Curable composition
A composition and polymer technology, applied in the field of curable composition of calcium citrate, to achieve the effect of increasing viscosity ratio, improving mechanical properties and adhesiveness, and improving scraper peelability
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preparation example 1
[0435] (Synthesis of alkenyl-containing carboxylate)
[0436] To methanol (250 ml) were added 10-undecenoic acid (150 g, 0.814 mol) and potassium tert-butoxide (91.3 g, 0.814 mol), and the mixture was stirred at 0°C. Heating under reduced pressure, distilling off volatile substances to obtain potassium undecylenate represented by the following formula: CH 2 =CH-(CH 2 ) 8 -CO 2 -+ K.
[0437] (Semi-batch Polymerization BA-5kg)
[0438] A 10 L glass reaction was charged with cuprous bromide (35.3 g, 0.246 mol) and acetonitrile (470 mL) and the contents heated at 70°C for 60 minutes. Butyl acrylate (970 ml, 6.56 mol) was further added thereto, and the mixture was stirred for an additional 60 minutes. Pentamethyldiethylenetriamine (2.00 mL, 9.58 mmol) was added to initiate polymerization. Then, after 55 minutes, butyl acrylate (3.76 L, 26.2 moles) was added over a period of 260 minutes, during which time the reaction was followed by sampling the reaction mixture while pent...
preparation example 2
[0442] A 2-liter separable flask equipped with a reflux condenser and stirrer was charged with CuBr (8.39 g, 0.0585 mol). The interior of the reactor was purged with nitrogen. Acetonitrile (112 ml) was added, and the mixture was stirred on a 70°C oil bath for 30 minutes. Then, butyl acrylate (224 ml), diethyl 2,5-dibromoadipate (23.4 g, 0.0650 mol) and pentamethyldiethylenetriamine (hereinafter referred to as triamine) (0.500 ml) were added. , 0.244 mmol), start the reaction. With continuous stirring and heating at 70°C, butyl acrylate (895 mL) was continuously added dropwise over 150 minutes. Additional triamine (2.50 mL, 12.0 mmol) was added during the dropwise addition of butyl acrylate. 310 minutes after the start of the reaction, 1,7-octadiene (288 ml, 1.95 mol) and triamine (4.0 ml, 0.0195 mol) were added, and the whole mixture was stirred under heating at 70° C. for 240 minutes.
[0443] The reaction mixture was diluted with hexane, passed through an activated alumi...
preparation example 3
[0448] (Synthesis of alkenyl-containing carboxylate)
[0449] To methanol (250 ml) were added 10-undecenoic acid (150 g, 0.814 mol) and potassium tert-butoxide (91.3 g, 0.814 mol), and the mixture was stirred at 0°C. Heating under reduced pressure, distilling off volatile substances to obtain potassium undecylenate represented by the following formula: CH 2 =CH-(CH 2 ) 8 -CO 2 -+ K.
[0450] (semi-batch polymerization BA-1 kg)
[0451] A 2 liter glass reaction was charged with cuprous bromide (8.39 g, 0.0585 mol) and acetonitrile (112 mL) and the contents heated at 70°C for 60 minutes. Butyl acrylate (224 ml, 1.56 mol) was further added thereto, and the mixture was stirred for an additional 30 minutes. To this was added pentamethyldiethylenetriamine (0.41 mL, 1.95 mmol) to initiate polymerization. During this period, the reaction was followed by sampling the reaction mixture, while pentamethyldiethylenetriamine (5.66 ml, 27.1 mmol) was added, and butyl acrylate (895 ml...
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