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Novel method for preparing metaaminophenol by reducing metanitrophenol with byproduct ammonium thiosulfate recovered from coking desulfurization waste liquid

A technology for coking desulfurization waste liquid and ammonium thiosulfate, which is applied in the field of comprehensive utilization of waste resources, can solve the problems of serious environmental pollution, inconvenient use, and many three wastes, etc., and achieves the effects of simple process, simple equipment, and improved economic benefits.

Inactive Publication Date: 2015-06-10
苏州久王环保科技股份有限公司 +1
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  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0002] Meta-aminophenol is an important organic intermediate, which has a wide range of uses in medicine, dyes, pesticides, metal corrosion inhibitors in alkaline media, and other aspects. However, the existing production methods of meta-aminophenol include nitrobenzene sulfonation Alkali fusion method, m-phenylenediamine hydrolysis method, aniline hydroxylation method, resorcinol ammonification method, etc.; these methods have low productivity, many wastes, and pollute the environment; at present, nitrobenzene sulfonated alkali is mostly used in the production of m-aminophenol in China Melting method and nitrobenzene oleum sulfonation method cause serious environmental pollution; it has been reported that m-nitrophenol is prepared by decomposing and reducing m-nitrophenol in an alcoholic acid solution with a drop Hg electrode, although the Hg electrode has a high hydrogen evolution potential , but due to serious pollution and inconvenient use, its development is limited; and China is the largest steel producer in the world, which makes the coking industry closely related to the steelmaking industry continue to expand; extract sulfur from coke oven gas desulfurization waste liquid Ammonium sulfosulfate has also become a popular process. For this reason, we have developed a new method to prepare m-aminophenol by reducing m-nitrophenol with ammonium thiosulfate, a by-product recovered from coking desulfurization waste liquid, to realize the reuse of waste resources. Utilization and safety and environmental protection, simple process, simple equipment, suitable for industrialized continuous production

Method used

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  • Novel method for preparing metaaminophenol by reducing metanitrophenol with byproduct ammonium thiosulfate recovered from coking desulfurization waste liquid

Examples

Experimental program
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Effect test

Embodiment 1

[0015] Embodiment 1: In four-neck bottle, add 1g m-nitrophenol. Then 20ml of ethanol and 10ml of water were added. Start heating and stirring; After all dissolving, add 6g purity and be 96.1% ammonium thiosulfate (NH 4 ) 2 S 2 o 3； Make it all dissolve; Reflux reaction at 80 DEG C; Stop reaction after 4 hours, cool to room temperature naturally; Have white crystal to separate out, the crystal that suction filtration separates out; Obtain product m-aminophenol after complete drying; Weighing is 0.71g, The yield is about 91%.

Embodiment 2

[0016] Embodiment 2: in four-neck bottle, add 1g m-nitrophenol. Then 80ml of ethanol and 40ml of water were added. Start heating and stirring. After all dissolving, add 6g purity and be 96.1% ammonium thiosulfate (NH 4 ) 2 S 2 o 3 . Let it all dissolve. The reaction was refluxed at 80°C. After 4 hours, the reaction was stopped and cooled to room temperature naturally. White crystals were precipitated, and the precipitated crystals were filtered with suction. The product is obtained after complete drying: m-aminophenol. The weighed weight was 0.68g. The yield is about 87.2%.

Embodiment 3

[0017] Embodiment 3: in four-neck bottle, add 1g m-nitrophenol. Then 200ml of ethanol and 80ml of water were added. Start heating and stirring. After all dissolving, add 6g purity and be 96.1% ammonium thiosulfate (NH 4 ) 2 S 2 o 3 . Let it all dissolve. The reaction was refluxed at 80°C. After 4 hours, the reaction was stopped and cooled to room temperature naturally. White crystals were precipitated, and the precipitated crystals were filtered with suction. The product is obtained after complete drying: m-aminophenol. The weighed was 0.74 g. The yield is about 94.9%.

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Abstract

The invention relates to a novel method for preparing metaaminophenol by reducing metanitrophenol with a byproduct ammonium thiosulfate recovered from a coking desulfurization waste liquid, which comprises the following steps: adding the raw material metanitrophenol into an organic solvent-water mixed solution, stirring, completely dissolving, adding an ammonium thiosulfate reducer, heating, naturally cooling to room temperature to precipitate a crystal, carrying out vacuum filtration to obtain the crystal, and completely drying to obtain the metaaminophenol. By using the byproduct ammonium thiosulfate recovered from the coking desulfurization waste liquid as the reducer, the method reutilizes the waste resources, enhances the economic benefit, has the advantages of high safety, environment friendliness, convenient technique and simple equipment, and is suitable for industrialized continuous production.

Description

technical field [0001] The invention relates to the field of comprehensive utilization of waste resources, in particular to a new method for preparing m-aminophenol by reducing m-nitrophenol with by-product ammonium thiosulfate recovered from coking desulfurization waste liquid. Background technique [0002] Meta-aminophenol is an important organic intermediate, which has a wide range of uses in medicine, dyes, pesticides, metal corrosion inhibitors in alkaline media, and other aspects. However, the existing production methods of meta-aminophenol include nitrobenzene sulfonation Alkali fusion method, m-phenylenediamine hydrolysis method, aniline hydroxylation method, resorcinol ammonification method, etc.; these methods have low productivity, many wastes, and pollute the environment; at present, nitrobenzene sulfonated alkali is mostly used in the production of m-aminophenol in China Melting method and nitrobenzene oleum sulfonation method cause serious environmental polluti...

Claims

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Application Information

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IPC IPC(8): C07C215/76C07C213/02
Inventor 张超智孙晓飞王宏明顾智杰
Owner 苏州久王环保科技股份有限公司
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