Chromium oxide and preparation method thereof

A technology of chromium oxide and chromate, applied in the direction of chromium trioxide, chromium oxide/hydrate, nanotechnology, etc., can solve the problems of difficult control of the reaction process, poor performance, low added value, etc., and achieve the goal of avoiding side reactions Effect

Active Publication Date: 2019-02-19
青海省博鸿化工科技股份有限公司 +1
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  • Abstract
  • Description
  • Claims
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AI Technical Summary

Problems solved by technology

The thermal decomposition method of chromic anhydride uses chromic anhydride as raw material and calcines at high temperature to prepare Cr 2 o 3 , this method is expensive and pollutes seriously
The hexavalent chromium salt reduction method uses sulfur or sulfide as a reducing agent to prepare Cr through wet or dry reduction of hexavalent chromium salt. 2 o 3 , mainly include sodium chromate alkaline liquid sulfur or sodium sulfide reduction method, potassium dichromate sulfur roasting reduction method, sodium dichromate ammonium sulfate reduction method, etc. The above methods have a long process and the introduction of impurity sulfur makes it difficult to obtain high-quality products and other issues, and will produce low value-added by-products in the production process
In this method, the reducing gas is introduced in advance, and then the reaction is heated. The reaction process is difficult to control, resulting in uneven composition of the product, poor performance, and the problem of high reaction temperature and pressure.

Method used

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  • Chromium oxide and preparation method thereof

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preparation example Construction

[0057] The specific embodiment part of the present invention provides a kind of preparation method of chromium oxide, described method comprises the following steps:

[0058] (1) Adding the hexavalent chromium salt solution into the reaction device, feeding in the protective gas and raising the temperature in an airtight manner, and continuously feeding in the reducing gas to react after reaching the target temperature to obtain a mixed slurry;

[0059] (2) separating the mixed slurry obtained in step (1) from solid to liquid to obtain chromium oxyhydroxide powder;

[0060] (3) Calcining the chromium oxyhydroxide powder obtained in step (2) to obtain chromium oxide.

Embodiment 1

[0063] The present embodiment provides a kind of preparation method of chromium oxide, described method comprises the following steps:

[0064] (1) Place 200mL of sodium chromate solution with a concentration of 0.2mol / L in a vertical reactor with a volume of 500mL, feed nitrogen to discharge the air in the reactor and the pipeline, heat up after sealing, and reach the target reaction temperature of 250 After ℃, hydrogen gas was introduced to react, and the partial pressure of hydrogen gas was maintained at 5 MPa. After 2 hours of reaction, the temperature was rapidly cooled by water cooling, and the cooling rate was 10 °C / min to obtain a mixed slurry;

[0065] (2) suction-filtering the mixed slurry obtained in step (1) to obtain a solid and a filtrate, the gained solid is washed and dried to obtain a chromium oxyhydroxide powder;

[0066] (3) Calcining the chromium oxyhydroxide powder obtained in step (2) at a temperature of 800° C. for 3 hours to obtain pigment grade chromiu...

Embodiment 2

[0070] The present embodiment provides a kind of preparation method of chromium oxide, described method comprises the following steps:

[0071] (1) Put 200mL of potassium chromate solution with a concentration of 0.6mol / L in a horizontal reactor with a volume of 500mL, feed helium gas to discharge the air in the reactor and pipeline, heat up after sealing, and reach the target reaction temperature After 200°C, hydrogen gas was introduced to react, and the partial pressure of hydrogen gas was maintained at 8MPa. After 4 hours of reaction, the temperature was rapidly cooled by water cooling, and the cooling rate was 5°C / min to obtain a mixed slurry;

[0072] (2) suction-filtering the mixed slurry obtained in step (1) to obtain a solid and a filtrate, the gained solid is washed and dried to obtain a chromium oxyhydroxide powder;

[0073] (3) Calcining the chromium oxyhydroxide powder obtained in step (2) at a temperature of 1000° C. for 1 hour to obtain pigment grade chromium oxi...

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Abstract

The invention provides chromium oxide and a preparation method thereof. The method includes adding a hexavalent chromium salt solution into a reaction device, injecting a protective gas, sealing the reaction device, increasing the temperature, and after a target temperature is reached, injecting a reducing gas continuously for reaction to obtain mixed paste; subjecting the obtained mixed paste tosolid-liquid separation to obtain chromium oxyhydroxide powder; calcinating the chromium oxyhydroxide powder to obtain the chromium oxide. The chromium oxide and the preparation method thereof have the advantages that a hydrothermal reduction method is applied to prepare the chromium oxide from hexavalent chromium salt, the controllability of the reaction process is enhanced through regulation ofthe reducing gas and the reaction conditions, and the reduction rate can reach more than 99%; obtained reduction products have uniform phases and narrow particle size distribution; the obtained chromium oxide products have high quality and can reach the standards of pigment-grade chromium oxide; the method has a short process, low energy consumption, a low cost and no pollutant emission, thereby being a clean production process with remarkable economic benefits.

Description

technical field [0001] The invention belongs to the technical field of material preparation, and relates to a chromium oxide and a preparation method thereof, in particular to a method for preparing pigment grade chromium oxide by hydrothermal reduction. Background technique [0002] Chromium oxide (Cr 2 o 3 ) is an important industrial raw material, which is widely used in the fields of metallurgy, pigments, ceramics, coatings, green polishing, and organic catalytic synthesis. Currently, the industrial production of Cr 2 o 3 The methods mainly include chromic anhydride thermal decomposition method and hexavalent chromium salt reduction method. The thermal decomposition method of chromic anhydride uses chromic anhydride as raw material and calcines at high temperature to prepare Cr 2 o 3 , this method is expensive and pollutes seriously. The hexavalent chromium salt reduction method uses sulfur or sulfide as a reducing agent to prepare Cr through wet or dry reduction ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01G37/033B82Y30/00B82Y40/00
CPCB82Y30/00B82Y40/00C01G37/033C01P2002/72C01P2004/64C01P2006/62C01P2006/63C01P2006/64
Inventor 徐红彬史建斌王劲松张红玲史海琴梅海军刘宏辉杨海王爱山雒敏婷
Owner 青海省博鸿化工科技股份有限公司
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