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Preparation method of benzaldehyde

A technology of benzaldehyde and cinnamaldehyde, which is applied in the field of benzaldehyde preparation, can solve the problems affecting the purity and yield of benzaldehyde, and achieve the effects of novel technology, direct and fast separation, and green reaction process

Inactive Publication Date: 2019-05-17
GUANGXI UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The reaction is an intermittent gas-liquid-solid three-phase reaction, and the water produced by the reaction will be enriched in the reactor, thereby affecting the purity and yield of benzaldehyde

Method used

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  • Preparation method of benzaldehyde

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preparation example Construction

[0023] The preparation method of above-mentioned a kind of benzaldehyde, the reaction in the described ozonation reaction unit and the dewatering operation of dewatering device are carried out simultaneously, and process is as follows:

[0024] The oxygen of described oxygen cylinder 16 enters in the ozone generator 19 from the outlet pipe through the oxygen inlet 20 of the first pressure gauge 17, rotameter 18 and ozone generator 19; Ozone outlet 21 passes into ozone by the air inlet 8 of air guiding device 1, and the outlet pipe of air outlet 9 is directly inserted in the tail gas absorption tank 22; Under the catalysis of the catalyst, the reaction generates benzaldehyde; the water generated in the reaction process is pushed by the pressure of the vacuum pump connected to the air inlet 13, and flows through the filter membrane 6 and the sand core filter platform 7 into the receiving bottle 4, so as to achieve water and organic Product separation.

Embodiment 1

[0026] Taking cinnamaldehyde as raw material, load the mixed solution of 20.0g cinnamaldehyde and dehydrated alcohol into the ozonation reactor, the mass ratio of cinnamaldehyde and dehydrated alcohol is 1: 4, add the CaO catalyst of 3.0wt%, in- At 10°C, 0.05 g of ozone was injected per gram of cinnamaldehyde per hour to carry out ozonation reaction for 0.5 h. While reacting, the reaction product is dehydrated through the NaA type zeolite molecular sieve membrane in the water removal device of the ozonation reaction device with a pressure of 0.001 MPa, and the natural benzaldehyde with a purity of more than 85% is obtained after molecular distillation, and the yield is 65%. .

Embodiment 2

[0028] Taking cinnamaldehyde as raw material, load the mixed solution of 20.0g cinnamaldehyde and dehydrated alcohol into the ozonation reactor, the mass ratio of cinnamaldehyde and dehydrated alcohol is 1: 4, add the CaO catalyst of 3.0wt%, in- At 10°C, 0.95g of ozone per hour per gram of cinnamaldehyde was introduced to carry out ozonation reaction for 12.0h. While reacting, the reaction product is dehydrated through the PVA organic membrane with a pressure of 1.0 MPa in the water removal device of the ozonation reaction device, and the natural benzaldehyde with a purity of more than 85% is obtained after molecular distillation, and the yield is 85%.

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Abstract

The invention discloses a preparation method of benzaldehyde. The preparation method comprises the steps that cinnamyl aldehyde serves as raw materials, a mixed solution of 20.0 g of cinnamyl aldehydeand absolute ethyl alcohol is loaded into an ozonization reactor, the mass ratio of the cinnamyl aldehyde to the absolute ethyl alcohol is 1:4, 3.0wt% of CaO is added as a catalyst, 0.05-0.95 g of ozone is introduced into per gram of cinnamyl aldehyde per hour at the temperature of minus 10 DEG C, and the ozonization reaction is conducted for 0.5-12.0 hours; while the reaction is conducted, a reaction product is subjected to membrane filter dehydration in a dewatering device of an ozonization reacting device at the pressure of 0.001-1.0 MPa through one of a PVA organic membrane, a NaA-type zeolite molecular sieve membrane, a T-type zeolite molecular sieve membrane, and a CHA-type zeolite molecular sieve membrane, thus the reaction is conducted in the forward direction, the high benzaldehyde yield is obtained, the obtained product is subjected to molecular distillation treatment, and then the natural benzaldehyde with the purity reaching 85% or above can be obtained. The preparation method has the advantages that the process is novel, operation is easy, the reaction process is environmentally friendly, the natural degree of the benzaldehyde is good, and the obtained benzaldehyde ishigh in purity and yield.

Description

technical field [0001] The invention belongs to the field of deep processing of forestry products, in particular to a preparation method of benzaldehyde. Background technique [0002] Since the 21st century, with the development of the economy and the improvement of living standards, consumers gradually tend to use safer and healthier natural food additives, thinking that "natural compounds are healthier than chemically synthesized ones". Benzaldehyde (Benzaldehyde), also known as benzoin aldehyde, has a special smell of bitter almonds. Natural benzaldehyde is often found in essential oils such as bitter almond oil, hyacinth oil, patchouli oil and ylang-ylang oil, and is also mainly present in the leaves, seeds or stem bark of plants in the form of glycosides. At the same time, benzaldehyde is also an important organic intermediate, which can be used in medicine, pesticide, fragrance and other industries. Although benzaldehyde is second only to vanillin, the world's most c...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C45/40C07C45/78C07C47/54
Inventor 罗轩王怡媛秦祖赠苏通明谢新玲纪红兵
Owner GUANGXI UNIV
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