Device and method for extracting 2-naphthol methyl ether from 2-naphthol, methyl alcohol, 2-naphthol methyl ether and p-toluenesulfonic acid and recovering components

A technology of p-toluenesulfonic acid and naphthalene methyl ether, which is applied in ether separation/purification, chemical instruments and methods, ether preparation, etc., can solve the problem of low yield in the refining process, achieve high purity and yield, simple process, highly operable effect

Active Publication Date: 2018-09-25
NANJING NORMAL UNIVERSITY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] The preparation of 2-naphthyl methyl ether by the above-mentioned sulfuric acid method and the dimethyl sulfate method all needs neutralization, solubilization crystallization and recrystallization. The yield of the refining process is low

Method used

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  • Device and method for extracting 2-naphthol methyl ether from 2-naphthol, methyl alcohol, 2-naphthol methyl ether and p-toluenesulfonic acid and recovering components
  • Device and method for extracting 2-naphthol methyl ether from 2-naphthol, methyl alcohol, 2-naphthol methyl ether and p-toluenesulfonic acid and recovering components
  • Device and method for extracting 2-naphthol methyl ether from 2-naphthol, methyl alcohol, 2-naphthol methyl ether and p-toluenesulfonic acid and recovering components

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0021] The present invention adopts above-mentioned device to extract 2-naphthyl methyl ether and reclaims the method for other components, comprises the steps:

[0022] (1) adopt the continuous intermediate feeding mode, add the mixed solution (2-naphthol) of 2-naphthol, methyl alcohol, 2-naphthyl methyl ether and p-toluenesulfonic acid from the mixture inlet 3 of double side line rectifying tower 1 0.1958, methyl alcohol 0.5498, 2-naphthyl methyl ether 0.1969, p-toluenesulfonic acid 0.0575), through the condenser 11 and heater 19 at the top of the tower, the temperature at the top and bottom of the double-side line rectification tower 1 is controlled to be 28.3~30.2°C respectively and 256.7~259.1°C, set the reflux ratio of the condenser 11 at the top of the tower to 3:1, and adjust the pressure of the tower to 0.02MPa;

[0023] (2) When the top and bottom temperatures and the reflux ratio of the double-side line rectifying tower 1 were stable, the mixture feed port 3, methan...

Embodiment 2

[0029] The present invention adopts above-mentioned device to extract 2-naphthyl methyl ether and reclaims the method for other components, comprises the steps:

[0030] (1) adopt the continuous intermediate feeding mode, add the mixed solution (2-naphthol) of 2-naphthol, methyl alcohol, 2-naphthyl methyl ether and p-toluenesulfonic acid from the mixture inlet 3 of double side line rectifying tower 1 0.1958, methanol 0.5498, 2-naphthyl methyl ether 0.1969, p-toluenesulfonic acid 0.0575), through the condenser 11 and the heater 19 control the temperature of the top and bottom of the double-side line rectification tower to be 28.2~30.4°C and 256.5~260.2°C respectively , the reflux ratio of setting condenser 11 is 4:1, and the pressure of regulating tower is 0.02MPa;

[0031](2) When the top and bottom temperatures and the reflux ratio of the double-side line rectifying tower 1 were stable, the mixture feed port 3, methanol discharge port 8, 2-naphthyl methyl ether side line disc...

Embodiment 3

[0034] The present invention adopts above-mentioned device to extract 2-naphthyl methyl ether and reclaims the method for other components, comprises the steps:

[0035] (1) adopt the continuous intermediate feeding mode, add the mixed solution (2-naphthol) of 2-naphthol, methyl alcohol, 2-naphthyl methyl ether and p-toluenesulfonic acid from the mixture inlet 3 of double side line rectifying tower 1 0.1958, methanol 0.5498, 2-naphthyl methyl ether 0.1969, p-toluenesulfonic acid 0.0575), through the condenser 11 and the heater 19 control the temperature of the top and bottom of the double-side line rectification tower to be 28.3~30.2°C and 256.7~259.1°C respectively , the reflux ratio of setting condenser 11 is 4:1, and the pressure of regulating tower is 0.02MPa;

[0036] (2) When the top and bottom temperatures and the reflux ratio of the double-side line rectifying tower 1 were stable, the mixture feed port 3, methanol discharge port 8, 2-naphthyl methyl ether side line dis...

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Abstract

The invention discloses a device and a method for extracting 2-naphthol methyl ether from 2-naphthol, methyl alcohol, 2-naphthol methyl ether and p-toluenesulfonic acid and recovering components. Thedevice comprises a double-sidestream rectifying tower and a stripping tower connected therewith. The preparation method thereof comprises the following steps: adding a 2-naphthol, methyl alcohol, 2-naphthol methyl ether and p-toluenesulfonic acid mixture; after performing purification in the double-sidestream rectifying tower, obtaining p-toluenesulfonic acid at a tower bottom, obtaining methyl alcohol at a tower top, and obtaining 2-naphthol methyl ether through a 2-naphthol methyl ether sidestream discharging collector; after delivering 2-naphthol distillate to the stripping tower for refining through a 2-naphthol sidestream discharging collector, obtaining 2-naphthol at a tower bottom, and circulating a product obtained at a tower top to the double-sidestream rectifying tower. The device and the method have the significant advantages that when the device is adopted to extract 2-naphthol methyl ether from the mixture, the purity and the yield are high, and no by-products is producedin the whole reaction process.

Description

technical field [0001] The invention belongs to the technical field of 2-naphthyl methyl ether extraction, and in particular relates to a device and a method for extracting 2-naphthyl methyl ether from 2-naphthol, methanol, 2-naphthyl methyl ether and p-toluenesulfonic acid and recovering components. Background technique [0002] 2-Naphthylmethyl ether is a spice with the aroma of orange blossom. It is used to prepare low-grade colored soaps, detergents and essences for daily necessities. The applicable fragrance types are orange blossom, jasmine, and lily. In addition, it can also be used in low-grade cologne and floral essences to impart a heavy floral fragrance, and it can also be used in the fragrance of plastic products that require alkali and heat resistance, and synthetic rubber products. [0003] At present, there are two main methods for preparing 2-naphthyl methyl ether: one is obtained by reacting 2-naphthol with methanol, heating 2-naphthol, methanol and sulfuric...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C41/40C07C43/20C07C37/70C07C39/14
CPCC07C37/70C07C41/40C07C43/202C07C39/14
Inventor 顾正桂汪凯军黄鑫王庆雄
Owner NANJING NORMAL UNIVERSITY
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