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ChemicalBook CAS DataBase List Isobutyl acrylate

Isobutyl acrylate synthesis

7synthesis methods
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Yield:106-63-8 98.2 %

Reaction Conditions:

with dihydrogen hexachloroplatinate;10H-phenothiazine;2,6-di-tert-butyl-4-methyl-phenol in 2-methyl-propan-1-ol at 80; under 7500.75 Torr;Sealed tube;Inert atmosphere;Large scale;Reagent/catalyst;Temperature;

Steps:

2-3 Embodiment two

Add 410g of isobutanol, 99.5g of phenothiazine (0.5mol) and 41g of chloroplatinic acid (0.1mol) into a 1000ml flask equipped with stirring, and stir for 15 minutes to completely dissolve the phenothiazine and chloroplatinic acid in isobutanol In the process, a platinum complex catalyst was obtained and bottled for future use.Add 1447.2kg (20kmol) of acrylic acid with a content of 99.5%, 1.5kg of antioxidant BHT and the prepared platinum complexation After the addition, close the reaction kettle, replace the air in the reaction kettle with nitrogen for 3 times, add 1346.7kg (24kmol) of isobutene with a content of 99.8% into the reaction kettle, and fill the kettle with argon to a pressure of 1.0MPa, turn off the reactor and turn on the heating to raise the temperature of the material in the reactor to 80°C and keep it for 30 minutes. When it is observed that the material in the reactor is self-heating due to the exothermic reaction, remove the heat medium and slowly pour in cold water to control the cooling The water flow makes the temperature in the kettle rise slowly to 95~100°C. At this time, the pressure in the kettle is about 1.8MPa. Keep the temperature in the kettle at 95~100 for 10 hours. After the reaction, the pressure in the kettle drops to about 1.3MPa. Increase the cooling water to cool down the reactorWhen the temperature dropped to 50-55°C, the exhaust valve of the reaction kettle was opened to recover isobutene, and the reaction liquid in the kettle was de-rectified to obtain about 2526.6kg of isobutyl acrylate. The gas chromatography detection content was 99.6%, and the yield was 98.2% based on acrylic acid.

References:

CN115536527,2022,A Location in patent:Paragraph 0035-0038

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