Method of preparing diisocyanate composition
A technology of diisocyanate and composition, applied in the field of triphosgene composition, can solve the problems of reduced yield, increased purity of final product, difficulty in storage and management, etc., and achieves high yield, excellent handling convenience and excellent processability. Effect
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example A1
[0226] Into a 5-liter 4-neck reactor, 963.5 g (9.25 moles) of 35% aqueous hydrochloric acid was charged, and then the internal temperature of the reactor was lowered to 15°C while stirring. While maintaining the temperature of the reactor at 50° C., 600.0 g (4.4 moles) of m-xylylenediamine (m-XDA) was introduced for 1 hour. After the introduction was completed, the internal temperature of the reactor was lowered to 10° C., and it was stirred for 1 hour. Thereafter, 1,200.0 g of diethyl ether (Et 2 O) as an organic solvent, and the internal temperature of the reactor was lowered to -5°C, followed by stirring for 1 hour. After the reaction was completed, it was vacuum filtered using a filter, and the filtered diethyl ether was recovered for reuse. The recovery of diethyl ether was 73%. After vacuum filtration, m-xylylenediamine (m-XDA) hydrochloride composition was obtained. In order to remove the residual organic solvent and water, the reactor was dried under the conditions...
example A2
[0228] Into a 5-liter 4-neck reactor, 986.5 g (9.47 moles) of 35% aqueous hydrochloric acid was charged, and then the internal temperature of the reactor was lowered to 15° C. while stirring. While maintaining the temperature of the reactor at 50°C, 600.0 g (4.4 moles) of m-XDA was introduced for 1 hour. After the introduction was completed, the internal temperature of the reactor was lowered to 10° C., and it was stirred for 1 hour. Thereafter, 1,260 g of isopropanol (i-PrOH) was introduced as an organic solvent, and the internal temperature of the reactor was lowered to -5° C., followed by stirring for 1 hour. After the reaction was completed, it was vacuum filtered using a filter, and the filtered isopropanol was recovered for reuse. Here, the recovery rate of isopropanol was 75%. After vacuum filtration, the m-XDA hydrochloride composition was obtained. In order to remove the residual organic solvent and water, drying was carried out under the condition that the externa...
example A3
[0230]Into a 5-liter 4-neck reactor was charged 1,009.4 g (9.69 moles) of a 35% aqueous hydrochloric acid solution, and then the internal temperature of the reactor was lowered to 15° C. with stirring. While maintaining the temperature of the reactor at 50°C, 600.0 g (4.4 moles) of m-XDA was introduced for 1 hour. After the introduction was completed, the internal temperature of the reactor was lowered to 10° C., and it was stirred for 1 hour. Thereafter, 1,320 g of tetrahydrofuran was introduced, and the internal temperature of the reactor was lowered to -5° C., followed by stirring for 1 hour. After the reaction was finished, it was vacuum filtered using a filter, and the filtered tetrahydrofuran was recovered for reuse. The recovery of tetrahydrofuran was 82%. After vacuum filtration, the m-XDA hydrochloride composition was obtained. In order to remove the residual solvent and water, drying was carried out under the condition that the external temperature of the reactor ...
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