antimony(3+);triacetate

反応条件: temp:254.01; pressure:0.00; stir:; See reaction.notes.procedure_details.

実験手順: Synthesis of the co-cyclohexane-tbia was carried out in a batch reactor which was charged with the following raw materials: 1,4 cyclohexane dicarboxylic acid (37 kg), tertiary butyl isophthalic acid (59.9 kg), 1,4 cyclohexane dimethanol (37.8 kg), neopentyl glycol (11.2 kg), ethylene glycol (60.3 kg), trimethylol propane (0.5 kg), and antimony (III) acetate (90 g). Under a pressure of 2 atmospheres (2×105 N/m2), this mixture was heated to 254 degrees C. while removing the reaction by-product, water. After completing this reaction and removing the water, the pressure was gradually reduced to 1 torr (263 N/m2) while heating to 290° C. The condensation by-product, ethylene glycol, was continuously removed until a polymer with intrinsic viscosity of 0.72 dl/g, as measured in 60/40 wt % phenol/o-dichlorobenzene, was produced. The polymer had a glass transition temperature of about 67° C. as measured by DSC with a temperature ramp of 20° C./min. This CCH-tbia had a refractive index of 1.519 as measured with a Metricon refractometer at 632 nm. was carried out in a batch reactor while removing the reaction by-product, water this reaction removing the water while heating to 290° C The condensation by-product, ethylene glycol, was continuously removed until a polymer with intrinsic viscosity of 0.72 dl/g was produced

反応条件: temp:254.01; pressure:0.00; stir:; See reaction.notes.procedure_details.

実験手順: Synthesis of the co-cyclohexane-tbia was carried out in a batch reactor which was charged with the following raw materials: 1,4 cyclohexane dicarboxylic acid (37 kg), tertiary butyl isophthalic acid (59.9 kg), 1,4 cyclohexane dimethanol (37.8 kg), neopentyl glycol (11.2 kg), ethylene glycol (60.3 kg), trimethylol propane (0.5 kg), and antimony (III) acetate (90 g). Under a pressure of 2 atmospheres (2×105 N/m2), this mixture was heated to 254 degrees C. while removing the reaction by-product, water. After completing this reaction and removing the water, the pressure was gradually reduced to 1 torr (263 N/m2) while heating to 290° C. The condensation by-product, ethylene glycol, was continuously removed until a polymer with intrinsic viscosity of 0.72 dl/g, as measured in 60/40 wt % phenol/o-dichlorobenzene, was produced. The polymer had a glass transition temperature of about 67° C. as measured by DSC with a temperature ramp of 20° C./min. This CCH-tbia had a refractive index of 1.519 as measured with a Metricon refractometer at 632 nm. was carried out in a batch reactor while removing the reaction by-product, water this reaction removing the water while heating to 290° C The condensation by-product, ethylene glycol, was continuously removed until a polymer with intrinsic viscosity of 0.72 dl/g was produced

反応条件: temp:254.01; pressure:0.00; stir:; See reaction.notes.procedure_details.

実験手順: Synthesis of the co-cyclohexane-tbia was carried out in a batch reactor which was charged with the following raw materials: 1,4 dimethyl cyclohexane dicarboxylate (8.45 kg), 1,4 cyclohexane dimethanol (8.98 kg), neopentyl glycol (1.8 kg), ethylene glycol (7.95 kg), trimethylol propane (0.2 kg), cobalt (II) acetate (3.6 g), zinc acetate (5.0 g), and antimony (III) acetate (6.5 g). Under a pressure of 2 atmospheres (2×105 N/m2), this mixture was heated to 254 C while removing the reaction by-product, methanol. After completing this reaction and removing the methanol, tertiary butyl isophthalate (9.48 kg) was charged to the reactor. Under a pressure of 2 atmospheres (2×105 N/m2), the mixture was heated to 254° C. until the reaction by-product, water, was removed. Triethyl phosphonoacetate (7.0 g) was then charged to the reactor and the pressure was gradually reduced to 1 torr (263 N/m2) while heating to 290° C. The condensation by-product, ethylene glycol, was continuously removed until a polymer with intrinsic viscosity of 0.72 dl/g, as measured in 60/40 wt % phenol/o-dichlorobenzene, was produced. The polymer had a glass transition temperature of about 67° C. as measured by DSC with a temperature ramp of 20° C./min. This CCH-tbia had a refractive index of 1.519 as measured with a Metricon refractometer at 632 nm. was carried out in a batch reactor Under a pressure of 2 atmospheres (2×105 N/m2), this mixture was heated to 254 C while removing the reaction by-product, methanol this reaction removing the methanol, tertiary butyl isophthalate (9.48 kg) was charged to the reactor was removed Triethyl phosphonoacetate (7.0 g) was then charged to the reactor while heating to 290° C The condensation by-product, ethylene glycol, was continuously removed until a polymer with intrinsic viscosity of 0.72 dl/g was produced

