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Preparation method of natural benzaldehyde by ozone collaborative heterogeneous catalysis of cinnamaldehyde or cinnamon oil

A technology of benzaldehyde and cinnamon oil is applied in the directions of ozone decomposition preparation, chemical instruments and methods, metal/metal oxide/metal hydroxide catalyst, etc. It can solve the problems of difficult contact with materials, etc., to achieve the effect of high reusability, good selectivity and yield, and high utilization rate.

Active Publication Date: 2016-05-25
广西庚源香料有限责任公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The main shortcoming that this method exists is: cinnamaldehyde and water are mutually immiscible, cause the reactants to be difficult to contact, finally cause the yield of benzaldehyde to reduce greatly
However, the single-component oxide catalyst is susceptible to H in the air 2 O.CO 2 impact, and poor reusability

Method used

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  • Preparation method of natural benzaldehyde by ozone collaborative heterogeneous catalysis of cinnamaldehyde or cinnamon oil

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0022] Take by weighing 16.86g of barium nitrate and 18.25g of tin chloride dihydrate and dissolve them in deionized water to make a solution with a concentration of 0.2mol / L; similarly, take 32.39g of ammonium bicarbonate and dissolve them in deionized water to make A solution with a concentration of 0.4mol / L. At a water bath temperature of 40°C and a speed of 300 rpm, the barium nitrate and tin chloride solutions prepared above were added dropwise to the ammonium bicarbonate solution by co-current co-precipitation method, and the solution changed from clear to turbid. When the temperature is 7 to 8, stop adding the metal salt solution dropwise, wait for the precipitate to age in the mother liquor at a constant temperature of 40° C. for 10 hours, and then carry out suction filtration to obtain the precipitate. The obtained precipitate was dried at 90°C for 12h, and calcined at 950°C for 2h to obtain the BaO / SnO catalyst. In the bubbling reactor, add 4.91g cinnamaldehyde (the...

Embodiment 2

[0024] Take by weighing 17.86g nickel nitrate hexahydrate, 18.97g tin chloride dihydrate and be dissolved in deionized water respectively, be made into the solution that concentration is 0.2mol / L; Similarly, take by weighing 24.59g ammonium bicarbonate and dissolve in deionized water, Dubbed a solution with a concentration of 0.4mol / L. At a water bath temperature of 40°C and a speed of 300 rpm, the nickel nitrate and tin chloride solutions prepared above were added dropwise to the ammonium bicarbonate solution by co-current co-precipitation method, and the solution changed from clear to turbid. When the temperature is 7-8, stop adding the metal salt solution dropwise, wait for the precipitate to age in the mother liquor at a constant temperature of 40° C. for 6 hours, and then carry out suction filtration to obtain the precipitate. The obtained precipitate was dried at 90°C for 12h and calcined at 600°C for 4h to obtain the NiO / SnO catalyst. In the bubble reactor, add 5.06g o...

Embodiment 3

[0026] Take by weighing 18.26g tin chloride dihydrate, 19.82g lanthanum nitrate hexahydrate and be dissolved in deionized water respectively, be made into the solution that concentration is 0.05mol / L; Similarly, take by weighing 22.39g ammonium bicarbonate and dissolve in deionized water, Dubbed a solution with a concentration of 0.3mol / L. At a water bath temperature of 40°C and a rotational speed of 300 rpm, the above-prepared lanthanum nitrate and tin chloride solutions were added dropwise to the ammonium bicarbonate solution by co-current co-precipitation method, and the solution changed from clear to turbid. When the temperature is 7 to 8, stop adding the metal salt solution dropwise, wait for the precipitate to age in the mother liquor at a constant temperature of 40°C for 2 hours, and then carry out suction filtration to obtain the precipitate. The obtained precipitate was dried at 90°C for 20h, and calcined at 700°C for 5h to obtain La 2 o 3 / SnO catalyst. In the bub...

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Abstract

The invention discloses a preparation method of natural benzaldehyde by ozone collaborative heterogeneous catalysis of cinnamaldehyde or cinnamon oil. The method is as below: adding 0.5%-10% of aNiO, BaO, MgO, La2O3, SnO2 binary or ternary oxide component catalyst into a raw material cinnamic aldehyde or cinnamon oil, introducing ozone in a bubble reactor under conditions of atmospheric pressure temperature of -10 to 30 DEG C and flow rate of 0.1-5 g / L, and reacting at low temperature for 1-8 h to obtain a benzaldehyde crude product; and finally, using a molecular distillation apparatus to obtain high-purity natural benzaldehyde. The invention has the advantages of simple process, convenient operation, no toxicity or harm of the catalyst, environment-friendliness; the cinnamaldehyde is fully utilized; and the benzaldehyde has good selectivity, high yield, and natural degree intact.

Description

technical field [0001] The invention relates to a method for preparing natural benzaldehyde through ozone synergistic heterogeneous catalysis of cinnamaldehyde or cinnamon oil, belonging to the field of heterogeneous catalysis. Background technique [0002] Natural benzaldehyde, colorless or pale yellow transparent liquid, smells of bitter almonds, and is commonly known as bitter almond oil, benzoin aldehyde, benzaldehyde, is the most simple and industrially important aromatic aldehyde. It is mainly used as an intermediate or raw material in the manufacture of dyes, medicines, spices, seasonings and pesticides. [0003] With the improvement of living standards, people are more inclined to use safer and healthier natural food additives. The demand for natural benzaldehyde is increasing day by day, and it is one of the commodities in short supply in the world; at the same time, natural flavors usually have good economic value and obvious market competitiveness. Guangxi is ri...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C45/40C07C47/54B01J23/14B01J23/835B01J23/02
CPCB01J23/02B01J23/14B01J23/835C07C45/40C07C47/54
Inventor 秦祖赠吴坚锋蒋月秀纪红兵
Owner 广西庚源香料有限责任公司
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