Technique for preparing polyester polyol
The technology of a polyester polyol and a process method, which is applied in the field of chemical material synthesis, can solve the problems of single heating and temperature control method, high acid value, large loss of diol, etc., so as to reduce the probability of product yellowing, Reduce the molecular weight distribution coefficient and reduce the effect of diol cyclization
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Embodiment 1
[0024] 1) Add 374.54g of ethylene glycol to the reactor equipped with rectification device, start to stir and raise the temperature, add 810g of adipic acid (theoretical alkyd ratio 1.089) under the protection of nitrogen, and raise the temperature to 220°C for esterification reaction and dehydration in 4h. The temperature at the top of the distillation tower is controlled at 98~100℃;
[0025] 2) Constant temperature sampling at 220℃ to test the acid value. After the acid value is lower than 20mgKOH / g, add 30ppm catalyst tetraisopropyl titanate, and add ethylene glycol 14.98g, total alkyd ratio 1.13, and catalytic reaction under normal pressure for 1h ;
[0026] 3) Then slowly load the vacuum, load the vacuum to -0.09MPa within 1h, and react under reduced pressure for 3.5h;
[0027] 4) After the test acid value is lower than 0.5mgKOH / g, keep the temperature under reduced pressure, the temperature in the reactor drops to 135℃ and sample for analysis. The final reaction process (inclu...
Embodiment 2
[0035] 1) Add 466.39g of butanediol to the reactor equipped with rectification device, start to stir and raise the temperature, add 720.39g of adipic acid (theoretical alkyd ratio 1.050) under nitrogen protection, the adipic acid will gradually dissolve, and the temperature will rise to 230 in 5h ℃ esterification reaction dehydration, the top temperature of the distillation tower is controlled at 98~100℃;
[0036] 2) 230℃ constant temperature sampling test acid value, after the acid value is lower than 20mgKOH / g, add 60ppm catalyst tetraisopropyl titanate, at the same time add 16.32g butanediol, total alkyd ratio is 1.09, normal pressure catalysis 0.5 h;
[0037] 3) Then slowly load the vacuum, load the vacuum to -0.095MPa within 1h, and react under reduced pressure for 5.0h;
[0038] 4) After the test acid value is lower than 0.5mgKOH / g, keep the temperature under reduced pressure, the temperature in the reactor drops to 130℃ and take samples for analysis. The final reaction proces...
Embodiment 3
[0047] 1) Add 523.44g of butanediol to a reactor equipped with a rectification device. After the nitrogen is evacuated, turn on the stirring and increase the temperature, add 657g of succinic acid (theoretical alkyd ratio 1.04), and after the succinic acid is dissolved, within 5h Heat up to 225℃ for esterification reaction dehydration, and control the top temperature of the distillation tower at 99-100℃;
[0048] 2) Constant temperature sampling at 225°C to test the acid value. After less than 20mgKOH / g, add 50ppm of the catalyst tetraisopropyl titanate and 77.86g of butanediol, the total alkyd ratio is 1.2, and the normal pressure catalysis is 1h;
[0049] 3) Then slowly load the vacuum, load the vacuum to -0.092Mpa within 1h, and react under reduced pressure for 4h;
[0050] 4) After the acid value is lower than 0.5mgKOH / g, the temperature is kept under reduced pressure and the temperature in the reactor drops to 135°C for sampling and analysis. The final reaction process takes 13...
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