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Preparation method for p-hydroxy benzaldehyde

A technology of p-hydroxybenzaldehyde and methanol solution, which is applied in the chemical industry, can solve the problems of complex preparation process and low production efficiency, and achieve the effects of improving purity, improving utilization rate and rapid response

Inactive Publication Date: 2019-01-11
南京雪郎化工科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] The technical problem to be solved in the present invention is to provide a kind of preparation method of p-hydroxybenzaldehyde, to solve the problems such as complicated preparation process and low production efficiency existing in the prior art

Method used

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  • Preparation method for p-hydroxy benzaldehyde
  • Preparation method for p-hydroxy benzaldehyde

Examples

Experimental program
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Effect test

Embodiment 1

[0022] Such as figure 1 A kind of preparation method of shown p-Hydroxybenzaldehyde, comprises the steps:

[0023] 1) Preparation of Intermediate I: P-cresol solution is placed in a quartz reactor, and then an excess of 50-64% (NH3) H2O solution and an appropriate amount of catalysis are added to the quartz reactor. Keep the temperature in the range of 8-16° C., and stir and mix with a stirring device for 70-90 minutes under strong light irradiation to obtain a mixed solution of intermediate I, methanol solution and (NH3)·H2O.

[0024] 2) Preparation of Intermediate II: In the mixed solution obtained in Step 1) to obtain Intermediate I, methanol solution and (NH 3 )·H 2 O, oxygen with a concentration of 90-98% is continuously fed into it, and a stirring device is used while feeding oxygen The mixed solution was stirred for 2h to obtain a mixed solution of intermediate II, methanol solution and (NH3)·H2O.

[0025] 3) Preparation of p-Hydroxybenzaldehyde: In a low temperature ...

Embodiment 2

[0033] Such as figure 1 A preparation method for p-Hydroxybenzaldehyde, comprising the steps of:

[0034] (1) Preparation of Intermediate I: P-cresol solution is placed in a quartz reactor, then an excess of 50-64% (NH3) H2O solution and an appropriate amount of The catalyzed methanol solution was kept at a temperature of 8-16°C, and under strong light irradiation, it was stirred and mixed with a stirring device for 70-90 minutes to obtain a mixed solution of intermediate I, methanol solution and (NH3)·H2O.

[0035] 2) Preparation of Intermediate II: In the mixed solution obtained in Step 1) to obtain Intermediate I, methanol solution and (NH 3 )·H 2 O, oxygen with a concentration of 90-98% is continuously fed into it, and a stirring device is used while feeding oxygen The mixed solution was stirred for 3h to obtain a mixed solution of intermediate II, methanol solution and (NH3)·H2O.

[0036] 3) Preparation of p-Hydroxybenzaldehyde: In a low temperature environment of 4-8°C...

Embodiment 3

[0044] Such as figure 1 Shown, a kind of preparation method of p-Hydroxybenzaldehyde comprises the steps:

[0045] 1) Preparation of Intermediate I: P-cresol solution is placed in a quartz reactor, and then an excess of 50-64% (NH3) H2O solution and an appropriate amount of catalysis are added to the quartz reactor. Keep the temperature in the range of 8-16° C., and stir and mix with a stirring device for 70-90 minutes under strong light irradiation to obtain a mixed solution of intermediate I, methanol solution and (NH3)·H2O.

[0046] 2) Preparation of Intermediate II: In the mixed solution obtained in Step 1) to obtain Intermediate I, methanol solution and (NH 3 )·H 2 O, oxygen with a concentration of 90-98% is continuously fed into it, and a stirring device is used while feeding oxygen The mixed solution was stirred for 2.5h to obtain a mixed solution of intermediate II, methanol solution and (NH3)·H2O.

[0047] 3) Preparation of p-Hydroxybenzaldehyde: In a low temperatur...

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Abstract

The invention provides a preparation method for p-hydroxy benzaldehyde. The preparation method comprises the following five steps: preparation of an intermediate I, preparation of an intermediate II,preparation of p-hydroxy benzaldehyde, impurity removal from a p-hydroxy benzaldehyde solution, and purification of the p-hydroxy benzaldehyde solution. The synthetic process is simple and standard, the production process and the production flow are easy to master, and the utilization ratio of a p-methylphenol raw material is improved effectively while the production operational standard of a p-hydroxy benzaldehyde product is improved effectively. By taking ammonia monohydrate as a reactant for the p-methylphenol raw material, the reaction on the p-methylphenol raw material is quicker and morecomplete, and ammonium sulfate impurity generated by the reaction is more easily treated. In the preparation process of the p-hydroxy benzaldehyde, a purification process on the p-hydroxy benzaldehyde is increased, so that the purity of the p-hydroxy benzaldehyde prepared can be improved effectively.

Description

technical field [0001] The invention relates to a preparation method of p-hydroxybenzaldehyde, which belongs to the technical field of chemical industry. Background technique [0002] p-Hydroxybenzaldehyde is an important intermediate in organic synthesis, widely used in fine chemical products such as medicine, spices, electroplating, food and pesticides. The demand in the international market for p-hydroxybenzaldehyde has increased significantly in recent years, and the price has continued to rise. Although there are more than a dozen manufacturers of p-hydroxybenzaldehyde in my country, most of them still use the traditional phenol (formaldehyde) method, which not only affects the utilization rate of formaldehyde is not high, and the prepared p-hydroxybenzaldehyde purity is not ideal enough, so there is an urgent need for a method for preparing p-hydroxybenzaldehyde with high utilization rate and high purity. Contents of the invention [0003] The technical problem to be...

Claims

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Application Information

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IPC IPC(8): C07C47/565C07C45/64C07C45/78C07C45/80
CPCC07C37/00C07C45/36C07C45/64C07C45/78C07C45/80C07C39/07C07C47/565
Inventor 李云政张磊
Owner 南京雪郎化工科技有限公司
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