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Catalyst for preparing DNS (4, 4'-dinitrostilbene-2, 2'-disulfonic acid) acid and salt of DNS acid and preparation method of catalyst

A catalyst and oxidant technology, applied in the field of chemical engineering, can solve the problems of poor oxidation resistance of metal phthalocyanine, reduced reusability, low catalyst utilization rate, etc., and achieves the effects of high oxidation resistance stability, easy separation and low cost

Inactive Publication Date: 2014-07-23
DALIAN UNIV OF TECH
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  • Abstract
  • Description
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  • Application Information

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Problems solved by technology

However, relatively speaking, the oxidation resistance of metal phthalocyanine is poorer than that of inorganic materials. When the reaction temperature is higher or the reaction time is longer, the metal phthalocyanine will be oxidized and its structure will be destroyed to a certain extent. its reusable performance
And above-mentioned metal phthalocyanine is the powder of a kind of solid particle, only the metal phthalocyanine molecule that is exposed on the outer surface of particle just has catalytic activity, so the utilization rate of catalyst is low
On this basis, CN101 823 003A immobilized water-soluble metal phthalocyanine on magnesium-aluminum hydrotalcite to prepare a homogeneous catalyst with immobilization. Therefore, the utilization rate of the catalyst was improved, but it did not solve the problem. The Problem of Poor Oxidation Resistance of Metal Phthalocyanines

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0022] mn 1.5 Mg 1.5 Al 1.0 Preparation of hydrotalcite

[0023] 0.015 mol of MnCl 2 4H 2 O, 0.015 moles of Mg(NO 3 ) 2 ·6H 2 O and 0.010 mol of Al(NO 3 ) 3 9H 2 O was dissolved in 100ml deionized water to prepare a salt solution; then 0.08 moles of NaOH and 0.05 moles of Na 2 CO 3Dissolve in 100ml of water to prepare an alkaline solution. Under vigorous stirring, drop the above salt solution and alkali solution into a round bottom flask containing 10 mL of deionized water at the same time, and maintain the pH value of the system between 9.5-10, continue stirring for 30 minutes after the addition, and then raise the temperature to 65 ℃ crystallization 18h. After the reaction was completed, the reaction solution was filtered, the filter cake was washed with water until neutral, dried in vacuum at 80°C for 8 hours, and ground to obtain Mn 1.5 Mg 1.5 Al 1.0 Hydrotalcite powder.

Embodiment 2

[0025] co 1.5 Mg 1.5 Al 1.0 Preparation of hydrotalcite

[0026] 0.015 moles of Co(CH 3 COO) 2 4H 2 O, 0.015 moles of Mg(NO 3 ) 2 ·6H 2 O and 0.010 mol of Al(NO 3 ) 3 9H 2 O was dissolved in 100ml deionized water to prepare a salt solution; then 0.08 moles of NaOH and 0.05 moles of Na 2 CO 3 Dissolve in 100ml of water to prepare an alkaline solution. Under vigorous stirring, drop the above salt solution and alkali solution into a round bottom flask containing 10 mL of deionized water at the same time, and maintain the pH value of the system between 9.5-10, continue stirring for 30 minutes after the addition, and then raise the temperature to 65 ℃ crystallization 18h. After the reaction was completed, the reaction solution was filtered, the filter cake was washed to neutrality, dried in vacuum at 80°C for 8 hours, and the Co 1.5 Mg 1.5 Al 1.0 Hydrotalcite powder.

Embodiment 3

[0028] Mg 3 Al 0。6 Fe 0.4 Preparation of hydrotalcite

[0029] 0.030 moles of Mg(NO 3 ) 2 ·6H 2 O, 0.006 moles of Al(NO 3 ) 3 9H 2 O and 0.004 moles of Fe(NO 3 ) 3 9H 2 O was dissolved in 100ml deionized water to prepare a salt solution; then 0.08 moles of NaOH and 0.05 moles of Na 2 CO 3 Dissolve in 100ml of water to prepare an alkaline solution. Under vigorous stirring, drop the above salt solution and alkali solution into a round bottom flask containing 10mL of deionized water at the same time, and maintain the pH value of the system between 9-10, continue to stir for 30min after the dropwise addition, and raise the temperature to 65°C Crystallization 20h. Then filter, wash the filter cake with water until neutral, dry in vacuum at 80°C for 8 hours, and grind to obtain Mg 3 Al 0.6 Fe 0.4 Hydrotalcite powder.

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Abstract

The invention provides a catalyst for preparing a DNS (4, 4'-dinitrostilbene-2, 2'-disulfonic acid) acid and a salt of the DNS acid and a preparation method of the the catalyst, belongs to the technical field of chemical engineering, and relates to a preparation method of a dye and a fluorescent brightener intermediate of the dye. The method comprises the steps of getting nitrotoluene sulphonic acid as a raw material; adding hydrotalcite formed by magnesium, aluminum and transition metal as a catalyst to replace the traditional transition metal salt catalyst; taking air or oxygen as an oxidant; and carrying out oxidative condensation on an alkaline aqueous solution so as to obtain 4, 4'-dinitrostilbene-2, 2'-disulfonic acid (DNS). The catalyst and the preparation method provided by the invention have the effects and beneficial effects that the hydrotalcite doped with the transition metal is adopted as the catalyst, so that the advantages of high activity, good selectivity and easiness of separation of the catalyst are achieved; when the catalyst is adopted to carry out oxidization reaction of NTS (nitrotoluene-2-sulphonic acid), the yield is more than that of the current production technology. The catalyst provided by the invention is a catalyst which is high in anti-oxidation stability and low in cost, capable of being regenerated and recycled, and has no sewage of transition metal ions, so that the current production technology can be replaced.

Description

technical field [0001] The invention belongs to the technical field of chemical engineering, and relates to a preparation method of a dye and a fluorescent whitening agent intermediate thereof, in particular to a catalyst for preparing DNS acid and a method for preparing DNS acid and a salt thereof. Background technique [0002] DNS (4,4'-dinitrostilbene-2,2'-disulfonic acid) is a raw material for the production of DSD acid (4,4'-diaminostilbene-2,2'-disulfonic acid) , DSD acid is an important intermediate widely used in optical brightener and direct dye industries. 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] The preparation process of DSD acid mainly includes three-step reactions: firstly, p-nitrotoluene is sulfonated to generate p-nitrotoluene orthosulfonic acid (NTS), then oxidizes NTS to generate DNS, and finally reduces DNS to DSD acid. In these ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): B01J23/34B01J23/755B01J23/75B01J23/745C07C309/40C07C303/22
Inventor 王梅徐绍平王晓璐
Owner DALIAN UNIV OF TECH
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