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A kind of 2-naphthalenesulfonic acid and 2-naphthalenesulfonic acid sodium salt and preparation method thereof

A technology of sodium naphthalenesulfonate and naphthalenesulfonic acid, which is applied in the field of naphthalenesulfonic acid and its sodium salt, can solve problems such as inability to fully utilize existing resources, difficulty in technical transformation, and increase investment, and achieve high product quality and full utilization , the effect of reducing environmental pollution

Inactive Publication Date: 2011-12-14
WUHAN UNIV OF SCI & TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

But the process uses SO 3 Nitrogen or air mixed gas with a content of 1-50V% is used as a sulfonating agent, and the reaction produces a large amount of waste gas, and the tail gas needs to be passed into gas treatment facilities; a large number of kettle reactors used in traditional processes are converted into membrane or tube reactors Technical transformation is difficult, and it needs to be equipped with an additional aging device, which cannot make full use of existing resources and increases additional investment; so far, there have been no reports of this method being used in industrial production.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0015] A kind of 2-naphthalenesulfonic acid and 2-naphthalenesulfonic acid sodium salt and its preparation method.

[0016] Put anhydrous sodium sulfate and naphthalene in a molar ratio of 0.0009 to 0.0156:1 into a reactor containing 98% sulfuric acid, the molar ratio of naphthalene to sulfuric acid is 1:0.1 to 0.2, and heat up to 80 to 90°C while stirring. Sodium sulfate and naphthalene are completely dissolved in water.

[0017] Add SO while stirring 3 The gas undergoes sulfonation reaction, the reaction temperature is 160-180°C, SO 3 The gas purity is 98wt% ~ 100wt%, and SO 3 The molar ratio of the total amount of the naphthalene to the input amount of naphthalene is 1~1.2:1, and the SO 3 The time of gas is 2-3 hours, and the sulfonated mixture is obtained.

[0018] Then, under the condition of 150-180°C, the unreacted naphthalene and SO in the above-mentioned sulfonated mixture were decomposed with compressed nitrogen while stirring. 3 Naphthalene and SO produced by d...

Embodiment 2

[0023] A kind of 2-naphthalenesulfonic acid and 2-naphthalenesulfonic acid sodium salt and its preparation method.

[0024] Anhydrous sodium sulfate and naphthalene with a molar ratio of 0.0156 to 0.0303:1 are put into a reactor containing 98% sulfuric acid, the molar ratio of naphthalene to sulfuric acid is 1:0.2 to 0.3, and the temperature is raised to 90 to 100°C while stirring to make no Sodium sulfate and naphthalene are completely dissolved in water.

[0025] Add SO while stirring 3 The gas undergoes sulfonation reaction, the reaction temperature is 140-160°C, SO 3 The gas purity is 98wt% ~ 100wt%, and SO 3 The molar ratio of the total amount of the naphthalene to the input amount of naphthalene is 0.8~1:1, and the SO 3 The time of gas is 1-2 hours, and the sulfonated mixture is obtained.

[0026] Then, under the condition of 150-180°C, the unreacted naphthalene and SO in the above-mentioned sulfonated mixture were decomposed with compressed nitrogen while stirring. ...

Embodiment 3

[0031] A kind of 2-naphthalenesulfonic acid and 2-naphthalenesulfonic acid sodium salt and its preparation method.

[0032] Put anhydrous sodium sulfate and naphthalene in a molar ratio of 0.0303 to 0.045:1 into a reactor containing 98% sulfuric acid, the molar ratio of naphthalene to sulfuric acid is 1:0.3 to 0.4, and heat up to 100 to 110°C while stirring to make no Sodium sulfate and naphthalene are completely dissolved in water.

[0033] Add SO while stirring 3 The gas undergoes sulfonation reaction, the reaction temperature is 120-140°C, SO 3 The gas purity is 98wt% ~ 100wt%, and SO 3 The molar ratio of the total amount of the naphthalene to the input amount of naphthalene is 0.6~0.8:1, and the SO 3 The time of gas is 1-2 hours, and the sulfonated mixture is obtained.

[0034] Then, under the condition of 150-180°C, the unreacted naphthalene and SO in the above-mentioned sulfonated mixture were decomposed with compressed nitrogen while stirring. 3 Naphthalene and SO ...

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Abstract

The invention relates to 2-naphthalenesulfonic acid and sodium salt of 2-naphthalenesulfonic acid and its preparation technology. Its technical scheme is: put naphthalene and a small amount of anhydrous sodium sulfate into a reactor containing 98% sulfuric acid, the molar ratio of naphthalene to sulfuric acid is 1: 0.1 to 0.5, and heat up while stirring until the naphthalene and anhydrous sodium sulfate are completely dissolved; Then, in 1 to 3 hours, SO3 gas is passed into the reactor for sulfonation reaction at a temperature of 120 to 180°C; then, under the condition of 150 to 180°C, the naphthalene and SO3 in the sulfonated mixture are sulfonated with compressed nitrogen gas while stirring. Blow away to produce 2-naphthalenesulfonic acid. In the present invention, the prepared 2-naphthalenesulfonic acid can also be added to the neutralization pot, and the sodium sulfite solution preheated to 80-90°C with a concentration of 5% to 15% can be added to the neutralization pot through the metering tank for neutralization reaction , After crystallization and separation, 2-naphthalenesulfonic acid sodium salt was obtained. The invention has the characteristics of sufficient utilization of existing resources, high conversion rate of naphthalene, good product quality, reduced environmental pollution, low cost and high economic benefit.

Description

technical field [0001] The invention belongs to the technical field of naphthalenesulfonic acid and its sodium salt. Specifically relates to a kind of 2-naphthalenesulfonic acid and 2-naphthalenesulfonic acid sodium salt and preparation technology thereof. Background technique [0002] 2-naphthalenesulfonic acid is the production of 2-naphthol (C 10 h 7 OH) is also a raw material for the synthesis of azo dyes. The naphthalenesulfonic acid formaldehyde condensate obtained by the further condensation of naphthalenesulfonic acid and formaldehyde is an important intermediate for pigments, dyes, dispersants for emulsification synthesis, and cement water reducers. [0003] The existing preparation methods of 2-naphthalenesulfonic acid mainly include concentrated sulfuric acid sulfonation method and gas SO 3 Sulfonation method. The traditional production method is to use the concentrated sulfuric acid process, generally need to use excess sulfuric acid during the reaction, oth...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C309/35C07C303/06
Inventor 易德莲官章伟张恒明周建锋伍林黄义和
Owner WUHAN UNIV OF SCI & TECH