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Method for synthesizing 2-naphthol-3,7-naphthalenedisulfonic acid disodium salt

A technology of sodium naphthalene disulfonate and naphthol, applied in the preparation of sulfonate, organic chemistry and other directions, can solve problems such as low atom economy, and achieve the effect of mild reaction conditions and simple method

Inactive Publication Date: 2018-08-17
NANTONG BAISHENG CHEM
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

But existing introduction in the prior art of the synthetic method of other sodium naphthalene sulfonate, for example: the Chinese patent that application number is 200410010659.1 and 200810197213.2 has introduced a kind of method that adopts the vitriol oil to prepare 2-sodium naphthalenesulfonate as sulfonating agent, this Method In order to maintain the concentration of sulfuric acid, a large excess of concentrated sulfuric acid must be used. Usually, the utilization rate of sulfuric acid will not exceed 50%, and a large amount of acid-containing wastewater will be produced at the same time; The method for preparing sodium butylnaphthalene sulfonate with a sulfonating agent requires the use of excessive oleum in the process, which also produces a large amount of acid-containing wastewater; the Chinese patent application number 200610096806.0 reports a preparation using chlorosulfonic acid as a sulfonating agent The method of sodium salt of 1-naphthalenesulfonic acid, but the sulfonation method with chlorosulfonic acid as sulfonating agent has low atom economy

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0018] In a 250ml autoclave, add diglyme 25.0ml, 2-naphthol-7-naphthalene disulfonic acid 24.6g, calcium iodide 0.1g, ozone 4.9g, then pass into 0.5Mpa of sulfur dioxide, stir The temperature was raised to 50° C. and the reaction was carried out at this temperature for 3 hours. Then release the pressure and vent the sulfur dioxide, add 8.4g of sodium bicarbonate to the resulting mixed solution, stir vigorously at 60°C for 4 hours, filter and dry to obtain the crude product of sodium 2-naphthol-3,7-naphthalene disulfonate 32.6g. Liquid chromatographic analysis of the product showed that the content of sodium 2-naphthol-3,7-naphthalene disulfonate in the product was 92.7% (yield 86.8%).

Embodiment 2

[0020] In a 250ml autoclave, add diglyme 25.0ml, 2-naphthol-7-naphthalene disulfonic acid 24.6g, calcium iodide 0.1g, ozone 4.9g, then pass into 0.2Mpa sulfur dioxide, stir The temperature was raised to 50° C. and the reaction was carried out at this temperature for 3 hours. Then release the pressure and vent the sulfur dioxide, add 8.4g of sodium bicarbonate to the resulting mixed solution, stir vigorously at 60°C for 4 hours, filter and dry to obtain the crude product of sodium 2-naphthol-3,7-naphthalene disulfonate 30.1g. Liquid chromatographic analysis of the product showed that the content of sodium 2-naphthol-3,7-naphthalene disulfonate in the product was 93.8% (yield 81.1%).

Embodiment 3

[0022] The catalyzer that adopts is calcium bromide, and all the other are identical with embodiment 1, and final productive rate is 62.6%.

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Abstract

The invention relates to a method for synthesizing 2-naphthol-3,7-naphthalenedisulfonic acid disodium salt. The method comprises the following steps: adding a reaction solvent, 20-30 parts of 2-naphthol-7-naphthalene disulfonic acid, 0.05-0.5 part of a catalyst and 4-6 parts of ozone in an autoclave, then feeding 0.2-0.6 Mpa of sulfur dioxide, stirring and heating to the temperature of 40-70 DEG C, reacting for 2-4 h, and then relieving pressure to empty sulfur dioxide to obtain a mixed solution; and adding 6-10 parts of sodium bicarbonate in the mixed solution, reacting for 3-7 hours while stirring at the temperature of 40-70 DEG C, and then filtering and drying to obtain the final product. Compared with a traditional method for synthesizing naphthalene sulfonic acid sodium salt, the method is simple and is gentle in reaction conditions; an adopted sulfonation method has 100% atom economy, any waste water is not generated in a synthesizing process, and the method is economical and environmentally friendly.

Description

technical field [0001] The invention relates to a method for synthesizing hydroxynaphthalene, in particular to a new method for synthesizing sodium 2-naphthol-3,7-naphthalene disulfonate, which belongs to the technical field of fine chemicals. Background technique [0002] Sodium 2-naphthol-3,7-naphthalene disulfonate (CAS No.: 83949-45-5) is a slightly yellow powder, which is widely used as a dye, a pigment intermediate, etc. At present, there are very few reports on the synthesis method of sodium 2-naphthol-3,7-naphthalene disulfonate, and no patent documents in this regard have been retrieved. But existing introduction in the prior art of the synthetic method of other sodium naphthalene sulfonate, for example: the Chinese patent that application number is 200410010659.1 and 200810197213.2 has introduced a kind of method that adopts the vitriol oil to prepare 2-sodium naphthalenesulfonate as sulfonating agent, this Method In order to maintain the concentration of sulfuric...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C303/32C07C309/43
CPCC07C303/32C07C309/43
Inventor 胡兴邦仲飞黄彩红
Owner NANTONG BAISHENG CHEM