A kind of unsaturated polyether monomer and its preparation method and application
A polyether monomer, unsaturated technology, applied in the field of polyether, can solve the problem of low polymerization activity of polyether monomer, achieve the effect of improving dispersion performance, simple preparation method, and environmental friendliness
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Embodiment 1
[0029] 240 parts of unsaturated polyoxyalkyl ether (methallyl polyoxyethylene ether with a molecular weight of 2400) was vacuum dehydrated at 85° C. for about 1 hour until the water content was as low as 0.3%. Then place it in a three-necked flask equipped with a nitrogen protection device, a thermometer and a stirrer, perform nitrogen replacement, turn on the heating, stir and heat up to 70°C, then slowly add 13.32 parts of m-toluene isocyanate to the flask at a uniform speed, and control the reaction temperature to 70°C. ℃, the dropping time is 20 minutes, after the dropwise addition is completed, keep warm for 2 hours, vacuumize and degas, and discharge the material to obtain the new unsaturated end-capped polyether product.
[0030] NMR nuclear magnetic resonance proton spectrum measures novel unsaturated capped polyether structural formula as shown in formula (3), 1 See attached for HNMR spectrum figure 1 .
[0031]
[0032] According to the hydroxyl value method, th...
Embodiment 2
[0034] 300 parts of unsaturated polyoxyalkyl ether (methallyl polyoxyethylene ether with a molecular weight of 3000) was vacuum dehydrated at 85° C. for about 1 hour until the water content was lower than 0.3%. Then place it in a three-necked flask equipped with a nitrogen protection device, a thermometer and a stirrer, perform nitrogen replacement, turn on the heating, stir and heat up to 70°C, then slowly add 19.97 parts of butyl isocyanate to the flask at a uniform speed, and control the reaction temperature to 70°C. ℃, the dropping time is 40 minutes, after the dropping is completed, keep warm for 2 hours, after vacuuming and degassing, the material is discharged, and the new unsaturated end-capped polyether product is obtained. The structural formula of the novel unsaturated end-capped polyether determined by hydrogen NMR spectroscopy is shown in formula (4).
[0035]
[0036] The end-capping rate calculated by the hydroxyl value method was 91.2%.
Embodiment 3
[0038] 400 parts of unsaturated polyoxyalkyl ether (3-methyl-3-butenyl polyoxypropylene polyoxyethylene ether with a molecular weight of 4000, block, EO / PO mass ratio = 7:1) were vacuum dehydrated at 85°C For about 1 hour, dehydrate until the moisture content is as low as 0.3%. Then place it in a three-necked flask equipped with a nitrogen protection device, a thermometer and a stirrer, perform nitrogen replacement, turn on the heating, stir and raise the temperature to 80°C, then slowly add 39.95 parts of p-toluene isocyanate to the flask at a uniform speed, and control the reaction temperature to 80°C. ℃, the dropping time is 10 minutes, after the dropping is completed, the temperature is kept for 2 hours, and after vacuuming and degassing, the material is discharged to obtain the novel unsaturated end-capped polyether product. The structural formula of the novel unsaturated capped polyether determined by hydrogen nuclear magnetic resonance spectrum is shown in formula (5). ...
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