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Dipropylene glycol dibenzoate(DPGDB)
CAS №:
27138-31-4
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+++поиск в Reaxys
Последний раз редактировалось Indazole Вс июн 16, 2024 8:43 pm, всего редактировалось 1 раз.
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dipropylene glycol dibenzoate
C20H22O5
342.392
27138-31-4
одно получение
Current Patent Assignee: DYNAMIT NOBEL - US4112240, 1978, A
1 EXAMPLE 1
EXAMPLE 1 In a 10-liter flask with electrcal heating, stirrer, a fractioning column with glass Raschig rings and a nitrogen feed, 2144 weight parts of dipropylene glycol (= 16 moles) and 5227 weight parts of technical methyl benzoate with a purity of 93.6 wt-% (= 36 moles of pure ester content) were heated at atmospheric pressure with the addition of 7.4 weight parts of aluminum-sec.-butylate (Al(OC4 H9 -sec.)3) as catalyst (=0.1 wt-% with reference to the sum of the input quantities) as catalyst. At temperatures in the reaction flask up to 160° C, easily volatile compounds and water at first distilled out of the mixture. At 160° C the evolution of methanol began. For 5 hours the flask temperature rose steadily to 240° C. After this time the evolution of methanol had ended. The methanol-containing distillate had a content of 95% as measured by gas chromatography; the rest consisted of substances accompanying the technical methyl benzoate input product. Low-boiling substances and the excess methyl benzoate were then removed by distillation, after cooling, at temperatures up to 200° C in a vacuum of 20 Torr. The dipropyleneglycol dibenzoate obtained in a yield of 98% of the theory with reference to the dipropyleneglycol input had an acid number of 1.6, a saponification number of 326.5 (calculated 328) and an iodine color number of 10. The product was cooled to 150° C and ozonized for 30 minutes (ozone apparatus Model S2 made by Argentox, Hamburg; output: 1.5 g O3 per hour at 12 kV and 90W). After the ozonization the iodine color number was 3, and after aqueous-alkaline refinement it was 2. The acid number of the final product was 0.3, the saponification number 329.5.
и дейтерированный аналог
спирт + дейтеро-бензоил хлорид
at 90 - 110℃;
Hetayothin, Boonta; Cabaniss, Roy A.; Blum, Frank D.
[Macromolecules, 2012, vol. 45, # 22, p. 9128 - 9138]
C20H22O5
342.392
27138-31-4
одно получение
Current Patent Assignee: DYNAMIT NOBEL - US4112240, 1978, A
1 EXAMPLE 1
EXAMPLE 1 In a 10-liter flask with electrcal heating, stirrer, a fractioning column with glass Raschig rings and a nitrogen feed, 2144 weight parts of dipropylene glycol (= 16 moles) and 5227 weight parts of technical methyl benzoate with a purity of 93.6 wt-% (= 36 moles of pure ester content) were heated at atmospheric pressure with the addition of 7.4 weight parts of aluminum-sec.-butylate (Al(OC4 H9 -sec.)3) as catalyst (=0.1 wt-% with reference to the sum of the input quantities) as catalyst. At temperatures in the reaction flask up to 160° C, easily volatile compounds and water at first distilled out of the mixture. At 160° C the evolution of methanol began. For 5 hours the flask temperature rose steadily to 240° C. After this time the evolution of methanol had ended. The methanol-containing distillate had a content of 95% as measured by gas chromatography; the rest consisted of substances accompanying the technical methyl benzoate input product. Low-boiling substances and the excess methyl benzoate were then removed by distillation, after cooling, at temperatures up to 200° C in a vacuum of 20 Torr. The dipropyleneglycol dibenzoate obtained in a yield of 98% of the theory with reference to the dipropyleneglycol input had an acid number of 1.6, a saponification number of 326.5 (calculated 328) and an iodine color number of 10. The product was cooled to 150° C and ozonized for 30 minutes (ozone apparatus Model S2 made by Argentox, Hamburg; output: 1.5 g O3 per hour at 12 kV and 90W). After the ozonization the iodine color number was 3, and after aqueous-alkaline refinement it was 2. The acid number of the final product was 0.3, the saponification number 329.5.
и дейтерированный аналог
спирт + дейтеро-бензоил хлорид
at 90 - 110℃;
Hetayothin, Boonta; Cabaniss, Roy A.; Blum, Frank D.
[Macromolecules, 2012, vol. 45, # 22, p. 9128 - 9138]
Re: поиск в Reaxys
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