Catalyst and method for preparing beta-phenylethanol by using same

A catalyst and silica technology, applied in chemical instruments and methods, physical/chemical process catalysts, hydrolysis preparation, etc., can solve the problems of poor catalyst structure and performance, shortened catalyst life, complicated separation process, etc., and achieve simplified products. The effect of separation process, reduction of gas-liquid ratio, and reduction of circulating hydrogen

Active Publication Date: 2019-06-07
WANHUA CHEM GRP CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The β-phenylethanol preparation processes proposed by patents CN1111169A, US6979753, US4943667, US2524096, etc. all require the use of solvents, which reduces production efficiency, complicates the product separation process, and increases the cost of solvent removal, etc.
[0006] To sum up, the existing technologies all have certain deficiencies to varying degrees. If additives need to be added to improve selectivity, but at the same time cause problems such as reduced catalyst life, difficult product separation, and even affect product quality; such as catalyst structure and Poor performance, which leads to easy deactivation of the catalyst and short catalyst life; if a solvent is required due to the heat transfer limitation of the reactor, the separation cost is increased

Method used

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  • Catalyst and method for preparing beta-phenylethanol by using same
  • Catalyst and method for preparing beta-phenylethanol by using same

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0046] Add 54ml ammonia water (concentration 25wt%) into 150ml deionized water, then add a volume of 48ml ethyl orthosilicate absolute ethanol solution (concentration 50wt%), stir at 35℃ for 4h to obtain a silica microsphere solution. The silica microsphere solution was filtered by centrifugation and washed with ethanol and deionized water for 3 times to obtain silica microspheres (6.3g). The obtained silica microspheres were dispersed in deionized water for later use (solid content 9.5% by weight) ).

[0047] Add 14.52g copper nitrate, 104.4g nickel nitrate and 78ml ammonia water (concentration 25wt%) into 1200ml deionized water, add dropwise a volume of 360ml silica microsphere aqueous solution (solid content 9.5% by weight) under stirring, at 45℃ Stir for 2.5h under conditions, then incubate at 150℃ for 3h, then centrifuge and filter, wash with deionized water until the washing liquid PH=7, filter the product under 0.05KpaA, 60℃, vacuum drying for 12h, and then at 450℃ , Calc...

Embodiment 2

[0050] Add 90ml ammonia water (concentration 25wt%) into 210ml deionized water, and then add 72ml methyl orthosilicate absolute ethanol solution (concentration 55wt%), stir at 55℃ for 1h to obtain silica microsphere solution. The silica microsphere solution was filtered by centrifugation and washed with ethanol and deionized water three times to obtain 10.4 g of silica microspheres. The obtained silica microspheres were dispersed in deionized water (solid content 12wt%) for later use.

[0051] Add 30.99g copper acetate, 202.1g nickel acetate and 60ml ammonia water (concentration 25wt%) into 900ml deionized water, add dropwise a volume of 270ml silica microsphere aqueous solution (solid content 12wt%) under stirring, at 60℃. After stirring for 2h, then incubating at 120℃ for 36h, then centrifugal filtration, washing with deionized water to pH=7, the filtered product was vacuum dried at 1KpaA, 75℃ for 8h, and then at 550℃, air atmosphere It is calcined under conditions for 3h, and ...

Embodiment 3

[0054] Add 30ml ammonia water (concentration 28wt%) into 90ml deionized water, then add 36ml methyl orthosilicate absolute ethanol solution (concentration 45wt%), stir at 45°C for 3h to obtain a silica microsphere solution. The silica microsphere solution was centrifuged and filtered, and washed with ethanol and deionized water three times to obtain 4.3 g of silica microspheres. The obtained silica microspheres were dispersed in deionized water (solid content 8.2 wt%) for later use.

[0055] Add 14.87g copper chloride, 123.4g nickel chloride and 90ml ammonia water (concentration 28wt%) into 1800ml deionized water, and add 480ml of silica microsphere aqueous solution (solid content 12wt%) dropwise under stirring. Stir at ℃ for 3h, then incubate at 135℃ for 18h, then centrifuge and filter, wash with deionized water to wash pH=7, filter the product under 2KpaA, vacuum drying at 90℃ for 4h, then at 350℃, It is calcined in air atmosphere for 6 hours, and finally compressed, crushed an...

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Abstract

The invention discloses a catalyst and a method for preparing beta-phenylethanol by the catalyst. The catalyst is a nickel-copper silicate composite echinus-shaped reactor type nanocatalyst. Accordingto the catalyst, the problem that the content of a byproduct, i.e., ethylbenzene is high due to the fact that a hydrogenation reaction speed of styrene oxide is too high and the supply of hydrogen isinsufficient is solved, the beta-phenylethanol can be prepared from the styrene oxide under mild conditions through high-selectivity and high-yield hydrogenation, the conversion ratio of the styreneoxide is higher than 99%, the selectivity of the beta-phenylethanol is not lower than 99.5%; and due to sufficient hydrogen supply, the high selectivity of the product can also be guaranteed under thecondition that hydrogenation of the styrene oxide is carried out in the absence of auxiliaries, the procedure of removing the auxiliaries is avoided, and product separating flows are simplified. Themethod for preparing the beta-phenylethanol can achieve continuous production of the beta-phenylethanol, and the production efficiency is increased greatly.

Description

Technical field [0001] The invention relates to a catalyst for the hydrogenation of styrene oxide to prepare β-phenylethanol, in particular to a nickel silicate-copper composite sea urchin-like nano-reactor type catalyst, and a method for preparing β-phenylethanol using the catalyst. Background technique [0002] β-Phenylethanol (PEA), also known as 2-phenylethyl alcohol, phenylethyl alcohol, and ethyl phenylethyl alcohol, is a simple primary aromatic alcohol. It is a colorless liquid at room temperature and has a delicate, delicate and long lasting rose aroma. It was first discovered as a characteristic aroma compound in plant flowers and naturally exists in neroli oil, rose oil, geraniol oil and other aromatic oils. [0003] β-Phenylethanol is widely used in various edible flavors and tobacco flavors because of its soft, pleasant and long lasting rose aroma. It is the main raw material for the preparation of rose-flavored food additives and rose-flavored flavors. The use of β-ph...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J23/755C07C29/10C07C33/22B01J35/02
Inventor 曾伟王明永王磊黎源杨恒东赵欣王展宋延方杨洋陈永
Owner WANHUA CHEM GRP CO LTD
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