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Process for continuous hydrolysis synthesis of guaiacol

A technology of guaiacol and hydrolysis kettle, which is applied in the fields of chemical instruments and methods, preparation of organic compounds, organic chemistry, etc. It can solve the problems of sharp increase in alkali consumption and the loss outweighs the gain, and achieve the improvement of reaction selectivity and the reduction of unit consumption , the effect of increasing costs

Active Publication Date: 2005-01-26
浙江纵华香料股份有限公司
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AI Technical Summary

Problems solved by technology

The alkali consumption during wastewater neutralization and copper sulfate recovery will increase sharply, and the cost will exceed the benefit of selectivity improvement, and the gain outweighs the gain

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0027] 40g of anthranil was diazotized with 23g of sodium nitrite dissolved in 92g of water in 200g of water and 50g of 98% sulfuric acid to obtain 329ml of diazonium solution.

[0028] Pre-set 350ml of hydrolyzate in the hydrolyzer, containing 183g of water, 67g of sodium sulfate, 14g of sulfuric acid and 296g of CuSO 4 ·5H 2 O.

[0029] Heat the preset hydrolyzate to 103°C. Add the diazonium solution listed above to the preset hydrolyzate within 1 hour, and the guaiacol produced by hydrolysis will be continuously distilled out with water vapor. Continue to stir for 0.5 hour after the addition, during which 100ml of water is added, and the same amount of water is distilled off (to take out the remaining guaiacol). The yield of tar was 6.4%, and the yield of guaiacol was 90.3%.

Embodiment 2

[0031] 80kg of anthranil was diazotized with 48kg of sodium nitrite dissolved in 192kg of water in 700kg of water and 100kg of 98% sulfuric acid to obtain 1000L of diazonium solution. This is a batch of diazo solution.

[0032] 1650L hydrolyzate is preset in the hydrolyzer, which contains 990kg water and 150kgH 2 SO 4 and 1500kgCuSO 4 ·5H 2 O.

[0033] Heat the preset hydrolyzate to 105°C. To the preset hydrolyzate, continuously add the above 10 batches of diazonium solution within 10 hours, and at the same time add basic copper sulfate (30wt%) suspension at a speed of 324L / h, and discharge part continuously at a speed of 270L / h Hydrolysis raffinate. The generated guaiacol is continuously distilled out with water vapor. Continue to stir for 2 hours after the addition, during which 200L of water is added, and the same amount of water is distilled off (to take out the remaining guaiacol). The yield of tar was 8.1%, and the yield of guaiacol was 88.8%.

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Abstract

The invention provides a process for continuous hydrolysis synthesis of guaiacol consisting of, converting copper salt discharged from the hydrolysis kettle into alkali type copper, reacting the alkali type copper returning the hydrolysis kettle with sulphuric acid carried in by the diazonium liquid, so as to convert into copper sulfate again, thus realizing the circulation of copper sulfate catalyst.

Description

technical field [0001] The invention relates to an improved method for synthesizing guaiacol. Background technique [0002] Guaiacol, or o-methoxyphenol, is an important pharmaceutical intermediate and an important starting material for the synthesis of various raw materials and spices. At present, o-aminoanisole is still mainly used as raw material to produce guaiac in China. Phenol is diazotized first, and then hydrolyzed with copper sulfate as a catalyst. [0003] The hydrolysis adopts a semi-continuous operation mode: the copper sulfate aqueous solution is placed in the hydrolysis kettle in advance, and then the diazo solution is continuously added to the hydrolysis kettle; the guaiacol produced by hydrolysis is continuously stripped with steam, and condensed and collected after leaving the hydrolysis kettle. The non-volatile sulfuric acid, sodium sulfate and by-product tar that enter the hydrolysis tank with the diazo solution gradually accumu...

Claims

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Application Information

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IPC IPC(8): C07C41/26C07C43/253
Inventor 陈敏恒何刚张瑞生
Owner 浙江纵华香料股份有限公司
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