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Method for purifying para-fluoroaniline industrial product by adopting acid extraction technique
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A technology for p-fluoroaniline and industrial products, applied in the field of purifying p-fluoroaniline industrial products, can solve the problems that have not been seen before, and achieve the effects of low cost, simple process and strong economic benefits
Inactive Publication Date: 2012-12-19
吕*泉
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Problems solved by technology
[0005] Regarding the purification of p-fluoroaniline industrial products, there are no literature reports and patented technologies that adopt the same or similar methods as this patent
Method used
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Examples
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Embodiment 1
[0021] The crude product of p-fluoroaniline in this example contains 99.42% p-fluoroaniline, 0.13% aniline, 0.24% o-fluoroaniline, 0.19% m-fluoroaniline and 37ppm iron in the crude product.
[0022] (1) In the separatory funnel, add 35-50mL10 -2 mol / L hydrochloric acid solution, 100mL crude product of p-fluoroaniline, after mixing, shaking for 10 minutes, standing still for 5-10 minutes, and layering, release the organic phase and the water phase successively, and repeat 2-3 times to extract the organic phase. Combine the aqueous phase and discard, and the organic phase (note A) is followed up;
[0023] (2) Take the organic phase A and 150-200mL 2mol / L hydrochloric acid solution that have been processed in (1) and place them in a separatory funnel, mix and shake for 10 minutes, let stand for 5-10 minutes, and separate the layers. Add an appropriate amount of 0.5mol / L hydrochloric acid drop by volume, shake for 10 minutes, let stand for 5-10 minutes, and separate layers. When ...
Embodiment 2
[0028] Add aniline, o-fluoroaniline and m-fluoroaniline to the same p-fluoroaniline crude product as in Example 1, so that the crude product contains 99.04% p-fluoroaniline, 0.43% aniline, 0.31% o-fluoroaniline, and 0.22% m-fluoroaniline Aniline and 34 ppm iron.
[0029] According to the same operating procedure and consumption as in Example 1, the crude product added to aniline, o-fluoroaniline and m-fluoroaniline was subjected to acid extraction and purification, and was respectively used for 10 -2 mol / L sulfuric acid, nitric acid solution instead of 10 -2 mol / L hydrochloric acid solution, 2mol / L sulfuric acid, nitric acid solution replace 2mol / L hydrochloric acid solution, and 0.1mol / L sodium carbonate or sodium bicarbonate solution replace sodium hydroxide solution, all can obtain the similar pair of purification effect with embodiment 1 Fluoroaniline industrial products.
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Abstract
The invention discloses a method for purifying p-fluoroaniline industrial products by using acid extraction technology. In the method, a 10-2 mol / L acid solution of 1 / 3 to 1 / 2 times the volume of p-fluoroaniline is used as an extraction agent to extract A small amount of impurities such as aniline and salts; then first use 2mol / L acid solution with 1.5 to 2.0 times the volume of p-fluoroaniline as the extraction agent to convert p-fluoroaniline into water-soluble substances, so as to realize the removal of impurities such as o-fluoroaniline and m-fluoroaniline In the separation from p-fluoroaniline, the water-soluble substance is washed with alkali and water to obtain high-purity p-fluoroaniline industrial products. This method has simple process, good treatment effect, low input cost, and the obtained p-fluoroaniline industrial products have high purity.
Description
(1) Technical field: [0001] The invention relates to a method for purifying p-fluoroaniline industrial products by using acid extraction technology. (two) background technology: [0002] p-Fluoroaniline is an important fine chemical product, widely used in medicine, pesticide, dyestuff, photosensitive material industry, especially fluorine-containing drugs have special biological activity and chemical properties, it is a low toxicity and high efficiency that has developed rapidly in the past ten years new drug. It is used as an intermediate in the synthesis of various fluorine-containing antibiotics, anti-epileptic psychosis, and ulcer treatment drugs, as well as agricultural plant growth regulators, herbicides, insecticides, and certain dyes, bringing obvious economic benefits and strong market competition. power, has aroused people's great attention. [0003] The development of p-fluoroaniline industrial products was earlier in foreign countries, while it started in the ...
Claims
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