Production method for preparing sodium m-aminobenzene sulfonate by means of continuous hydrogenation reduction

A technology of sodium sulfanilate and sodium nitrobenzenesulfonate, which is applied in the field of continuous hydrogenation reduction to prepare sodium m-aminobenzenesulfonate, which can solve the problems of unstable continuous hydrogenation process, high cost of hydrogenation catalyst, low reaction The problem of low concentration of substances can be solved to achieve the effect of increasing production capacity and equipment utilization rate, reducing production cost and equipment investment, and not reducing reactivity

Active Publication Date: 2017-05-24
SHENYANG RES INST OF CHEM IND
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The continuous hydrogenation production and preparation of sodium aminoaryl sulfonate must solve two scientific problems. The first is that the cost of the catalytic hydrogenation catalyst is too high due to the poisoning and loss of activity of the hydrogenation noble metal catalyst in the raw material, which makes the hydrogenation continuous Second, when the concentration is high in the hydrogenation reduction process, the condensation side reactions of azo compounds and azo oxide compounds are prone to occur, and the dimer and polymer side reactions caused by the deamination reaction are also prone to occur. Reaction, the formation of tar-like substances covering the surface of the catalyst becomes a catalyst poison, making the continuous hydrogenation process unstable, and the hydrogenation of low-concentration substrates tends to have low production efficiency and high energy consumption
[0004] German Bayer Company has improved its technology by adopting series reflux reactors (US5144056), studied a series of continuous hydrogenation processes of nitroarylsulfonic acid intermediates, and the production efficiency has been mentioned, but the reaction substrate concentration is very low, M-nitrobenzenesulfonic acid can only reach 9%, the efficiency is still not enough, and a large amount of waste water is produced

Method used

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  • Production method for preparing sodium m-aminobenzene sulfonate by means of continuous hydrogenation reduction
  • Production method for preparing sodium m-aminobenzene sulfonate by means of continuous hydrogenation reduction
  • Production method for preparing sodium m-aminobenzene sulfonate by means of continuous hydrogenation reduction

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Embodiment 1

[0024] Embodiment 1Pt-V-Mg / C catalyst preparation

[0025] Weigh 4.1g of activated carbon, place it in a 250ml round-bottomed flask, put it into a magnetic stirrer, add 200ml of concentrated nitric acid (65-68%), stir at 100-120°C for 4-16 hours, cool to deionize Wash and filter with water until the pH of the filtrate is neutral, and then dry in an oven at 50-120° C. for 12 hours to obtain 4 g of nitric acid-treated activated carbon. 0.32g chloroplatinic acid (H 2 PtCl 6 6H 2 O) Dissolve in 4ml of concentrated hydrochloric acid and add 40ml of water to dilute. Add 240ml of water and 4g of activated carbon treated with nitric acid into a 500ml four-necked bottle, add the pre-prepared chloroplatinic acid solution dropwise under stirring at 50°C, control the dropping time for about 2 hours, and continue stirring for 30 minutes after the dropping It is completely impregnated with activated carbon. Use saturated sodium carbonate solution to adjust the pH value between 7 and 8,...

Embodiment 2

[0027] Embodiment 2 adopts Pt-V-Mg / C catalyst continuous hydrogenation to prepare sodium m-aminobenzenesulfonate

[0028]Add 600ml of sodium m-nitrobenzenesulfonate aqueous solution (45%) to three hydrogenation reactors (1L) respectively, add respectively the Pt-V-Mg / C catalyst 0.8g prepared in Example 1 simultaneously, and replace the system with nitrogen After 3 times of air, hydrogen was introduced to replace nitrogen 3 times, the hydrogen pressure in the kettle was adjusted to 1.5Mpa, stirring was started, the temperature was raised to 130°C, the metering pump was turned on, and the sodium m-nitrobenzenesulfonate solution was pumped into a The flow rate of the three-stage hydrogenation kettle is controlled at 1L / h, and the temperature and pressure of the three reactors are kept the same. The method of continuously feeding hydrogen, continuous feeding and continuous discharging is adopted. The material solution after the reaction is discharged from the third-stage reactor. ...

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Abstract

The invention belongs to the field of fine chemical engineering, and in particular relates to a production method for preparing sodium m-aminobenzene sulfonate by means of continuous hydrogenation reduction. The method is characterized in that a sodium m-nitrobenzene sulfonate solution is pumped into multiple stages of hydrogenation reaction kettles which are in series connection, and a multi-element catalyst is added into all the reaction kettles; overflow pipes used for conveying a reaction solution are arranged among all the hydrogenation reaction kettles, and a microporus filter used for filtering the catalyst is installed at the front end of each overflow pipe; the reaction solution enters the next kettle by means of liquid level difference after being filtered by the microporus filter; furthermore, balance pipes used for transmitting hydrogen are arranged among all the hydrogenation reaction kettles so as to maintain all the hydrogenation reaction kettles to be communicated with one another in a pressure balance way; therefore, the sodium m-aminobenzene sulfonate can be prepared by means of continuous hydrogenation reduction. After the catalyst provided by the invention is adopted, a condensation side reaction producing azo compounds and oxidized azo compounds is effectively avoided in a high concentration hydrogenation process, dimer and polymer side reactions caused by a deamination reaction can be avoided, and the problem that tarry matters, formed in the side reactions, cover the surface of the catalyst and become catalyst poisons can be solved.

Description

technical field [0001] The invention belongs to the field of fine chemical industry, and specifically relates to a production method for preparing sodium m-aminobenzenesulfonate through continuous hydrogenation reduction. Background technique [0002] Sodium m-aminobenzenesulfonate, English name: metanilic acid; is an important chemical intermediate, mainly used in the following aspects: 1) Preparation of azo, reactive, sulfur and vat dyes, etc.; 2) Preparation of m-hydroxy Benzenesulfonic acid, p-aminosalicylic acid, m-aminophenol, vanillin and sulfonamide agents, etc.; 3) Because it can increase the water solubility of other insoluble substances, it is widely used in detergents and oil additives to protect engines ; 4) Sulfonated polyaniline prepared by doping m-aminobenzenesulfonic acid and aniline compounds has great advantages in device manufacturing, such as chemical sensors, biosensors, light-emitting diodes, optical switches, optical resistors and molecular devices ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C303/32C07C309/46B01J23/648B01J8/10
CPCB01J8/006B01J8/10B01J23/6482B01J2208/00867C07C303/32C07C309/46
Inventor 鄢冬茂闫士杰刘东蔡文蓉杨林涛
Owner SHENYANG RES INST OF CHEM IND
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