Synthesis method of m-xylylene diisocyanate (MXDI)
A technology of xylylene diisocyanate and synthetic method, which is applied to the preparation of isocyanic acid derivatives, purification/separation of isocyanic acid derivatives, chemical instruments and methods, etc., can solve the problems of increasing raw material costs, and achieve reduction The effect of production investment cost, equipment requirement reduction and strong market competitiveness
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[0035] Example 1
[0036] (1) Weigh 150g of solid phosgene and dissolve it in 300g of chlorobenzene to obtain the first solid phosgene solution, which is heated to 55°C for later use;
[0037] (2) Weigh 100g of metaxylylenediamine (MXDA) and dissolve it in 200g of chlorobenzene to obtain a metaxylylenediamine solution;
[0038] (3) The metaxylylenediamine solution of step (2) was added dropwise to the solution of the first solid phosgene of step (1) at 55° C. within 2 hours. During the dropping, the precipitate under stirring Gradually generated
[0039] (4) After the dropwise addition is completed, the temperature is increased to 80°C at a heating rate of 15°C / h and the reaction is kept for 2h, and then the temperature is raised to the reflux temperature within 2h, so that the reaction system is in a reflux state.
[0040] (5) Dissolve 100 g of solid phosgene in 500 g of chlorobenzene to obtain a second solid phosgene solution, and add the second solid phosgene solution to the reactio...
Example Embodiment
[0044] Example 2
[0045] (1) Weigh 150g of solid phosgene and dissolve it in an inert solvent consisting of chlorobenzene, dichlorobenzene and toluene with a total weight of 450g to obtain the first solid phosgene solution, which is heated to 60°C for use;
[0046] (2) Weigh 100g of metaxylylenediamine (MXDA) and dissolve it in 400g of said inert solvent to obtain a metaxylylenediamine solution;
[0047] (3) The metaxylylenediamine solution of step (2) was added dropwise to the solution of the first solid phosgene of step (1) at 60° C. within 2.5 hours. During the dripping process, precipitation was carried out under stirring. Things gradually formed;
[0048] (4) After the dropwise addition is completed, the temperature is increased to 90° C. at a heating rate of 17° C. / h and the reaction is kept for 2.5 hours, and then the temperature is raised to the reflux temperature within 2 hours, so that the reaction system is in a reflux state.
[0049] (5) Dissolve 100 g of solid phosgene in...
Example Embodiment
[0053] Example 3
[0054] (1) Weigh 150g of solid phosgene and dissolve it in an inert solvent composed of chlorobenzene, dichlorobenzene, toluene and xylene with a total weight of 750g, to obtain the first solid phosgene solution, and raise the temperature to 70°C for use;
[0055] (2) Weigh 100g of metaxylylenediamine (MXDA) and dissolve it in 500g of the inert solvent to obtain a metaxylylenediamine solution;
[0056] (3) Add the metaxylylenediamine solution of step (2) dropwise to the first solid phosgene solution of step (1) at 70°C within 3 hours. During the dropping process, the precipitate under stirring Gradually generated
[0057] (4) After the dropwise addition is completed, the temperature is raised to 100°C at a heating rate of 20°C / h and the reaction is kept for 3 hours, and then the temperature is raised to the reflux temperature within 2 hours, so that the reaction system is in a reflux state.
[0058] (5) Dissolve 100 g of solid phosgene in 1000 g of the inert solvent ...
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