Method for preparing rutile type titanium dioxide by using ilmenite as raw material

A technology for preparing ilmenite and gold, which is applied in the direction of titanium dioxide, titanium oxide/hydroxide, etc., can solve the problems of high cost of three wastes treatment, large waste discharge, complicated process, etc., to reduce equipment costs, increase production, and improve extraction rate effect

Active Publication Date: 2015-06-24
HAINAN UNIVERSITY
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  • Abstract
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  • