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
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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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