Refining method for n-butyl isocyanate
A technology of n-butyl isocyanate and refining method, which is applied to the preparation of isocyanic acid derivatives, purification/separation of isocyanic acid derivatives, chemical instruments and methods, etc., and can solve problems such as affecting product quality and reducing reaction yield. Achieve the effect of reducing temperature and time and improving purity
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Embodiment 1
[0026] Add xylene solution to the reaction kettle first, and cool the temperature in the reaction kettle to -10°C to allow cold reaction to reduce side reactions;
[0027] Pass phosgene into the xylene solution in the step 1 again, the time is 30 minutes, can make material can react completely;
[0028] Add n-butylamine solution dropwise to the reaction kettle again, and the temperature of the n-butylamine solution added dropwise is 20°C, while stirring while adding dropwise, the time is 1.0 hour, which can make the cold reaction react completely and reduce the generation of by-products;
[0029] Then continue to feed phosgene into the reaction kettle, the temperature in the reaction kettle is raised to 70°C, continue to stir, and at the same time continue to raise the temperature in the reaction kettle to 105°C for 1.0 hour, the second step of high temperature reaction can be carried out to generate n-butyl Isocyanate, and improve the reaction efficiency;
[0030] Into the r...
Embodiment 2
[0035] Add xylene solution to the reaction kettle first, and cool the temperature in the reaction kettle to -8°C to allow cold reaction to reduce side reactions;
[0036] Pass phosgene into the xylene solution in the step 1 again, the time is 35 minutes, can make material can react completely;
[0037] Add n-butylamine solution dropwise to the reaction kettle again, and the temperature of the n-butylamine solution added dropwise is 16°C, while stirring while adding dropwise, the time is 1.2 hours, which can make the cold reaction react completely and reduce the generation of by-products;
[0038] Then continue to feed phosgene into the reaction kettle, the temperature in the reaction kettle is raised to 74°C, continue to stir, and at the same time, continue to raise the temperature in the reaction kettle to 110°C for 1.5 hours, and the second step of high temperature reaction can be performed to generate n-butyl Isocyanate, and improve the reaction efficiency;
[0039] Into t...
Embodiment 3
[0044] Add xylene solution to the reaction kettle first, and cool the temperature in the reaction kettle to -4°C to allow cold reaction to reduce side reactions;
[0045] Pass phosgene into the xylene solution in the step 1 again, the time is 39 minutes, can make material can react completely;
[0046] Add n-butylamine solution dropwise to the reaction kettle again, and the temperature of the n-butylamine solution added dropwise is 14°C, while stirring while adding dropwise, the time is 1.5 hours, which can make the cold reaction completely react and reduce the generation of by-products;
[0047] Then continue to feed phosgene into the reaction kettle, the temperature in the reaction kettle is raised to 76°C, continue to stir, and at the same time continue to raise the temperature in the reaction kettle to 115°C for 1.8 hours, the second step of high temperature reaction can be carried out to generate n-butyl Isocyanate, and improve the reaction efficiency;
[0048] Into the ...
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