecular sieves are converted into H-MFI molecular sieves, a transition metallic oxide is grafted into the H-MFI molecular sieves, and then organic stannic oxide is grafted to obtain the layered cross MFI molecular sieve inorganic-organic compound hybridization catalyst. The activation carbonyl groups of the inorganic transition metallic oxide grafted into the catalyst can improve electrophilic capacity of DMC, the activation phenolic hydroxyl groups of the grafted organic stannic oxide can improve the nucleophilic capacity of BPA, then the conversion rate of the BPA can be improved, a PC intermediate is selectively synthesized, and alkylation of the BPA can be effectively suppressed. The synthesized catalyst belongs to typical heterogeneous catalysts and is not soluble with a product, and therefore the problem that a homogeneous catalyst is difficult to separate from the product is solved by applying the synthesized heterogeneous catalyst to a synthetic reaction.

Description

technical field [0001] The invention belongs to a method for preparing a chemical synthesis catalyst, in particular to a method for preparing a catalyst for synthesizing bisphenol A diester of dimethoxycarbonate. Background technique [0002] Polycarbonate (PC) has the advantages of heat resistance, impact resistance, flame retardancy, transparency and excellent mechanical properties, so it is widely used in glass assembly industry, automobile industry and electronics, electrical industry, office equipment, medical care, film and protective equipment, etc. widely used. PC is the only product with good transparency among the five major engineering plastics, and it is also the general engineering plastic with the fastest growth rate in recent years. [0003] PC is mainly prepared by the phosgene method, but because it uses dichloromethane as a solvent and highly toxic phosgene reactants, it is seriously harmful to the environment and human beings. Therefore, it is urgent to c...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): B01J31/38B01J31/36C07C69/96C07C68/06
Inventor 李振环刘秀培苏坤梅程博闻何小龙
Owner TIANJIN POLYTECHNIC UNIV
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