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Preparation method of 2, 7-naphthalene disulfonic acid

A technology of naphthalene disulfonic acid and acidity, applied in the preparation of sulfonic acid, organic chemistry, etc., can solve the problems of low naphthalene utilization rate, low conversion rate, increased reaction cost, etc., and achieves improved conversion rate, improved purity, and high utilization rate. Effect

Pending Publication Date: 2021-03-09
GUANGDONG SUNION CHEM & PLASTIC +1
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, it can be seen that most of the preparation methods used in the prior art have the problems of high reaction temperature and low conversion rate. The high reaction temperature will cause high energy consumption of the reaction, and it is easy to cause the raw material naphthalene to be oxidized and carbonized in the reaction process. , which leads to a series of problems such as low utilization rate of naphthalene, high reaction cost and insufficient product purity.

Method used

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  • Preparation method of 2, 7-naphthalene disulfonic acid
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  • Preparation method of 2, 7-naphthalene disulfonic acid

Examples

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Effect test

Embodiment 1

[0037] A kind of preparation method of 2,7-naphthalene disulfonic acid, specifically comprises the steps:

[0038] (1) Heating 1 mol of industrial naphthalene to 80° C., and after all of them melted, slowly added 1.15 mol of concentrated sulfuric acid with a concentration of 98%, raised the temperature to 90° C. under nitrogen protection conditions, and reacted for 150 minutes to obtain an intermediate product;

[0039] (2) Add 2 mol of concentrated sulfuric acid with a concentration of 98% to the intermediate product obtained in step (1), vacuumize, so that the negative pressure of the reaction is 10Pa, heat up to 135 ° C, after reacting for 6 hours, cool to 50 ° C, add water to control The acidity is 50 mgKOH / g, dissolved and filtered to obtain the 2,7-naphthalene disulfonic acid.

Embodiment 2

[0041] A preparation method of 2,7-naphthalene disulfonic acid, the only difference from Example 1 is that the concentration of 98% concentrated sulfuric acid in step (1) is added in an amount of 1.3mol, other components, consumption and process The parameters were all the same as in Example 1 to obtain the 2,7-naphthalene disulfonic acid.

Embodiment 3

[0043] A preparation method of 2,7-naphthalene disulfonic acid, the only difference from Example 1 is that the concentration of 98% concentrated sulfuric acid in step (1) is added in an amount of 1.55mol, other components, consumption and process The parameters were all the same as in Example 1 to obtain the 2,7-naphthalene disulfonic acid.

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Abstract

The invention provides a preparation method of 2, 7-naphthalene disulfonic acid, which comprises the following steps: (1) reacting naphthalene with concentrated sulfuric acid under inert gas shieldingconditions to obtain an intermediate product; and (2) reacting the intermediate product obtained in the step (1) with concentrated sulfuric acid under a negative pressure condition to obtain the 2, 7-naphthalene disulfonic acid, and according to the preparation method, by controlling reaction conditions in different reaction periods, the conversion rate of naphthalene is increased, the purity ofthe prepared 2, 7 -naphthalene disulfonic acid is improved, and the preparation method is low in energy consumption and cost and has industrial application prospects.

Description

technical field [0001] The invention belongs to the technical field of material synthesis, and in particular relates to a preparation method of 2,7-naphthalene disulfonic acid. Background technique [0002] 2,7-Naphthalene disulfonic acid is a white, gray crystal, easy to absorb water, is an important intermediate in the dye industry, can be used to prepare the important dye intermediate H acid, mainly used in cotton, wool, hemp, silk fiber and other industries , and with the continuous deepening of various researches, the use of sodium 2,7-naphthalene disulfonate is becoming more and more extensive. [0003] The traditional method of preparing 2,7-naphthalene disulfonic acid is to use refined naphthalene to heat and stir to melt it. After the refined naphthalene is completely melted, add a certain amount of concentrated sulfuric acid dropwise, and then control the temperature, reaction time and other parameters to prepare 2,7-naphthalene disulfonic acid. Studies have show...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C303/06C07C309/35
CPCC07C303/06C07C309/35
Inventor 季成忠曹勇俊黎广贞李宇辉杨寿盛郑岩邹增生
Owner GUANGDONG SUNION CHEM & PLASTIC
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