Реакция #975741

Уравнение реакции

Phosgene

guaiacol BPA

BPA

p-cumylphenol

sodium gluconate

→

4-(2-(4-hydroxyphenyl)propan-2-yl)-2-methoxyphenol

Растворители

triethylamine

water

Methylene chloride

Условия реакции

Обработка

1. 1
   Другоеequipped with mechanical agitation, condenser, and caustic scrubber vent system
2. 2
   workup.ADDITIONwas added at a rate
3. 3
   Температураto maintain pH=10
4. 4
   ДругоеThe reactor contents were purged with nitrogen
5. 5
   Другоеto remove the brine layer
6. 6
   workup.ADDITIONThe organic layer containing the polymer
7. 7
   Промывкаwas washed on a centrifuge train with 1N HCl
8. 8
   ДругоеThe polymer was isolated by steam precipitation
9. 9
   Другоеby drying under hot nitrogen

Методика

Run 3—1% guaiacol BPA: Methylene chloride (23 L), water (8 L), BPA (4500 g, 19.8 mol), monomethoxyBPA (55 g of the above mixture), p-cumylphenol (135 g, 0.64 mol), triethylamine (40 ml) and sodium gluconate (10 g) was charged to a 75 L reactor equipped with mechanical agitation, condenser, and caustic scrubber vent system. Phosgene (2300 g, 23.2 mol) was added at a rate of 80 g/min to the reactor while 33 wt % caustic was added at a rate to maintain pH=10. The reactor contents were purged with nitrogen then transferred to another tank and centrifuged to remove the brine layer. The organic layer containing the polymer was washed on a centrifuge train with 1N HCl and then with deionized water until residual chloride levels were <5 ppm. The polymer was isolated by steam precipitation followed by drying under hot nitrogen. The final dried resin weighed 4.1 lbs, had Mw=27652 daltons and PDI=2.5 by GPC vs PC standard, <1 ppm TEA, 0.6 ppm chloride ion, <10 ppm residual free BPA, and <0.05 ppm Fe. The glass transition temperature was determined to be 153 C.

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