Improved production method of unsaturated carboxylic ester
A production method and unsaturated technology, applied in the preparation of carboxylate, chemical instruments and methods, separation methods, etc., can solve the problems of polymer clogging, complex reaction zone, clogging of sieve plates, etc., and achieve high selectivity and simplified purification. Actionable, high-converting effects
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Embodiment 1
[0051] Example 1: Production of butyl acrylate
[0052] The equipment used in this embodiment is the equipment described with reference to the only drawing, except that there is no jacketed resin column 13 in front of the mixing tank 1. The tank 1 with thermostatic jacket 3 is stainless steel, and its effective volume is 700 ml. Jacket 3 adds 130°C oil. The stirrer 4 is of an anchor type. The inner diameter of the packed tower 6 is 22.5 mm, and the volume of the decanter is 50 ml.
[0053] The catalytic reactor 9 is composed of a jacketed stainless steel pipe, and the jacket is filled with 130°C oil; the reactor inner diameter is 30 mm and the height is 600 mm. It contains 134 grams of No. 1 resin, which has been pre-dried in a ventilated oven.
[0054] The whole equipment can be operated at low pressure.
[0055] The reactant AA (+inhibitor) + BuOH is 0.77 / 1 in terms of the AA / BuOH molar ratio, and is added to tank 1 at a flow rate of 270 ml / h. The above-mentioned inhibitor consi...
Embodiment 2
[0072] Example 2: Production of 2-ethylhexyl acrylate
[0073] The same equipment and the same resin as in Example 1 were used.
[0074] Based on the total amount of AA+E2HOH, it contains 500ppm 1,1,3-tris(2-methyl-4-hydroxy-5-tert-butylphenyl)butane (TOPANOL CA) and 500 ppm HQ of AA (81 g / h) and E2HOH (64 g / h) were continuously added to mixing tank 1. The temperature of tank 1 is 99°C.
[0075] In order to avoid the increase of AA, E2HOH (96 g / h) containing 500 ppm HQ was added at the top of the tower 6. The total molar ratio of AA / E2HOH is therefore 0.91 / 1.
[0076] The crude reaction product was recycled to the resin column 9 at a flow rate of 36 liters / g. The core temperature of the resin bed 9 is 95°C.
[0077] The water of reaction was removed as a water / E2HOH azeotrope that also contained AA and A2EH.
[0078] The steam condenses on the top and is decanted at room temperature.
[0079] The pressure at the top is 1.86×10 4 Pa (140 mmHg).
[0080] The decanted water phase w...
Embodiment 3
[0098] Example 3: Production of 2-ethylhexyl acrylate
[0099] Using the equipment of Example 1, the method of the tubular reactor 13 described in the sole figure was adopted.
[0100] Reactor 13 is a stainless steel jacketed-tube reactor with 130°C oil in the jacket. It contains 134 grams of resin No. 1 dried in a ventilated oven.
[0101] Reactant: Contains polymerization inhibitor (500ppm 1,1,3-tris(2-methyl-4-hydroxy-5-tert-butylphenyl)butane (TOPANOL) CA) and 500ppmHQ) AA are mixed with E2HOH, preheated to 90°C, and then added to the lower part of the catalytic reactor 13 with a pump at a flow rate of 615 ml / h. The initial AA / E2HOH molar ratio is 1.26.
[0102] The temperature at the inlet of column 13 is 90°C. The outlet temperature of column 13 is 95°C. The reaction does not need to move the balance. The passing direction of the reactants in the resin is upward. The residence time in the resin is 36 minutes.
[0103] The mass composition of the crude product at the outlet...
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