2-Methyl-3-Butyn-2-ol CAS 115-19-5

Preparation of reaction solution

First, replace the 500L autoclave with ammonia gas three times, lower the temperature in the reactor to -20°C, add liquid ammonia (144.5Kg, 8500mol), start stirring, and feed acetylene (16800L, 750mol) at a concentration of 20wt%. Magnesium sulfate aqueous solution 43.5g and concentration are 50wt% potassium hydroxide aqueous solution (1008g, the potassium hydroxide consumption as solute is 3mol% of acetone), be warming up to 10 ℃ and add acetone (17.4Kg, 300mol), control acetone to add The feed rate is completed in about 1h; the reaction temperature is 10°C, after 2h of reaction, add 5Kg of 10wt% ammonium sulfate aqueous solution for neutralization, and obtain 1# reaction solution containing 3-methylbutynol-3, and take a sample The reaction solution was checked by GC.

The composition of 1# reaction solution: the content of inorganic salt is 2.16wt%, the content of water is 16.61wt%, the content of 3-methylbutynol-3 is 77.30wt%, the content of acetone is 3.56wt%, 2, The content of 5-dimethyl-3-hexyne-2,5-diol is 0.05wt%, and the content of other components is 0.32wt%, based on the total weight of the components of the 1# reaction solution as 100wt%.

Immobilization of 1-butyl-3-methylimidazolium hydroxide basic ionic liquid by COF-108 bond method

10.0 g of catalyst carrier COF-108 and 4.11 g of N-methylimidazole were refluxed in toluene for 24 hours. After the reaction mixture was cooled to room temperature, it was filtered, washed with toluene, 0.1mol/L hydrochloric acid, water and methanol, and dried under reduced pressure to obtain the immobilized ionic liquid [Bmim][Cl]/COF-108, 15.88g[ Bmim][Cl]/COF-108 and 2.8g of solid potassium hydroxide were dispersed in 100ml of water, stirred vigorously at 600 r/min at room temperature for 24 hours, then the mixture was filtered, washed with water until neutral, and dried under reduced pressure to obtain a solid Supported basic ionic liquid [Bmim][OH]/COF-108. It is prepared as a filler with a particle size of Φ1×(1-2)mm.

Take 1000g of the above-mentioned catalyst and fill it in a Φ20mm×20m stainless steel tubular reactor with an acetylene distributor inside. Under normal pressure, feed the raw material acetone into the reactor equipped with catalyst, the molar ratio of acetylene to acetone is 1.1:1.0, the reaction temperature is 60°C, the flow rate of acetone in the reactor is 0.5m/min, and the reaction time is 40min. After the reaction, the reaction liquid is sent to the degassing tower, separated at 0.5MPa, and all the acetylene is extracted from the top of the tower, and then re-enters the reactor through the pipeline. The reaction liquid enters the acetonization tower, and the acetone is removed by rectification under normal pressure. The acetone recovered from the top of the tower is recycled, and the crude methyl butynol is obtained from the tower reactor, which is sent to the acetylenic alcohol tower for further separation to obtain the final product of methyl butynol. The liquid product was detected and analyzed by gas chromatography, the conversion rate was 99.65%, the selectivity was 99.95%, the purity of the methyl butynol product was 99.60%, and the product yield in terms of acetone was 99.60% (mass yield).

The catalyst was operated for a long period. After 2000 hours, the conversion rate was 98.56%, the selectivity was 99.12%, the product purity of methyl butynol was 99.95%, and the product yield was 97.69% based on acetone.