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Method for increasing content of cis-dihydroterpilenol in terpilenol hydrogenation reaction

Pending Publication Date: 2021-04-27
厦门中坤化学有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] At present, there are few synthetic bibliographical reports of relevant dihydroterpineol, and the hydrogenation research of terpineol mostly concentrates on the research report to hydrogenation catalyst, hydrogenation process, mostly to improve dihydroterpineol yield, reduce For the purpose of cost, there is no report on increasing the content of cis-dihydroterpineol in the hydrogenation reaction of terpineol

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0031] 100g α-terpineol (95%), 3g ternary Raney nickel and 0.01g palladium carbon are placed in the autoclave, and the N 2 Replace it again, and then H 2 Replace three times, and then pass into H 2 , keep 1MPa, heat up to 90°C, stir at 400r / min, and react for 6h. After the reaction is finished, the temperature is lowered, the pressure is lowered, the kettle is opened and the material is discharged, and the catalyst is separated to obtain dihydro α-terpineol. The conversion rate of α-terpineol is 100%, the selectivity of dihydro α-terpineol is 99.9%, and the proportion of cis-dihydro α-terpineol in the product is 57.9%.

Embodiment 2

[0033] 100g α-terpineol (95%), 3g ternary Raney nickel and 0.03g palladium carbon are placed in the autoclave, first N 2 Replace it again, and then H 2 Replace three times, and then pass into H 2 , maintain 1MPa, raise the temperature to 75°C, raise the pressure to 3MPa, stir at 400r / min, and react for 4h. After the reaction is finished, the temperature is lowered, the pressure is lowered, the kettle is opened and the material is discharged, and the catalyst is separated to obtain dihydro α-terpineol. The conversion rate of α-terpineol is 100%, the selectivity of dihydro α-terpineol is 100%, and the proportion of cis-dihydro α-terpineol in the product reaches 80%.

Embodiment 3

[0035] Mix 100g of terpineol (among them, α-terpineol accounts for 64%, β-terpineol accounts for 11%, γ-terpineol accounts for 20%, 1-terpineol accounts for 2%), 3g terpineol Nickel and 0.02g ruthenium carbon are placed in the autoclave, first N 2 Replace it again, and then H 2 Replace three times, and then pass into H 2 , keep 1MPa, raise the temperature to 90°C, raise the pressure to 2MPa, stir at 400r / min, and react for 5h. After the reaction is finished, the temperature is lowered, the pressure is lowered, the kettle is opened for discharging, and the catalyst is separated to obtain a mixture of dihydroα-terpineol and dihydroβ-terpineol. The conversion rate of mixed terpineol is 99.8%, the selectivity of dihydroterpineol is 99.6%, and the proportion of cis-dihydroterpineol in the product is 62.0%.

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PUM

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Abstract

A method for increasing the content of cis-dihydroterpilenol in a terpilenol hydrogenation reaction relates to the field of chemical product preparation, and comprises the following steps of: (1) putting raw materials terpilenol and ternary raney nickel, a catalyst and an auxiliary agent into a high-pressure reaction kettle; (2) replacing the high-pressure reaction kettle with N2 and H2 in sequence, introducing H2 into the high-pressure kettle after replacement is completed, and controlling the pressure; and (3) controlling the reaction temperature and the reaction pressure, and carrying out a reaction for a certain time to obtain the product. The catalyst and the auxiliary agent provided by the invention have very high reaction activity on reaction and very high selectivity on dihydroterpilenol, and the content of cis-dihydroterpilenol in the product can be adjusted according to specific requirements.

Description

technical field [0001] The invention relates to the technical field of chemical product preparation, in particular to a method for increasing the content of cis-dihydroterpineol in the hydrogenation reaction of terpineol. Background technique [0002] Dihydroterpineol, also known as hydrogenated terpineol, has several isomers and is a colorless oily liquid with a wide range of uses. Dihydroterpineol has a sweet and pleasant lilac aroma, and the fragrance is long-lasting. It is a good raw material for blending flavors; at the same time, Dihydroterpineol is also an excellent solvent, which is widely used in the electronics industry, coating industry and chemical industry. Wait. [0003] At present, there are few synthetic bibliographical reports of relevant dihydroterpineol, and the hydrogenation research of terpineol mostly concentrates on the research report to hydrogenation catalyst, hydrogenation process, mostly to improve dihydroterpineol yield, reduce For the purpose o...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C29/17C07C31/135
CPCC07C29/172C07C2601/14C07B2200/09C07C31/1355
Inventor 谢世祎刘文通王彩明张玉蓉刘尧权杨毅融
Owner 厦门中坤化学有限公司