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Solvent method for preparing DNS (3,5-dinitrosalicylic acid)

A technology of solvent method and organic solvent, applied in the field of preparation of DNS acid by solvent method, can solve the problems of inconvenient production and preparation of DNS acid, and achieve the effect of improving solubility

Inactive Publication Date: 2018-05-11
JIANGSU HUAIHE CHEM
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] Aiming at the deficiencies of the prior art, the present invention provides a solvent method for preparing DNS acid, which solves the problem of inconvenient production and preparation of DNS acid

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0019] Embodiment 1: A, the selection of organic solvent: the organic solvent in the water-organic solvent mixed medium system includes: multiple choices of ether, alcohol, ester and aldehyde, and repeated experiments have been carried out to obtain water-methanol-ethylene glycol monoethyl ether Mixed media works best.

[0020] B. Determination of the concentration of the reactant: when the concentration of the reactant is between 8% and 20%, there is no obvious change in the experiment, and when the concentration of the reactant exceeds 25%, there will be a red pot Phenomenon.

[0021] C Determination of reaction time: The experimental formula uses paper chromatography to detect the reaction end point, and liquid chromatography to measure the purity of DNS. When the reaction time is 6 hours, the purity of DNS obtained is about 50%, and the reaction time is 7 hours. When the response time is 19%, the DNS purity is 19%. When the response time is 8 hours, the DNS purity is abou...

Embodiment 2

[0023] Embodiment 2: A, the selection of the organic solvent: the organic solvent in the water-organic solvent mixed medium system includes: multiple choices of ether, alcohol, ester and aldehyde, and repeated experiments have been carried out to obtain water-methanol-ethylene glycol monoethyl ether Mixed media works best.

[0024] B. Determination of the concentration of the reactant: when the concentration of the reactant is between 8% and 20%, there is no obvious change in the experiment, and when the concentration of the reactant exceeds 25%, there will be a red pot Phenomenon.

[0025] C. Determination of reaction time: the experimental formula uses paper chromatography to detect the reaction end point, and liquid chromatography is used to measure the purity of DNS. When the reaction time is 6 hours, the purity of DNS obtained is about 50%, and the reaction time is 7 When the response time is 8 hours, the DNS purity is about 195%, and when the response time is 9 hours, t...

Embodiment 3

[0027] Embodiment 3: A, the selection of the organic solvent: the organic solvent in the water-organic solvent mixed medium system includes: multiple choices of ether, alcohol, ester and aldehyde, and repeated experiments have been carried out to obtain water-methanol-ethylene glycol monoethyl ether Mixed media works best.

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Abstract

The invention discloses a solvent method for preparing DNS (3,5-dinitrosalicylic acid). The solvent method comprises steps of selection of an organic solvent, determination of reactant concentration,determination of reaction time and an experiment, wherein for selection of the organic solvent, the organic solvent in a water-organic solvent mixed medium system can be selected from ethers, alcohols, esters and aldehydes, and repeated experiments prove that a water-methanol-ethylene glycol monoethyl ether mixed medium has the best effect; for determination of the reactant concentration, when thereactant concentration is 8%-20%, the experiments are normal and obvious transformation is absent, however, when the reactant concentration is higher than 25%, a pot redness phenomenon occurs; for determination of the reaction time, paper chromatography is adopted for detecting a reaction endpoint during the experiments, liquid chromatography is adopted for determining DNS purity, the DNS purityis about 50% when reaction is performed for 6 h, the DNS purity is about 95% when reaction is performed for 8 h, and the DNS purity is about 19% when reaction is performed for 10 h.

Description

technical field [0001] The invention relates to the technical field of chemistry and chemical engineering, in particular to a solvent method for preparing DNS acid. Background technique [0002] DNS is dinitrosalicylic acid, DNS is the raw material for the production of DSD acid (4,4'-diaminostilbene-2,2'-disulfonic acid), DSD acid is an important intermediate, widely used Used in optical brightener and direct dye industry. There are more than 100 kinds of optical brighteners and more than 70 kinds of direct dyes based on DSD acid, so the market demand for DSD acid is very large. [0003] In the preparation process of DNS acid, due to the limitations of the current industrial level and science and technology, the production of DNS is relatively low, and the low concentration of various chemical reactants is the drawback of the current production process. Experimental debugging The concentration of various reactants is a key factor to increase the yield of DNS, and the reac...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C309/40C07C303/22
CPCC07C303/22C07C309/40
Inventor 厉业敏朱旭东夏珊珊孙小勇王仕祥张道胜
Owner JIANGSU HUAIHE CHEM
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