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Oxydation catalyst used in synthesizing 4-hydroxy 3-methoxy benzaldehyde and 4-hydroxyl-3-ethoxy benzaldehyde by glyoxalic acid method

A technology of methoxybenzaldehyde and ethoxybenzaldehyde, applied in physical/chemical process catalysts, condensation preparation of carbonyl compounds, organic chemistry, etc., can solve problems such as difficult filtration, large amount of copper sulfate, and easy blockage of the filter screen , to achieve the effect of easy filtering

Inactive Publication Date: 2004-10-20
CNPC JILIN CHEM GROUP CORP
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0023] At present, the production of vanillin and ethyl vanillin generally uses copper sulfate as an oxidation catalyst, and the amount of copper sulfate is large. After several hours of air oxidation, it is reduced to cuprous oxide, which is red fine particles, and its activity decreases. For a long time, the filter screen is cleaned frequently; the Na-type oxidation catalyst is now used, which has good activity and selectivity, but after it is used in industrial production, it is difficult to filter, the filter screen is easily blocked, and the number of cleaning times affects the normal operation of production

Method used

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  • Oxydation catalyst used in synthesizing 4-hydroxy 3-methoxy benzaldehyde and 4-hydroxyl-3-ethoxy benzaldehyde by glyoxalic acid method
  • Oxydation catalyst used in synthesizing 4-hydroxy 3-methoxy benzaldehyde and 4-hydroxyl-3-ethoxy benzaldehyde by glyoxalic acid method
  • Oxydation catalyst used in synthesizing 4-hydroxy 3-methoxy benzaldehyde and 4-hydroxyl-3-ethoxy benzaldehyde by glyoxalic acid method

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0051] (1) Catalyst preparation

[0052] Take 2g of iron oxide (Fe 2 o 3 ) is raw material (I); Take by weighing 16.62g ferric sulfate (Fe 2 (SO 4 ) 3 ·XH 2 O, containing Fe21%), 1.17g potassium sulfate (K 2 SO 4 ), 1.17g copper sulfate (CuSO 4 Anhydrous), 1.03g zinc sulfate (ZnSO 4 ·7H 2 O) is the raw material (II), and it is mixed evenly and added to a ball mill tank (volume 20L, 120 rpm, 15 φ35mm balls, 30 φ25mm balls) for ball milling for 1h, separate the balls, collect the product, and obtain the obtained product Needed catalyst, the composition formula of this catalyst composition is:

[0053] Fe 0.08 ·Cu 0.007 · Zn 0.004·K 0.01 ·O 0.49 ·S 0.11

[0054] (2) Catalyst application

[0055] React the above-mentioned oxidation catalyst, glyoxylic acid and guaiacol (or ethyl guaiacol) to obtain the condensed liquid mandelic acid (or ethyl mandelic acid), and put it in a glass oxidation tower of Φ80mm and H1200mm , Air is introduced into the c...

Embodiment 2

[0057] (1) Catalyst preparation

[0058] Take 10g of alumina (Al 2 o 3 ), 5g iron oxide (Fe 2 o 3 ) is raw material (I); Get 1.2g sodium molybdate (Na 2 MoO 4 2H 2 O) and 10g potassium sulfate (K 2 SO 4 ), 6g copper sulfate (CuSO 4 ·5H 2 O), 10g zinc sulfate (ZnSO 4 ·7H 2 O), 35.2g iron sulfate [Fe 2 (SO 4 ) 3 ·XH 2 O], 10.8g magnesium sulfate (MgSO 4 ·7H 2 O) is the raw material (II); mix the raw material (I) and the raw material (II) thoroughly, then put them into a ball mill tank and mill them for 1 hour, separate out the balls, and collect the product as the prepared oxidation catalyst. Its composition formula is:

[0059] Fe 0.2 ·Cu 0.02 · Zn 0.03 · Mg 0.04 ·Mo 0.005 ·Al 0.2 ·K 0.1 ·Na 0.009 ·O 1.84 ·S 0.36

[0060] (2) Catalyst application

[0061] Put the condensed liquid obtained by reacting the catalyst, glyoxylic acid and guaiacol (or ethyl guaiacol) prepared above into a glass oxidation tower with a diameter of φ80mm and H1200mm, an...

Embodiment 3

[0063] (1) Catalyst preparation

[0064] Carry out according to embodiment 2 preparation process. Take 1gFe 2 o 3 Is raw material (I); Then weigh 10gK 2 SO 4 , 6gCuSO 4 ·5H 2 O, 10gZnSO 4 ·7H 2 O, 35.2gFe 2 (SO 4 ) 3 ·XH 2 O, 10.8gMgSO 4 ·7H 2 O, 2gNa 2 MoO 4 2H 2 O is the raw material (II); fully mix the raw material (I) and the raw material (II), mill it with a ball mill for 1 hour, separate the balls, collect the product, and obtain the required catalyst. The composition composition formula of this catalyst is:

[0065] Fe 0.1 ·Cu 0.02 · Zn 0.03 · Mg 0.04 ·Mo 0.008 ·K 0.1 ·Na 0.02 ·O 1.49 ·S 0.20

[0066] (2) Catalyst application

[0067] The application method of the catalyst made above is the same as (2) of embodiment 2. Wherein catalyst, condensation liquid consumption and mandelic acid or ethyl mandelic acid content etc., see the corresponding batch number of embodiment 3 in table 1, table 2.

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Abstract

An oxidizing catalyst for preparing 4-hydroxy-3-methoxyphenyl formaldehyde or 4-hydroxy-3-ethoxyphenyl acetaldehyde from acetaldehyde by acid method contains Mg (0-0.3 mole%), Mo (0-0.02), Fe (0.03-0.3), Cu (0.004-0.04), Zn (0.002-0.07), Al (0-0.7), K (0.009-0.4), Na (0-0.03), O (0.1-3.0) and S (0.05-0.9). Its preparing process includes such steps as proportionally mixing aluminium oxide and / or iron oxide with the Na salt of Mo and sulfate of other metallic elements, and ball grinding. Its advantage is high output rate of products.

Description

technical field [0001] The invention relates to an oxidation catalyst needed for the synthesis of vanillin and ethyl vanillin by a glyoxylic acid method, that is, to a method for synthesizing 4-hydroxy-3-methoxybenzaldehyde, 4-hydroxy-3- Oxidation catalyst required for ethoxybenzaldehyde. Background technique [0002] Vanillin (vanillin), whose scientific name is 4-hydroxy-3-methoxybenzaldehyde, is a flavor enhancer, used as a food flavor; ethyl vanillin, whose scientific name is 4-hydroxy-3 - Ethoxybenzaldehyde is also a flavor enhancer, its fragrance is 3-4 times higher than that of vanillin, and it is also used as a food fragrance. [0003] 1. Synthesis of vanillin: The synthesis of vanillin by glyoxylic acid method is to use glyoxylic acid and guaiacol as raw materials, and it is obtained through condensation, oxidation and decarboxylation. The chemical reaction formula (main reaction) is as follows: [0004] 1.1 Condensation reaction ...

Claims

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Application Information

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IPC IPC(8): B01J27/043B01J27/051C07C45/45C07C47/575
Inventor 侯淑兰魏国峰周自刚王勋章郭双龙刘宇
Owner CNPC JILIN CHEM GROUP CORP
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