反応条件: temp:254.01; pressure:0.00; stir:; See reaction.notes.procedure_details.

実験手順: Synthesis of the co-cyclohexane-tbia was carried out in a batch reactor which was charged with the following raw materials: 1,4 dimethyl cyclohexane dicarboxylate (8.45 kg), 1,4 cyclohexane dimethanol (8.98 kg), neopentyl glycol (1.8 kg), ethylene glycol (7.95 kg), trimethylol propane (0.2 kg), cobalt (II) acetate (3.6 g), zinc acetate (5.0 g), and antimony (III) acetate (6.5 g). Under a pressure of 2 atmospheres (2×105 N/m2), this mixture was heated to 254 C while removing the reaction by-product, methanol. After completing this reaction and removing the methanol, tertiary butyl isophthalate (9.48 kg) was charged to the reactor. Under a pressure of 2 atmospheres (2×105 N/m2), the mixture was heated to 254° C. until the reaction by-product, water, was removed. Triethyl phosphonoacetate (7.0 g) was then charged to the reactor and the pressure was gradually reduced to 1 torr (263 N/m2) while heating to 290° C. The condensation by-product, ethylene glycol, was continuously removed until a polymer with intrinsic viscosity of 0.72 dl/g, as measured in 60/40 wt % phenol/o-dichlorobenzene, was produced. The polymer had a glass transition temperature of about 67° C. as measured by DSC with a temperature ramp of 20° C./min. This CCH-tbia had a refractive index of 1.519 as measured with a Metricon refractometer at 632 nm. was carried out in a batch reactor Under a pressure of 2 atmospheres (2×105 N/m2), this mixture was heated to 254 C while removing the reaction by-product, methanol this reaction removing the methanol, tertiary butyl isophthalate (9.48 kg) was charged to the reactor was removed Triethyl phosphonoacetate (7.0 g) was then charged to the reactor while heating to 290° C The condensation by-product, ethylene glycol, was continuously removed until a polymer with intrinsic viscosity of 0.72 dl/g was produced

反応条件: temp:60.01; pressure:0.00; stir:; See reaction.notes.procedure_details.

実験手順: Antimony oxalate solution was prepared by mixing antimony (III) acetate as obtained from Aldrich with a 1 M solution of oxalic acid in deionized water and heating the mixture to 60° C. A concentrated solution of ammonium hydroxide in deionized water was added dropwise to the antimony containing mixture until the solution became homogeneous. At this point, the solution was diluted as-required with oxalic acid solution or deionized water to desired metal concentration. The prepared antimony oxalate solution (3.3% antimony, 290.9 μL) was mixed with deionized water (1149.1 μL) and the resultant diluted solution (120 μL) was added to the supported rhodium-indium product of the first impregnation step and agitated by vibration for 30 minutes at room temperature. The obtained trimetallic material was dried at 120° C. for 2 hours and then calcined in air at 450° C. for 4 hours. to desired metal concentration The prepared antimony oxalate solution (3.3% antimony, 290.9 μL) was mixed with deionized water (1149.1 μL) the resultant diluted solution (120 μL) was added to the supported rhodium-indium product of the first impregnation step The obtained trimetallic material was dried at 120° C. for 2 hours calcined in air at 450° C. for 4 hours