반응 #1178389

반응 방정식

hydrogen peroxide

sulphuric acid

2,5-dimethyl-2,5-hexanediol

→

2,5-dimethyl-2,5-di(tert-butylperoxy)hexane

수율 90.0%

용매

water

반응 조건

후처리

1. 1
   기타were metered in within 60 min, in the course of which
2. 2
   기타rose from 20° C. to 30-32° C
3. 3
   workup.STIRRINGThe reaction mixture was stirred at 30° C. for another 90 min
4. 4
   기타the suspension formed
5. 5
   여과was filtered within 10 min
6. 6
   여과to the filtration devices (5)
7. 7
   세척was washed
8. 8
   workup.ADDITIONby adding 500 kg of water
9. 9
   workup.STIRRINGstirring the suspension for 3 min
10. 10
    여과filtering again
11. 11
    여과to the filtration devices (5)
12. 12
    workup.ADDITIONThereafter, 481 kg of tert-butanol were added
13. 13
    workup.DISSOLUTIONthe solid was dissolved
14. 14
    workup.STIRRINGby stirring
15. 15
    온도heating
16. 16
    workup.STIRRINGwith stirring
17. 17
    온도cooling of the reactor through the jacket, in the course of which the temperature
18. 18
    기타rose to from 40 to 45° C
19. 19
    workup.STIRRINGThe reaction mixture was stirred at this temperature for a further 60 min
20. 20
    기타The lower aqueous phase was removed
21. 21
    세척the liquid product was washed successively with 150 kg of water, 150 kg of 1% by weight sodium hydroxide solution and 150 kg of water
22. 22
    workup.STIRRINGby stirring the phases
23. 23
    기타removing the lower aqueous phase
24. 24
    기타After removal of residual water and volatile by-products

실험 절차

A reactor corresponding to FIG. 1 was initially charged with a mixture of 550 kg of 70% by weight hydrogen peroxide and 366 kg of 80% by weight sulphuric acid. With stirring and cooling of the reactor through the jacket, 250 kg of 2,5-dimethyl-2,5-hexanediol were metered in within 60 min, in the course of which the temperature rose from 20° C. to 30-32° C. The reaction mixture was stirred at 30° C. for another 90 min and then admixed with 200 kg of water. The stirrer was then switched off and the suspension formed was filtered within 10 min by applying reduced pressure to the filtration devices (5), in the course of which the liquid phase was sucked into the collecting vessel (7) and the precipitated 2,5-dimethylhexane-2,5-dihydroperoxide was retained in the vessel (2). The solid product retained in the reactor was washed by adding 500 kg of water, stirring the suspension for 3 min and filtering again by applying reduced pressure to the filtration devices (5). This washing operation was repeated once more. Thereafter, 481 kg of tert-butanol were added and the solid was dissolved therein by stirring and heating. 500 kg of 80% by weight sulphuric acid were metered into the resulting solution within 60 min with stirring and cooling of the reactor through the jacket, in the course of which the temperature rose to from 40 to 45° C. The reaction mixture was stirred at this temperature for a further 60 min and then admixed with 50 kg of water. The lower aqueous phase was removed and the liquid product was washed successively with 150 kg of water, 150 kg of 1% by weight sodium hydroxide solution and 150 kg of water, by stirring the phases and then removing the lower aqueous phase. After removal of residual water and volatile by-products by stripping under reduced pressure in a stripping column, 405 kg (90%) of 2,5-dimethyl-2,5-di(tert-butylperoxy)hexane were obtained.

출처