A method for preparing 3-methylthiopropanol by catalytic hydrogenation
A technology for the catalytic hydrogenation of methylthiopropanol, which is applied in the chemical industry, can solve the problems of complex preparation process, dangerous raw materials, high equipment and operation requirements, and achieve clean and simple reaction raw materials, easy-to-operate and controllable reaction conditions, and easy operation and low equipment requirements
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Embodiment 1
[0029] Example 1 Preparation of ultrafine amorphous catalyst (CoFeB)
[0030] 1 mol of analytically pure dark red cobalt acetate and 0.01 to 0.3 mol of ferric chloride were dissolved in 2.5 times the volume of ethanol, and stirred vigorously at 20 to 30°C until all of them were dissolved to obtain a brown-red clear solution. Slow down the stirring, start the ultrasonic wave to cover the reaction liquid under the ultrasonic atmosphere, the ultrasonic frequency is 20~40Hz, and at the same time, use a peristaltic pump to drip fresh 2mol / L potassium borohydride into the reaction liquid at a flow rate of 1~3ml / min. A large amount of hydrogen gas bubbles and black solid powder precipitated out of the solution at the same time, continue to slowly add potassium borohydride until the dripping is complete, continue to stir and react under ultrasonic atmosphere for 10 to 30 minutes, after the reaction is completed, suction filtration, repeated washing with deionized water to remove The salt...
Embodiment 2
[0032] Example 2 Mixed alcohol ratio experiment (ethanol:glycerol=6:1)
[0033] 1 mol of 3-methylthiopropionaldehyde with a purity greater than 99% and a monomer content greater than 95% is added to a mixed solution of ethanol and glycerin to prepare a 3-methylthiopropionaldehyde mixed alcohol solution with a concentration of 10 to 90% by weight. Ethanol in mixed alcohol solution: glycerol = 6:1. The mixed solution was transferred to the reactor, and the ultrafine amorphous CoFeB catalyst prepared in Example 1 was added with 1 to 30 wt% relative to the raw material, stirred at 40 to 50°C and injected with hydrogen at a pressure of 1 to 3Mpa for reaction for 30 to 180 minutes. At the end of the reaction, the reaction solution was transferred out under reduced pressure distillation, ethanol and 3-methylthiopropanol were recovered respectively, and glycerin was transferred out directly from the bottom of the kettle. The 3-methylthiopropanol with a purity of more than 99% is obtaine...
Embodiment 3
[0035] Example 3 Mixed alcohol ratio experiment (ethanol:glycerol=4:1)
[0036] 1 mol of 3-methylthiopropionaldehyde with a purity greater than 99% and a monomer content greater than 95% is added to a mixed solution of ethanol and glycerin to prepare a 3-methylthiopropionaldehyde mixed alcohol solution with a concentration of 10 to 90% by weight. . Ethanol in mixed alcohol solution: glycerol = 4:1. The mixed solution was transferred to the reactor, and the ultrafine amorphous CoFeB catalyst prepared in Example 1 was added with 1 to 30 wt% relative to the raw material, stirred at 40 to 50°C and injected with hydrogen at a pressure of 1 to 3Mpa for reaction for 30 to 180 minutes. At the end of the reaction, the reaction solution was transferred out under reduced pressure distillation, ethanol and 3-methylthiopropanol were recovered respectively, and glycerin was transferred out directly from the bottom of the kettle. The 3-methylthiopropanol with a purity of more than 99% is obta...
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