Process for continuous oligomerization of isocyanates
A technology of isocyanate and hexamethylene diisocyanate, applied in the field of continuous oligomerization of isocyanate
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Embodiment 1
[0079] Example 1: Continuous experiment in a plate reactor
[0080] 1- The characteristics of the reactor:
[0081] The plate reactor used is a laboratory-scale stainless steel reactor, and its processing flow rate can be between 200 ml per hour and 10 liters per hour. The reactor consists of three plates, and the design (splines with a diameter of about 2 mm on the plates) promotes turbulent flow of fluid across the plates, thus providing optimum heat transfer performance. For this reactor, its performance is characterized by a heat transfer coefficient (U) of 5,000 watts per cubic meter per degree Celsius. The coefficient U is tested as described above using water as the fluid. The total volume of the three plates arranged in series is 37.01 cm 3 , with a total exchange surface area of 0.074m 2 . The specific heat transfer coefficient (US / V) is therefore 8,020 kilowatts per cubic meter, per degree Celsius.
[0082] Any one of these plates is located between the other...
Embodiment 2
[0099] Embodiment 2: comparative experiment in batch reactor
[0100] For comparison, both reaction systems (choline / TBAOH) were tested in a jacketed glass stirred reactor. The reaction was carried out under batch conditions, the reactants were fed into the reactor, and the temperature of the heat transfer fluid flowing through the jacket was gradually increased from room temperature to 85°C (temperature ramp). Then, the temperature of the jacket was maintained at 85 °C until the end of the experiment.
[0101] 1- The characteristics of the reactor:
[0102] The inner diameter of the jacketed glass reactor was 0.08 m (8 cm). The volume of reactants fed to the reactor was about 0.3l (300ml), which represented a contact surface area with the wall of about 0.03m 2 . The heat transfer coefficient of glass in contact with organic solutions is usually given to be about 180W.m -2 .℃ -1。 . Therefore, the specific heat transfer coefficient (US / V) of the reactor is about 18 kilow...
Embodiment 3
[0112] Example 3.: Experiments on the Effect of Hydrolyzable Chlorine
[0113] As a comparison, a choline hydroxide catalytic system was tested in a jacketed glass stirred reactor with two HDI monomers with different levels of hydrolyzable chlorine (approximately 25 and 120 ppm expressed as chlorine) . The reaction was carried out under batch conditions, the monomer was charged into the reactor, and the temperature of the heat transfer fluid flowing through the jacket was raised to 85°C. The temperature of the jacket was then maintained at 85 °C until the end of the experiment. The catalytic solution (1.3% by weight of choline hydroxide in 2-ethylhexanol) was gradually introduced into the reaction medium by means of a syringe pump.
[0114] The reactor used was the same as in Example 2. The volume of reactants fed to the reactor is approximately 0.8 to 1 l (1,000 ml), which represents a contact surface area with the wall of approximately 0.04 to 0.05 m 2 . The heat transf...
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