Process for preparing polyisocyanate by solid phosgene
A polyisocyanate and solid phosgene technology, which is applied in the preparation of isocyanate derivatives, chemical instruments and methods, and the preparation of organic compounds, etc., can solve the problems of cumbersome process, complicated post-treatment and purification process, and insufficient color and mechanical properties of isocyanate polyurethane. Meet the use requirements and other issues
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Embodiment 1
[0018] Lysine Triisocyanate (LTI):
[0019] Add 449.6g (4.31mol) 35% HCl solution in 1L four-necked flask and dropwise add 167.2g (2.74mol) ethanolamine in 30 minutes, add 250.0g (1.37mol) lysine hydrochloride after dropwise addition, and The reaction was stirred at 45°C for 10 minutes. The temperature was raised to 110°C, the pressure was reduced to 4KPa, and the water in the reaction system was evaporated. After returning to normal pressure, HCl gas was passed through to react for 3 hours, and then the water was evaporated under reduced pressure. This process is repeated several times, and the reaction is stopped after lysine hydrochloride is consumed, and o-dichlorobenzene (ODCB) and methanol are added to crystallize, and the crystal is washed several times with ODCB to obtain lysine aminoethyl ester trihydrochloride (LAET) .
[0020] The 2500ml reactor is equipped with mechanical stirring and two sets of dripping devices. Add 100ml o-dichlorobenzene (ODCB) in the react...
Embodiment 2
[0022] Lysine Triisocyanate (LTI):
[0023] Except that bis-(trichloromethyl)carbonate is changed into 445.5g (1.5mol), other reaction conditions are the same as embodiment 1, obtain LTI content 68.6% (HPLC) in the product, NCO content 40.3wt% (theoretical value 47.2wt%) %), HCl content 0.70wt%, ODCB content 0.81wt%.
Embodiment 3
[0025] Lysine Triisocyanate (LTI):
[0026] Except that bis-(trichloromethyl) carbonate is changed to 891g (3mol), other reaction conditions are the same as in Example 1, and LTI content 86.3% (HPLC) is obtained in the product, NCO content 43.6wt% (theoretical value 47.2wt%) , HCl content 0.35wt%, ODCB content 0.31wt%.
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