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A kind of method for preparing adipaldehyde

A technology of adipaldehyde and cyclohexene, which is applied in the field of preparation of adipaldehyde, can solve the problems of high price, excessive oxidation, and difficulty in obtaining high selectivity of adipaldehyde, and achieve the effect of high product selectivity and simple operation

Active Publication Date: 2021-06-22
DALIAN INST OF CHEM PHYSICS CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0007] In summary, in the preparation of adipaldehyde by cyclohexene oxidation, metal complexes-NaIO 4 Catalytic system, catalyst preparation method is complex and expensive
When using high-concentration hydrogen peroxide as an oxidant to oxidize cyclohexene, there is a problem of over-oxidation, and it is difficult to obtain high adipaldehyde selectivity, which hinders the further industrial application of this process

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1-10

[0065] The preparation of embodiment 1-10 supported type W, Mo catalyst

[0066] Firstly, the carrier was calcined at 550 °C for 4 h in a nitrogen atmosphere to remove species adsorbed in the pores. Dissolve a certain amount of ammonium tungstate and ammonium molybdate in water, and set the volume according to the saturated water absorption of the carrier (when using MCM-41, set the volume to 50 ml, when using SBA-15, set the volume to 30 ml, use medium When using porous silica, set the volume to 20 ml), take 10 g of the carrier and use the equal volume impregnation method to load the metal salt solution on the carrier, then place it in an oven at 100°C for 12 hours, and then bake it in a muffle furnace at 500°C for 4 hours. h to prepare the catalyst. The types and qualities of carriers and metal salts are shown in Table 1.

[0067] Table 1 Preparation parameters of catalysts

[0068] Example catalyst Ammonium tungstate mass (g) Ammonium molybdate mass (g) ...

Embodiment 11

[0070] Example 11 Oxidation of cyclohexene to adipaldehyde

[0071] In a 250mL round-bottomed flask, add 1.0 g of cyclohexene, 0.10 g of methyl pyruvate, 25 mL of acetonitrile, 0.5W-1.0Mo / MCM-41 catalyst (0.10 g), raise the temperature to 20 °C, and inject ozone with a concentration of The mixed gas of 100mg / L, described mixed gas is made up of ozone and oxygen, and described mixed gas flow rate is 80 mL / min, is down to room temperature rapidly after reacting 1h, and is formed with gas chromatograph analysis product.

Embodiment 12-20

[0072] Example 12-20 Cyclohexene oxidation to adipaldehyde

[0073] The cyclohexene oxidation reaction was carried out according to the same steps as in Example 11, and the specific differences and results of the reaction conditions are shown in Table 2.

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Abstract

The present application discloses a method for preparing adipaldehyde, the preparation method comprising: oxidizing a mixed solution containing cyclohexene and a mixed gas containing ozone under reaction conditions to obtain adipaldehyde; wherein, the The reaction conditions include using a supported metal oxide as a catalyst, and the metal oxide is composed of W oxide and Mo oxide. The present invention adopts supported W, Mo double metal oxide as catalyst, highly selective oxidation of cyclohexene to produce adipaldehyde, overcomes the shortcoming of using precious metal complexes and sodium periodate in cyclohexene oxidation reaction, the present invention Ozone is used as an oxidant to selectively oxidize cyclohexene to adipaldehyde with high product selectivity.

Description

technical field [0001] The application relates to a method for preparing adipaldehyde, which belongs to the field of chemistry and chemical engineering. Background technique [0002] 1,6-Adipaldehyde is an important fine chemical product. It is a quick-acting and broad-spectrum chemical sterilizer. It can not only kill most bacteria, bacterial propagules, fungi, spores and viruses quickly and efficiently, but also does not Corrosion of metal instruments and glass and plastic products, because it is harmless to the human body, it can be widely used in the disinfection and sterilization of medical equipment, food utensils, etc. In addition, adipaldehyde is also used in oil extraction, which can inhibit sulfate-reducing bacteria and increase the sulfur content of crude oil. In addition, as a cross-linking agent, 1,6-hexanedialdehyde has the characteristics of high activity, fast reaction, large binding capacity, stable product, and strong resistance to acid, water, and enzymes...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C45/40C07C47/12
CPCC07C45/40C07C2523/30C07C2529/03C07C47/12
Inventor 袁扬扬许磊陆标李沛东赵晓炜史鑫
Owner DALIAN INST OF CHEM PHYSICS CHINESE ACAD OF SCI
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