Continuous nitrification method of naphthalene sulfonate compound

A technology of naphthalenesulfonic acid and compounds, which is applied in the field of continuous nitration of naphthalenesulfonic acid compounds, can solve the problems of not knowing the practical application value, not mentioning the reaction effect, heat exchange capacity limitation, etc., to reduce thermal risk and simple structure , the effect of ensuring safety

Active Publication Date: 2017-07-07
SHENYANG RES INST OF CHEM IND
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

The production of naphthalenesulfonic acid nitro compounds has the characteristics of large heat release, fast heat release rate, and easy overheating of the system. The production method of intermittent nitration in a reactor has small heat transfer area, high risk, and low production efficiency.
[0003] The Czech patent CS204080 and the Japanese patent JP58128364 respectively proposed a method for preparing 1-nitro-3,6,8-trisulfonic acid by continuous nitration in series in series, both of which improved production efficiency to varying degrees and reduced labor intensity , but due to the limitation of the heat transfer capacity of the reactor, the progress in improving efficiency and increasing safety is limited
[0004] Chinese patent CN102320995 proposes a tubular continuous nitration method for naphthalene-2,7-disulfonic acid in the production of H acid, using a tubular reactor with packing or mixing components inside and a jacket outside, and the material is continuous Through a tubular reactor, the reaction temperature is 40-50°C, and the reaction time is 60 minutes, but the specific reaction effect is not mentioned, and it is not known whether it has practical application value

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  • Continuous nitrification method of naphthalene sulfonate compound
  • Continuous nitrification method of naphthalene sulfonate compound

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Experimental program
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Effect test

Embodiment 1

[0033] The nitrated substance A is 1,3,6-naphthalenetrisulfonic acid sulfuric acid solution with a mass fraction of 45%, and the nitrating agent B is a mixed acid containing 80% fuming nitric acid, specifically, 97% fuming nitric acid and 98% fuming nitric acid in the mixed acid % sulfuric acid was prepared according to the mass ratio of 4.7:1, and the temperature of the constant temperature water bath in device C was 50°C. Preheat the nitrated substance A to 50°C, pass the quantitative pump with the nitrating agent B, and enter the circular channel synchronously according to the flow ratio A:B=8.0:1 to react to generate 8-nitro-1,3,6-naphthalenetrisulfonic acid , the nitric acid ratio is 1.2, the residence time is 100s, and the reacted material flows continuously into the receiving bottle. Through HPLC analysis, the conversion rate of the reaction reached 100%, and the selectivity was 99.2%.

Embodiment 2

[0035] The nitrated substance A is 1,3,6-naphthalenetrisulfonic acid sulfuric acid solution with a mass fraction of 55%, the nitrating agent B is fuming nitric acid with a nitric acid mass fraction of 97%, and the temperature of the constant temperature water bath in the device C is 70°C. Preheat the nitrated substance A to 70°C, pass the quantitative pump with the nitrating agent B, and enter the circular channel synchronously according to the flow ratio A:B=6.1:1 to react to generate 8-nitro-1,3,6-naphthalenetrisulfonic acid , the nitric acid ratio is 1.4, the residence time is 60s, and the reacted material flows continuously into the receiving bottle. Through HPLC analysis, the conversion rate of the reaction reached 100%, and the selectivity was 96.8%.

Embodiment 3

[0037] The nitrated substance A is 2,6-naphthalene disulfonic acid sulfuric acid solution with a mass fraction of 35%, and the nitrating agent B is a mixed acid containing 50% fuming nitric acid, specifically 97% fuming nitric acid and 98% fuming nitric acid in the mixed acid Sulfuric acid is prepared according to the mass ratio of 1:0.94. The temperature of the constant temperature water bath in device C is 40°C. The nitrated compound A is preheated to 40°C, and the nitrated agent B enters synchronously according to the flow ratio of 5.7:1 through the quantitative pump. 1-Nitro-3,7-naphthalene disulfonic acid is generated by reaction in the circular channel, the nitric acid ratio is 1.1 and the residence time is 80s. After the reaction, the material flows continuously into the receiving bottle. Through HPLC analysis, the reaction conversion rate reached 99.5%, and the selectivity was 93.7%.

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Abstract

The invention belongs to the field of organic synthesis, and particularly relates to a continuous nitrification method of a naphthalene sulfonate compound. The method comprises the steps of simultaneously and continuously making the nitrified matter naphthalene sulfonate compound and a nitrating agent enter a channel of a stainless steel annular reaction device under a water bath and supersonic environment through a metering pump on the basis that the nitrate ratio is 1.0-1.4 or 2.1-2.4, performing a mixing reaction for 40-120 s under mechanical action generated by supersonic and at 20-70 DEG C, and conducting discharging continuously after the reaction. According to the continuous nitrification method of the naphthalene sulfonate compound, a sulfuric acid solution and acid for nitration of the naphthalene sulfonate compound enter the annular channel simultaneously and continuously through the metering pump, and are mixed sufficiently by suffering from influences of mechanical effects of vibration, internal friction and the like generated by centripetal force and supersonic of liquid flow exerted on a liquid, and the reaction is completed.

Description

technical field [0001] The invention belongs to the field of organic synthesis, and in particular relates to a continuous nitration method for naphthalenesulfonic acid compounds. Background technique [0002] Naphthalenesulfonic acid nitro compounds are important intermediates for the production of acid dyes, direct dyes, reactive dyes and other types of dyes. The preparation method generally uses sulfuric acid as a solvent, adding nitric acid or nitric acid mixed acid in the reaction kettle. The intermittent nitration method conduct. The production of naphthalenesulfonate nitro compounds has the characteristics of large heat release, fast heat release rate, and easy overheating of the system. The production mode of intermittent nitration in a reactor has small heat transfer area, high risk, and low production efficiency. [0003] The Czech patent CS204080 and the Japanese patent JP58128364 respectively proposed a method for preparing 1-nitro-3,6,8-trisulfonic acid by conti...

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 刘东孟明扬马瑛高嘉新王玉灿杨林涛
Owner SHENYANG RES INST OF CHEM IND
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