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Method for manufacturing catalyst used for synthesizing benzaldehyde

A technology of catalyst and benzaldehyde, which is applied in the direction of chemical instruments and methods, organic compound/hydride/coordination complex catalyst, oxidation to prepare carbonyl compounds, etc., can solve the problem of low benzaldehyde conversion rate of benzyl alcohol, energy consumption, Serious material consumption and other problems, to achieve the effect of good reusability, low cost and high conversion rate

Inactive Publication Date: 2008-01-23
SHANXI INST OF COAL CHEM CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, heterogeneous catalysts such as titanium-silicon molecular sieves and alum-silicon molecular sieves commonly used at present all have the disadvantages of benzyl alcohol conversion rate and benzaldehyde selectivity lower (conversion rate<20%; selectivity<60%)
Therefore, it is necessary to purify the product and oxidize the reactant multiple times to meet the requirements of industrial production, and the energy consumption and material consumption are relatively serious.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0018] Add 5.0g of aminopropyltrimethoxysilane to 50g of cyclohexane to form a solution, stir evenly, add 3.0g of silica gel to it, heat to reflux for 8h, cool and filter with suction, extract the solid sample with toluene for 8h, 80℃ Dry under vacuum for 8h to obtain NH 2 / SiO 2 . Then, 25 g of absolute ethanol solution in which 0.55 g of o-phenylenediamine was dissolved was added dropwise to 25 g of absolute ethanol liquid in which 1.2 g of salicylaldehyde was dissolved, and refluxed at 80° C. for 1 hour, then 1.5 g of chromium chloride was added, and continued Stir and reflux for 3h, cool and filter with suction to obtain Cr(salphen). 1gNH 2 / SiO 2 Add 0.5g Cr(salphen) into 50g cyclohexane, stir and reflux for 8h, cool, filter with suction, extract the solid sample with toluene for 8h, and dry it in vacuum at 80°C for 8h to obtain the catalyst for this reaction. Add benzyl alcohol, hydrogen peroxide and catalyst into a 75mL autoclave, the molar ratio of benzyl alcohol ...

Embodiment 2

[0020] Add 5.0g of aminopropyltrimethoxysilane to 80g of cyclohexane to form a solution, stir evenly, add 3.3g of silica gel to it, heat to reflux for 9h, cool and filter with suction, extract the solid sample with toluene for 9h, 80℃ Dry under vacuum for 9h to obtain NH 2 / SiO 2 . Then, 30 g of absolute ethanol solution in which 0.55 g of o-phenylenediamine was dissolved was added dropwise to 30 g of absolute ethanol liquid in which 1.2 g of salicylaldehyde was dissolved, and refluxed at 80° C. for 2 hours, then 1.5 g of chromium chloride was added, and continued Stir and reflux for 3h, cool and filter with suction to obtain Cr(salphen). 1g NH 2 / SiO 2 Add 0.5g Cr(salphen) into 60g cyclohexane, stir and reflux for 9h, cool, filter with suction, extract the solid sample with toluene for 10h, and dry it in vacuum at 80°C for 10h to obtain the catalyst for this reaction. Add benzyl alcohol, hydrogen peroxide and catalyst into a 75mL autoclave, the molar ratio of benzyl alco...

Embodiment 3

[0023] Add 5.0g of aminopropyltrimethoxysilane to 100g of cyclohexane to form a solution, stir evenly, add 3.7g of silica gel to it, heat to reflux for 10h, cool, filter with suction, and extract the solid sample with toluene for 10h, 100℃ Dry under vacuum for 10h to obtain NH 2 / SiO 2 . Then, 40 g of absolute ethanol solution in which 0.55 g of o-phenylenediamine was dissolved was added dropwise to 40 g of absolute ethanol liquid in which 1.2 g of salicylaldehyde was dissolved, refluxed at 80° C. for 3 hours, and then 1.7 g of chromium chloride was added, and continued Stir and reflux for 6h, cool and filter with suction to obtain Cr(salphen). 1g NH 2 / SiO 2 and 0.8g Cr (salphen) were added to 100g cyclohexane, stirred and refluxed for 10h, cooled and filtered with suction, the solid sample was extracted with toluene for 10h, and vacuum dried at 90°C for 10h to obtain the catalyst for this reaction. Add benzyl alcohol, hydrogen peroxide and catalyst into a 75mL autoclave...

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PUM

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Abstract

A catalyst use for synthetizing benzaldehyde is provided, which is characterized in that the invention makes Co schiff base composition as the active component and silica gel as carrier. The silica gel is that: Co schiff base composition equals to 1g / 0.04 to 0.4mmol. The invention has simple preparation method and easy operation. In benzaldehyde synthesis reaction, the invention has the advantages of transforming benzaldehyde is higher, the produced benzaldehyde has good selectivity and good catalyst repeat use performance.

Description

Technical field: [0001] The invention belongs to a solid catalyst for preparing benzaldehyde by oxidizing benzyl alcohol, a preparation method and application. Background technique [0002] Benzaldehyde, also known as bitter almond oil, is the simplest and most industrially important aromatic aldehyde. It is an intermediate for the manufacture of dyes and an important raw material for the manufacture of fine chemicals such as medicines, spices, condiments, and paints. The traditional production method of benzaldehyde is toluene as raw material, through chlorination of toluene side chain followed by hydrolysis or as a by-product of toluene oxidation to prepare benzoic acid. In the former process, the benzaldehyde produced often contains traces of halide ions; in the latter process, its selectivity is lower. In order to produce the halogen-free benzaldehyde required in the perfume and pharmaceutical industries, selective catalytic oxidation of benzyl alcohol is currently the...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J31/22B01J31/34C07C47/54C07C45/29
Inventor 孙予罕魏伟王晓丽吴功德李军平肖福魁
Owner SHANXI INST OF COAL CHEM CHINESE ACAD OF SCI
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