tert-butyl benzenecarboperoxoate

反応条件: temp:0.00; pressure:0.00; stir:

反応条件: temp:0.00; pressure:0.00; stir:

反応条件: temp:100.01; pressure:0.00; stir:; See reaction.notes.procedure_details.

実験手順: To a monomeric mixture of the formulation shown in Table 8 were added 10 g of tert-butyl perbenzoate and 30 g of azobisbutyronitrile. The mixture was then added dropwise over the course of 4 hours to 1,000 ml of toluene heated at 100° C. The reaction was further continued for 10 hours at 100° C, and then the toluene was removed to provide an acrylic copolymer resin having a number average molecular weight of about 20,000 and an oxirane group content of 2,150 g·eq/106 g and a softening point of 110° C. Powder paints were prepared in the same way as in Example 1 except that the polyester and the acrylic resin in the amounts shown in Table 9 were used instead of the polyester A and triglycidyl isocyanurate. The powder paints were coated, and baked at a temperature of 200° C for 30 minutes. The resulting coatings had a film thickness of 60 to 65μ and the properties shown in Table 10. To a monomeric mixture of the formulation the toluene was removed

反応条件: temp:0.00; pressure:0.00; stir:

反応条件: temp:0.00; pressure:0.00; stir:

反応条件: temp:40.01; pressure:0.00; stir:; See reaction.notes.procedure_details.

実験手順: 30 g of M-TMI (M-TMI is 1-(1-isocyanato-1-methyl)ethyl-3-(1-methyl)ethenyl benzene, from Cytec industries), 5 g of ethyl acrylate, 15 g of methyl methacrylate and 8 g of t-butyl peroxybenzoate were heated to 120° C. in 232 g of Arcosolve PMAcetate (propylene glycol methyl ether acetate from Arco Chemicals) in a N2 purge. Then a mixture of 90 g of m-TMI, 15 g of ethyl acrylate, 45 g of methyl methacrylate, 16 g of t-butyl peroxybenzoate (Aldrich Chemicals) was added over 2 hours. After the addition was complete, an additional 8 g of t-butyl peroxybenzoate was added in two equal portions. The reaction was completed to theoretical % non-volatiles (50%) in 7 hrs. Then a partial batch of this solution (164.54 g), containing free —NCO groups of m-TMI, was further reacted with p-aminophenol (22.25 g) at 1:1 equivalent ratio. The reaction was monitored by IR-spectroscopy for disappearance of —NCO group at 2275 cm−1 and was completed by heating to 40° C. The product (AR-1), terpolymer of ethyl acrylate, methyl methacrylate and the urea adduct of m-TMI/p-aminophenol, was precipitated in powder form using water/ice, filtered and dried at room temperature. The product terpolymer AR-1 had the following structure: purge Then a mixture of 90 g of m-TMI, 15 g of ethyl acrylate, 45 g of methyl methacrylate, 16 g of t-butyl peroxybenzoate (Aldrich Chemicals) was added over 2 hours After the addition an additional 8 g of t-butyl peroxybenzoate was added in two equal portions in 7 hrs Then a partial batch of this solution (164.54 g), containing free —NCO groups of m-TMI was further reacted with p-aminophenol (22.25 g) at 1 The product (AR-1), terpolymer of ethyl acrylate, methyl methacrylate and the urea adduct of m-TMI/p-aminophenol, was precipitated in powder form filtered dried at room temperature

反応条件: temp:40.01; pressure:0.00; stir:; See reaction.notes.procedure_details.

実験手順: 30 g of M-TMI (M-TMI is 1-(1-isocyanato-1-methyl)ethyl-3-(1-methyl)ethenyl benzene, from Cytec industries), 5 g of ethyl acrylate, 15 g of methyl methacrylate and 8 g of t-butyl peroxybenzoate were heated to 120° C. in 232 g of Arcosolve PMAcetate (propylene glycol methyl ether acetate from Arco Chemicals) in a N2 purge. Then a mixture of 90 g of m-TMI, 15 g of ethyl acrylate, 45 g of methyl methacrylate, 16 g of t-butyl peroxybenzoate (Aldrich Chemicals) was added over 2 hours. After the addition was complete, an additional 8 g of t-butyl peroxybenzoate was added in two equal portions. The reaction was completed to theoretical % non-volatiles (50%) in 7 hrs. Then a partial batch of this solution (164.54 g), containing free —NCO groups of m-TMI, was further reacted with p-aminophenol (22.25 g) at 1:1 equivalent ratio. The reaction was monitored by IR-spectroscopy for disappearance of —NCO group at 2275 cm−1 and was completed by heating to 40° C. The product (AR-1), terpolymer of ethyl acrylate, methyl methacrylate and the urea adduct of m-TMI/p-aminophenol, was precipitated in powder form using water/ice, filtered and dried at room temperature. The product terpolymer AR-1 had the following structure: purge Then a mixture of 90 g of m-TMI, 15 g of ethyl acrylate, 45 g of methyl methacrylate, 16 g of t-butyl peroxybenzoate (Aldrich Chemicals) was added over 2 hours After the addition an additional 8 g of t-butyl peroxybenzoate was added in two equal portions in 7 hrs Then a partial batch of this solution (164.54 g), containing free —NCO groups of m-TMI was further reacted with p-aminophenol (22.25 g) at 1 The product (AR-1), terpolymer of ethyl acrylate, methyl methacrylate and the urea adduct of m-TMI/p-aminophenol, was precipitated in powder form filtered dried at room temperature

