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ChemicalBook CAS DataBase List 1,2-BUTADIENE
590-19-2

1,2-BUTADIENE synthesis

12synthesis methods
-

Yield:-

Reaction Conditions:

with silica gel;potassium hydroxide at 501 - 609; under 750.075 Torr;Inert atmosphere;

Steps:

16 Dehydration Reaction
The reaction tube filled with the catalyst was 15 heated in an electric furnace and the temperature of the reaction tube was raised while feeding a nitrogen gas at a rate of 189 mL/min from an inlet of the reaction tube through reaction the tube. Next, 2-butanone (a compound in which, in the 20 formula (II), R , 5 R , 6 R , 7 R 8 and R 9 are hydrogen atom) (manufactured by Wako Pure Chemical Industries, Ltd.) was charged in a gas absorbing bottle and cooled to 0°C; then into the gas absorbing bottle, a nitrogen gas was fed at rate a of 189 mL/min to make a nitrogen 25 gas stream in 2-butanone; the obtained nitrogen gas 91 accompanied with 2-butanone was fed from the reaction tube inlet instead of the feeding nitrogen gas at the time of temperature rise (2-butanone feed rate:0.017 mol/h, 2-butanone concentration in the feeding 5 gas:3.2% by volume) to start the reaction at reaction a pressure of 0.1 MPa. The ratio (GHSV) of the total gas flow rate with respect to the catalyst volume was 1,747 h-i. After the start of reaction, temperature the of the 10 catalyst layer was maintained at 550°C ± 3°C. After 60 minutes of the reaction start time, a gas from an outlet of the reactor was collected in a Tedlar bag and analyzed with gas chromatograph equipped with TCD and FID detectors to determine the amount of each 15 product. Once the sampling was completed, next, 2butanone and high boiling components were absorbed using a two stage trap including acetonitrile. Each absorption liquid the in first stage trap and the second stage trap was analyzed with a gas chromatograph 20 equipped with a FID detector to determine the amounts of 2-butanone and high boiling components.

References:

Sumitomo Chemical Co Ltd;MIURA, NAOKI;SEKI, KOHEI;YOSHIMURA, KAZUAKI CN104093682, 2016, B Location in patent:Paragraph 0427; 0428; 0437-0445

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