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A method for preparing 4-oxoisophorone by solid-liquid two-phase catalytic oxidation of β-isophorone

A technology for oxoisophorone and isophorone is applied in the field of solid-liquid two-phase catalytic oxidation of β-isophorone to prepare 4-oxoisophorone, which can solve the problem of not mentioning 4-oxoisophorone. Isophorone, long time, low conversion rate, etc., to achieve the effect of maintaining stable catalytic activity, mild reaction conditions, and environmental protection of the process route

Active Publication Date: 2021-04-20
WANHUA CHEM GRP CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

It takes a long time to directly oxidize α-IP to KIP, the conversion rate is not high, and the selectivity is low; while β-IP can be easily oxidized by oxygen to prepare KIP, but there will be a large amount of metal waste liquid in the catalytic oxidation of homogeneous catalysts. Formation, the catalyst is difficult to recycle, increasing the difficulty of disposal and the pressure of environmental protection costs
[0011] There is no mention of using gamma-alumina supported metal composite oxide as a catalyst to catalyze hydrogen peroxide to oxidize beta-isophorone in the current open literature to prepare 4-oxoisophorone

Method used

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  • A method for preparing 4-oxoisophorone by solid-liquid two-phase catalytic oxidation of β-isophorone
  • A method for preparing 4-oxoisophorone by solid-liquid two-phase catalytic oxidation of β-isophorone
  • A method for preparing 4-oxoisophorone by solid-liquid two-phase catalytic oxidation of β-isophorone

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0058] Preparation of catalyst:

[0059] Take a certain amount of Cu(NO 3 ) 2 ·H 2 O, Al(NO 3 ) 3 9H 2 O, Fe(NO 3 ) 3 9H 2 O, Co(NO 3 ) 3 ·6H 2 O, Mg(NO 3 ) 2 ·6H 2 O, anhydrous Na 2 CO 3 After dissolving in water, prepare 1mol / L standard aqueous solution respectively. Weigh 970mLNa 2 CO 3 Heat the aqueous solution to 70°C in a constant temperature water bath, mix 623mL aluminum nitrate aqueous solution with 19mL copper nitrate, 6.3mL cobalt nitrate, 2.1mL iron nitrate, 2.5mL magnesium nitrate aqueous solution, and slowly add it dropwise to Na 2 CO 3 in solution. During the dropping process, the temperature was controlled at 70±5°C. After the dropping was completed, the constant temperature stirring was continued for 40 minutes, and then the precipitate was poured into a beaker and aged for 24 hours at room temperature. After the precipitate was filtered, the precipitate was washed with deionized until the washing solution was neutral. Then, the filtered ...

Embodiment 2

[0063] Preparation of 4-oxoisophorone:

[0064] The catalyst obtained in Example 1 was washed and air-dried naturally, and used as the catalyst of Example 2.

[0065] A reactor equipped with a six-blade turbine high-speed stirring paddle is used as the reactor. Add 1380g of β-isophorone, 970g of ethanol, 1.38g of sodium carbonate, 13.8g of 1# catalyst, and 13.8g of azobisisobutylimidazoline hydrochloride successively in the reaction kettle; turn on electric heating and mechanical stirring, and react The liquid temperature was raised to 75°C, 2289g of 30% hydrogen peroxide solution was added dropwise for 6 hours, and the temperature was continued for 2 hours. After the reaction, gas chromatography analysis showed that the conversion rate of the raw material β-isophorone was 99.33%. The reaction liquid was filtered, and the catalyst was washed with ethanol, and the catalyst washing liquid was combined with the reaction liquid. After removing the solvent with a rotary evaporato...

Embodiment 3

[0067] Preparation of 4-oxoisophorone:

[0068] The catalyst obtained in Example 2 was washed and air-dried naturally, and used as the catalyst of Example 3.

[0069] A reactor equipped with a six-blade turbine high-speed stirring paddle is used as the reactor. Add 1380g of β-isophorone, 690g of methanol, 3.45g of potassium carbonate, 13.8g of 1# catalyst, and 34.5g of azobisisobutylimidazoline hydrochloride successively in the reaction kettle; turn on electric heating and mechanical stirring, and react The liquid temperature was raised to 60°C, 1387g of 50% hydrogen peroxide solution was added dropwise for 6 hours, and the temperature was continued for 2 hours. After the reaction, gas chromatography analysis showed that the conversion rate of the raw material β-isophorone was 99.25%. The reaction liquid was filtered, and the catalyst was washed with methanol, and the catalyst washing liquid was combined with the reaction liquid. After removing the solvent with a rotary evap...

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Abstract

The invention discloses a method for preparing 4-oxoisophorone by solid-liquid two-phase catalytic oxidation of β-isophorone. The method adopts γ-alumina supported metal composite oxide (CuO-Co 2 o 3 ‑Fe 2 o 3 ‑MgO / Al 2 o 3 ) as a catalyst. The method comprises the following steps: β-isophorone is oxidized with hydrogen peroxide in the presence of a solvent and a catalyst to prepare 4-oxoisophorone. The method has mild reaction conditions, simple process, high product yield, environmental protection, no waste liquid containing heavy metal elements, and can effectively solve the problem of non-recyclable catalyst preparation in the prior art.

Description

technical field [0001] The invention belongs to the technical field of chemical synthesis, and in particular relates to a method for preparing 4-oxoisophorone by solid-liquid two-phase catalytic oxidation of β-isophorone. Background technique [0002] 4-Oxoisophorone (KIP for short) is an important chemical intermediate product, which can be used not only in cosmetics and fragrances, but also in the synthesis of carotenoids and vitamins. Due to the importance of 4-oxoisophorone in chemical products, the synthesis of 4-oxoisophorone has been a research hotspot for a long time. [0003] At present, there are mainly two methods for synthesizing KIP commonly used, namely, oxidizing β-isophorone (abbreviated as β-IP) or α-isophorone (abbreviated as α-IP) to synthesize KIP. [0004] Patent US4046813 describes a method for preparing KIP by catalytic oxidation of β-isophorone using a vanadium, iron, cobalt, and manganese acetylacetonate complex in the presence of pyridine, although...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C45/28C07C49/603
CPCC07C45/28C07C2601/16C07C49/603Y02P20/584
Inventor 程晓波张涛郭劲资吕英东林龙朱龙龙王延斌张旭刘英瑞宋军伟李莉陈海波黎源华卫琦
Owner WANHUA CHEM GRP CO LTD
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