反応条件: temp:130.01; pressure:0.00; stir:; See reaction.notes.procedure_details.

実験手順: 10.76 g of N-vinyl-2-pyrrolidone and the temperature is raised to 130° C. Then 0.9 g of tert-butyl perbenzoate is added. After 1 and 2 hours, respectively, a 0.4 g portion of tert-butyl perbenzoate is fed in. The charge is maintained at 130° C. for another 5 hours. A clouded viscous solution is obtained. After 1 and 2 hours A clouded viscous solution is obtained

反応条件: temp:130.01; pressure:0.00; stir:; See reaction.notes.procedure_details.

実験手順: 10.76 g of N-vinyl-2-pyrrolidone and the temperature is raised to 130° C. Then 0.9 g of tert-butyl perbenzoate is added. After 1 and 2 hours, respectively, a 0.4 g portion of tert-butyl perbenzoate is fed in. The charge is maintained at 130° C. for another 5 hours. A clouded viscous solution is obtained. After 1 and 2 hours A clouded viscous solution is obtained

反応条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

実験手順: copolymer prepared by copolymerizing styrene with 1-(1-isocyanato-1-methylethyl)-3-(1-methylethenyl)benzene (hereinafter referred to as "TMI") (registered trademark) manufactured by Cyanamid Corporation in the presence of t-butyl peroxybenzoate as an initiator by solution polymerization (hereinafter referred to briefly as "PSTMI")

反応条件: temp:82.01; pressure:0.00; stir:; See reaction.notes.procedure_details.

実験手順: Deionized water (150 ml), isopropyl alcohol (200 ml) and oleic acid (43.78 g, 0.155 mol) were placed in a 1.0 liter flask equipped with stirrer, additional funnel, reflux condenser, thermometer and a gas inlet tube. To the additional funnel was added a premix which contained 15.2 g (0.08 mol) of sodium metabisulfite (Na2S2O5) and 1.28 g of NaOH in 55 g of water. The whole device was bubbled gently with nitrogen. After heating to reflux (82° C.), a small portion of t-butyl perbenzoate (out of total amount of 0.5 g, 2.5 mmol) was added to the flask. Then the Na2S2O5/NaOH premix was added through the addition funnel continuously over the course of five hours. The remaining t-butyl perbenzoate was also added in portions during this time. equipped with stirrer, additional funnel reflux condenser To the additional funnel was added a premix which The whole device was bubbled gently with nitrogen After heating was added through the addition funnel continuously over the course of five hours

反応条件: temp:82.01; pressure:0.00; stir:; See reaction.notes.procedure_details.

実験手順: Deionized water (150 ml), isopropyl alcohol (200 ml) and oleic acid (43.78 g, 0.155 mol) were placed in a 1.0 liter flask equipped with stirrer, additional funnel, reflux condenser, thermometer and a gas inlet tube. To the additional funnel was added a premix which contained 15.2 g (0.08 mol) of sodium metabisulfite (Na2S2O5) and 1.28 g of NaOH in 55 g of water. The whole device was bubbled gently with nitrogen. After heating to reflux (82° C.), a small portion of t-butyl perbenzoate (out of total amount of 0.5 g, 2.5 mmol) was added to the flask. Then the Na2S2O5/NaOH premix was added through the addition funnel continuously over the course of five hours. The remaining t-butyl perbenzoate was also added in portions during this time. equipped with stirrer, additional funnel reflux condenser To the additional funnel was added a premix which The whole device was bubbled gently with nitrogen After heating was added through the addition funnel continuously over the course of five hours