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Titanium-salt-modified Raney nickel catalyst and method for synthesizing dihydroterpineol

A technology of dihydroterpineol and Raney nickel, which is applied in Raney-type catalysts, chemical instruments and methods, physical/chemical process catalysts, etc. There are many problems such as reactions, and the effect of eliminating the rectification and purification process, the process is simple, and the probability of occurrence is reduced.

Active Publication Date: 2015-05-13
江西创赢香精香料科技协同创新有限公司 +2
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0008] The above hydrogenation reactions use Raney nickel as a catalyst, and most of them are carried out at relatively high temperature and pressure. Terpineol is easy to dehydrate, with many side reactions, and the unit consumption of terpineol is relatively high.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0025] 2100 kg of terpineol and 126 kg of titanium salt-modified Raney nickel catalyst were placed in a 3-ton high-pressure reactor. Vacuum the autoclave to 1-3Kpa, keep it for 30min, then fill it with hydrogen to 1.2Mpa, keep it for 10min;

[0026] After observing that there is no change in the value of the pressure gauge on the high-pressure reactor, the temperature was raised to 80°C, the pressure was raised to 3.5Mpa, the stirring speed was 300 r / min, and the reaction was carried out for 4 hours. After the pressure in the autoclave remains unchanged, turn off the hydrogen source, lower the temperature of the material in the autoclave to room temperature, open the vent valve, and reduce the pressure in the autoclave to normal pressure. Dihydroterpineol was obtained by filtration after standing for the first time, with a selectivity of 98.7% and a yield of 98.6%.

Embodiment 2

[0028] 2100 kg of terpineol and 65 kg of titanium salt-modified Raney nickel catalyst were placed in a 3-ton high-pressure reactor. Vacuum the autoclave to 1-3Kpa, keep it for 30 minutes and then fill it with hydrogen to 1.2Mpa. After observing that there is no change in the value of the pressure gauge on the high-pressure reactor, the temperature was raised to 75°C, the pressure was raised to 3.0Mpa, stirred at 200 r / min, and reacted for 5 hours. After the pressure in the autoclave remains unchanged, turn off the hydrogen source, lower the temperature of the material in the autoclave to room temperature, open the vent valve, and reduce the pressure in the autoclave to normal pressure. Dihydroterpineol was obtained by filtration after standing for the first time, with a selectivity of 98.2% and a yield of 98.0%.

Embodiment 3

[0030] 100 kg of nickel-aluminum alloy with a mass percentage of nickel of 55% was crushed to 100 mesh, stirred and treated with 600 kg of 30% sodium hydroxide solution for 1.5 hours at a temperature of 65°C, and washed with deionized water to obtain Raney nickel. Then soak the Raney nickel in 500 kg of 2.5 g / L titanium salt solution at 50°C for 24 hours, wash with deionized water and absolute ethanol respectively, and store in absolute ethanol.

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Abstract

The invention discloses a titanium-salt-modified Raney nickel catalyst and a method for synthesizing dihydroterpineol. A preparation method of the titanium-salt-modified Raney nickel catalyst comprises steps as follows: a nickel aluminium alloy with the mass percentage of nickel ranging from 40% to 65% is crushed to be at 60-120 meshes and subjected to stirring treatment by the aid of a 20%-35% sodium hydroxide solution at the temperature of 40-80 DEG C for 1-2 h, Raney nickel is obtained after washing with deionized water, and then the Raney nickel is modified with a titanium salt solution, washed with the deionized water and absolute ethyl alcohol respectively finally and stored in the absolute ethyl alcohol. The Raney nickel is used as a hydrogenation catalyst for terpilenol during synthesis, reaction conditions are mild, the occurrence probability of side reactions can be decreased, the selectivity of the dihydroterpineol is higher than 98%, the yield ranges from 98.0% to 98.6%, the purity is high, and the dihydroterpineol can be directly sold as a product after subjected to solid-liquid separation treatment together with the catalyst, so that the production efficiency is high, and the cost is low.

Description

technical field [0001] The invention belongs to the technical field of fine chemicals, and relates to a method for preparing spices, in particular to a titanium salt-modified Raney nickel catalyst and a method for synthesizing dihydroterpineol. Background technique [0002] Dihydroterpineol has an elegant lilac fragrance, long-lasting fragrance, stable structure, and the fragrance does not change when the temperature reaches 200 ° C. It is a good performance raw material for blending lilac essence. It is used in soap and synthetic detergent essence. The medium dosage can be 20%. Compared with terpineol, dihydroterpineol has more woody aroma. It is suitable for the fragrance of heavy-duty detergents. It has stable performance and is widely used in the deployment of daily chemical essence. At the same time, dihydroterpineol is also a good solvent for the production of hydrogen peroxide by anthraquinone method. Dihydroterpineol is usually prepared by catalytic hydrogenation wi...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J25/02C07C31/135C07C29/17
Inventor 任向荣周作良俞忠华
Owner 江西创赢香精香料科技协同创新有限公司
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