A kind of cyclic synthesis method of nitroaniline chloride
A technology of nitroaniline and a synthesis method, which is applied in chemical instruments and methods, preparation of amino compounds, preparation of organic compounds, etc., can solve the problems such as the inability to realize efficient cyclic synthesis of chlorinated nitroaniline, and achieves reduction of environmental protection pressure and efficiency. cost, improve efficiency, and promote the effect of dispersing and dissolving
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[0024] The circulation synthetic method flow process of chlorinated nitroaniline of the present invention is as figure 1 shown, including steps:
[0025] (1) Preheating to the chlorination reaction temperature after nitroaniline is mixed with sulfuric acid;
[0026] (2) The solution obtained in step (1) and the chlorine gas are respectively input into the reactor for chlorination reaction, and the material obtained from the reaction is transported to a buffer tank, and the temperature is lowered to obtain a supersaturated solution, and the supersaturated product chlorinated nitroaniline is crystallized simultaneously;
[0027] (3) The material after step (2) cooling is carried out solid-liquid separation, the obtained saturated nitroaniline chloride / sulfuric acid solution is flash evaporated, recycles back to step (1) after reclaiming hydrogen chloride gas and is used for nitroaniline instead of sulfuric acid Dissolved, no need to add additional sulfuric acid at this time, to...
Embodiment 1
[0029] Mix p-nitroaniline with 95wt% sulfuric acid, heat up to 35°C to obtain a sulfuric acid solution of p-nitroaniline, the mass ratio of p-nitroaniline to 95wt% sulfuric acid is 1:3; the solution and chlorine are passed through the advection pump and The gas flowmeter is sent to the supergravity reactor, the molar ratio of p-nitroaniline and chlorine is 1:0.55, the reaction temperature is controlled at 35°C, the pressure is 0.2MPa, and the reaction time is 2.5h; the temperature of the obtained material is cooled to 20°C , solid crystallization, solid-liquid separation, the saturated solution is refluxed to the mixing stage, mixed with p-nitroaniline, and the solid is the product o-chloro-p-nitroaniline. The product was analyzed by chromatography, the purity was 98.7%, and the yield was 98.4%.
Embodiment 2
[0031] Mix 2,4-dinitroaniline with 98wt% sulfuric acid, heat up to 50°C to obtain a sulfuric acid solution of 2,4-dinitroaniline, the mass ratio of 2,4-dinitroaniline to 98wt% sulfuric acid is 1 : 1.5; the solution and chlorine are transported to the supergravity reactor through an advection pump and a gas flow meter respectively, the molar ratio of 2,4-dinitroaniline to chlorine is 1:0.60, the reaction temperature is controlled at 50°C, and the pressure is 0.4 MPa, the reaction time is 2h; the temperature of the material obtained from the reaction is lowered to 25°C, the solid crystallizes out, the solid and liquid are separated, the saturated solution is refluxed to the mixing stage, mixed with 2,4-dinitroaniline, and the solid is the product 2,4-di Nitro-6-chloroaniline. The product was analyzed by chromatography, the purity was 97.4%, and the yield was 97.1%.
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