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Preparation of iron oxide black with side product of iron reduction process to prepare amino phenol

An aminophenol, iron oxide black technology, applied in ferrous oxide, iron oxide/iron hydroxide, organic chemistry and other directions, can solve problems such as environmental pollution and resource waste, reduce environmental pollution and improve utilization rate Effect

Inactive Publication Date: 2006-05-10
湖北开元化工科技股份有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

At this time, nitrophenol is reduced to aminophenol, and iron powder becomes iron sludge waste residue. The main component of iron sludge waste residue is ferric oxide. Failure to treat iron sludge waste residue causes environmental pollution and waste of resources.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0013] Add 105 grams of iron powder (more than 92% iron), 300ml of water, 10ml of HCl, and 2 grams of catalyst ammonium chloride into a 500ml beaker, heat to boiling, slowly add 100 grams of nitrophenol, and keep warm until the end point is pH5. Continue to react for 2 hours, filter, and collect the filtrate for crystallization to prepare aminophenol. Pass the iron mud through a 25-mesh sieve, and wash the iron mud with hot water above 70 degrees until there is no organic matter. Dry at 90±5°C and grind to obtain the finished product.

Embodiment 2

[0015] Add 120Kg of iron powder (more than 92% iron), 500L of water, 15L of HCl, and 5Kg of catalyst copper sulfate into a 1000L reactor, stir and heat to boiling, slowly add 100Kg of nitrophenol, keep warm until the end point is pH 7, and continue the reaction After 5 hours, filter and collect the filtrate for crystallization to prepare aminophenol. Add water to the iron mud and pass it through a 325-mesh sieve, and wash the iron mud with hot water above 70 degrees until there is no organic matter. Dry at 105±5°C and grind to obtain the finished product.

Embodiment 3

[0017] Add 500Kg of nitrophenol and 4000L of water into a 5000L reactor and heat to boiling. Add 100L hydrochloric acid, slowly add 650Kg iron powder, 30Kg catalyst copper sulfate. After reacting in a boiling state until the acidity of the solution reaches PH8, continue the reaction for 12 hours, stop the reaction, filter with plate and frame, and collect the filtrate for crystallization to prepare aminophenol. Add iron mud to the 3000L pit, add water to adjust the slurry, pump the slurry into a 325-mesh drum sieve for sieving, pump the underscreen into a 5000L washing tank, add hot water above 70 degrees to wash repeatedly for 5 -8 times until organic free. Then press filter the slurry, send the solid phase into a rotary flash dryer, control the feed temperature at 80-320°C, and control the discharge temperature at 50-170°C to obtain a finished product.

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PUM

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Abstract

A method for preparing iron oxide black by recovering by-products in the iron powder reduction process of aminophenol production. The main process is to add nitrophenol, iron powder, and hydrochloric acid to the reduction kettle, add a catalyst, heat the reaction until boiling, and stir After reacting to a pH value of 5-8, keep boiling. After filtering, the filtrate is collected and used for crystallization to prepare aminophenol. The solid phase, that is, iron sludge, is washed with water, filtered, dried, and then ground to obtain a finished product. The method can fully integrate the iron sludge in the aminophenol production process into ferric oxide, and obtain iron oxide black products after further treatment, thereby improving resource utilization and reducing environmental pollution caused by iron sludge discharge.

Description

technical field [0001] The invention relates to a method for preparing iron oxide black, in particular to a method for preparing iron oxide black from by-products in the process of preparing aminophenol. Background technique [0002] The traditional method of preparing iron oxide black is to dissolve the iron sheet with sulfuric acid to make a ferrous sulfate solution, then neutralize it with alkali, so that the ferrous iron in the solution first forms ferrous hydroxide precipitation, and then dissolves the ferrous hydroxide Heating and passing air for oxidation, or directly combining ferrous hydroxide and iron oxide in a certain proportion, the production cost of this process is relatively high. When nitrophenol is used as a raw material to prepare aminophenol, iron powder is usually added as a reducing agent to undergo redox with nitrophenol. At this time, nitrophenol is reduced to aminophenol, and iron powder becomes iron sludge waste residue. The main component of iron ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C01G49/08C07C215/76
Inventor 胡修权
Owner 湖北开元化工科技股份有限公司