2-butylene-1,4-diol synthesis method
A diol and selectivity technology, applied in hydrogenation preparation and other directions, can solve the problems such as the lack of a method for separating products and recovering catalysts, poor selectivity of 1,4-butene diol, corrosion separation, etc., and the production process is mature. , the effect of improved operating conditions and low production costs
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Embodiment 1
[0022] Weigh 300g of butynediol aqueous solution and the Pd-C catalyst poisoned with lead, and put them into a 0.5L stainless steel autoclave. The amount of catalyst in the reactor is 1g (accounting for 0.3322% of the mass of the total reaction material), wherein the content of Pd is 0.0166%, and the content of Pb is 0.0100%. Replace the air in the kettle with nitrogen, then replace the nitrogen with hydrogen, and then raise the temperature to 35-45°C while stirring at a low speed (450-550 rpm). The reaction pressure is increased and maintained at 0.6-1.5 MPa, and the reaction is started. The reaction time is 330-390 minutes. After the reaction, the stirring was stopped, the hydrogen gas was stopped, the temperature was rapidly lowered, and the pressure was released. After replacing the unreacted hydrogen in the still with nitrogen, open the still and pour out the product, remove the catalyst by filtration and take a sample for analysis. The finally obtained raw material bu...
Embodiment 2
[0024] Except catalyst consumption 2g (accounting for 0.6623% of total reaction mass), wherein the content of Pd is 0.0331%, the content of Pb is 0.0199%, and the reaction time is 200-230 minutes, all the other process steps, material proportioning and reaction parameters are all the same In Example 1, when the concentration of butynediol in the final raw material is zero, the concentration of butynediol is too high. The product yield is 93.4-94.8%, and the raw material selectivity is 93.9-95.6%.
Embodiment 3
[0026] Except catalyst consumption 3 grams (accounting for 0.9901% of total reaction mass), wherein the content of Pd is 0.0495%, the content of Pb is 0.0297%, and the reaction time is 150-180 minutes, all the other process steps, material proportioning and reaction parameters are all Same as Example 1, when the butynediol concentration of the raw material finally obtained is zero, the butanediol concentration is relatively low. The product yield is 93.4-94.3%, and the raw material selectivity is 93.4-94.7%.
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