A kind of method that hexanediol is prepared by catalytic hydrogenation of hexynediol
A technology for catalytic hydrogenation and hexynediol, which is applied in the direction of catalyst activation/preparation, hydrogenation preparation, chemical instruments and methods, etc. It can solve problems such as unstable product quality, high catalyst consumption, troublesome post-processing, etc., and achieve improved catalyst performance. Utilization rate, high catalytic activity and selectivity, good product quality effect
Active Publication Date: 2021-10-29
DALIAN INST OF CHEM PHYSICS CHINESE ACAD OF SCI
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Problems solved by technology
Usually expensive Raney nickel catalyst is used, the reaction time is long, the amount of catalyst is high, the product quality is unstable, post-processing is troublesome, and the production cost is high
[0011] During the reaction process of catalytic hydrogenation of 2,5-dimethyl-3-hexyne-2,5-diol, the activity is likely to decrease due to the accumulation of polymer condensation polymers on the surface of the catalyst and other reasons, so the batch reaction is adopted in China 2,5-dimethyl-2,5-hexanediol is produced in small batches by the still hydrogenation process, and there are few reports on the production by the continuous flow fixed bed hydrogenation process
Method used
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Embodiment 1
[0026] Weigh 8.794g Ni(NO 3 ) 2 ·6H 2 O and 0.349g Ca(NO 3 ) 2 4H 2 O was added to 30ml of deionized water, and 10.0g of SiO was impregnated twice 2 Carrier, dry in the shade naturally, dry at 120°C for 12 hours, bake at 400°C for 6 hours, the prepared catalyst is 15%Ni-0.5%Ca / SiO 2 .
Embodiment 2
[0028] Weigh 16.74g Ni(NO 3 ) 2 ·6H 2 O and 0.514g Cu(NO 3 ) 2 ·3H 2 O was added to 30ml of deionized water, and 10.0g of SiO was impregnated twice 2 Carrier, dry in the shade naturally, dry at 120°C for 12 hours, bake at 400°C for 6 hours, the prepared catalyst is 25%Ni-1%Cu / SiO 2 .
Embodiment 3
[0030] Weigh 21.86g Ni(NO 3 ) 2 ·6H 2 O and 0.541g (NH 4 ) 6 Mo 7 o 24 4H 2 O was added to 30ml of deionized water, and 10.0g of SiO was impregnated three times 2 Carrier, dry in the shade naturally, dry at 120°C for 12 hours, bake at 400°C for 6 hours, the prepared catalyst is 30%Ni-2%Mo / SiO 2 .
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The invention relates to a method for preparing hexynediol by catalytic hydrogenation of hexynediol, specifically the technical field of preparation of 2,5-dimethyl-2,5-hexanediol, which is characterized in that it is pumped and filled in continuous flow After the fixed bed reactor is activated, the reaction raw material of the supported nickel-based catalyst bed layer is 5-40% of the 2,5-dimethyl-3-hexyne-2,5-diol aqueous solution and hydrogen, and the reaction The temperature is 60-120°C, the hydrogen pressure is 0.5-4.0MPa, and the liquid hourly space velocity is 1.0-10.0h ‑1 Under certain conditions, 2,5-dimethyl-3-hexyne-2,5-diol is efficiently converted into 2,5-dimethyl-2,5-hexanediol. The method for preparing 2,5-dimethyl-2,5-hexanediol provided by the invention uses water as a solvent to realize green catalysis and achieve the purpose of no pollution to the environment. The reaction condition is mild, the technological process is simple, the product quality is good, the catalyst performance is stable, and the catalyst is suitable for industrial production.
Description
technical field [0001] The invention belongs to the technical field of preparation of 2,5-dimethyl-2,5-hexanediol, specifically a preparation method of 2,5-dimethyl-3-hexyne-2,5-diol by catalytic hydrogenation 2,5-Dimethyl-2,5-hexanediol method. Background technique [0002] 2,5-Dimethyl-2,5-hexanediol is a widely used fine chemical, mainly used for the preparation of pyrethroids, spices, cyclic musk, polyethylene plastic crosslinking agent and silicone rubber double 2,5 The basic raw material of vulcanizing agent; it is also widely used in the intermediates of plastics, rubber, adhesives, organic peroxides and defoamers, etc. [0003] The industrial production of 2,5-dimethyl-2,5-hexanediol mostly uses acetylene and acetone as raw materials, and usually adopts atmospheric pressure acetylation or pressurized acetylation to obtain 2,5-dimethyl-3 -hexyne-2,5-diol, followed by hydrogenation to give 2,5-dimethyl-2,5-hexanediol. [0004] 1. Atmospheric pressure alkynylation me...
Claims
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IPC IPC(8): C07C31/20C07C29/17B01J23/78B01J23/755B01J23/883B01J23/83B01J23/80B01J29/03B01J29/46B01J37/02B01J37/08B01J37/18
CPCB01J23/755B01J23/78B01J23/80B01J23/83B01J23/883B01J29/0333B01J29/46B01J37/0201B01J37/088B01J37/18C07C29/172C07C31/20
Inventor 王涛丁云杰龚磊峰宁丽丽金明
Owner DALIAN INST OF CHEM PHYSICS CHINESE ACAD OF SCI