The preparation method of low free m-xylylene isocyanate polyurethane prepolymer
A polyurethane prepolymer and low-free technology, which is applied in the field of prepolymer preparation, can solve the problems of difficult to achieve high-efficiency removal of monomers at one time and increased difficulty, and achieve the effects of long storage period, stable performance and low viscosity
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Embodiment 1
[0042] Melt polytetrahydrofuran polyol PTMEG1000, keep the temperature at 60°C, and wait for use; under the protection of nitrogen, add 282.3g of mXDI and 500g of glycerol triacetate into the reaction vessel, stir and mix evenly, and maintain the temperature at 60°C. Then, 500 g of polyol PTMEG1000 liquid was added dropwise into the reaction vessel under the condition of stirring, and the dropping time was 2 hours; after stirring and reacting at 60° C. for 5 hours, mXDI-PTMEG1000 polyurethane prepolymer reaction solution was obtained.
[0043] Under the condition of 80°C, the obtained mXDI polyurethane prepolymer reaction solution was added to the thin film evaporation equipment, the film temperature was set at 95°C, the vacuum degree was 0.1-0.2mmHg, and the condensation temperature was 20-25°C. The distillate was recombined to obtain a low-free mXDI polyurethane prepolymer with a measured NCO value of 4.86% (theoretical value 6.03%). The content of free mXDI in the polyureth...
Embodiment 2
[0045] Melt 500g of polytetrahydrofuran polyol PTMEG1000 at 60°C, and mix it with 300g of glycerol triacetate evenly in another container, keep the temperature at 25-30°C for use; under nitrogen protection, mix 282.3g of mXDI and 500g of Add glycerol triacetate into the reaction vessel, stir and mix evenly, and maintain the temperature at 25°C. The above polyol solution was slowly added to the reaction vessel containing the mXDI solution under the condition of stirring and nitrogen, and the dropping time was 2 hours. After the dropwise addition was completed, 200 g of glycerol triacetate was added. After continuing the reaction at 25° C. for 18 h, a mXDI-PTMEG1000 polyurethane prepolymer reaction solution was obtained.
[0046] At 60°C, the obtained polyurethane prepolymer was added to the thin film evaporation equipment, the film temperature was set at 100°C, the vacuum degree was 0.1-0.2mmHg, the condensation temperature was 20-25°C, and the low free mXDI- PTMEG1000 polyur...
Embodiment 3
[0048] Melt polytetrahydrofuran polyol PTMEG1000, keep the temperature at 60°C, and wait for use; under the protection of nitrogen, add 376.4g of mXDI and 300g of glycerol triacetate into the reaction vessel, stir and mix evenly, and keep the temperature at 70°C; 500g of polytetrahydrofuran polyol PTMEG1000 and 300g of glycerol triacetate were mixed uniformly in another container and then added to the above reaction container for 1.5 hours. After the addition, 200 g of glycerol triacetate was added, and the reaction was continued at 70° C. for 4 hours to obtain a mXDI-PTMEG1000 polyurethane prepolymer reaction solution.
[0049] Under the condition of 80°C, the obtained polyurethane prepolymer reaction solution was added to the thin film evaporation equipment, the film temperature was set at 100°C, the vacuum degree was 0.2-0.5mmHg, the condensation temperature was 20-25°C, and the low free The measured NCO value of mXDI-PTMEG1000 polyurethane prepolymer is 5.87%; the free mXD...
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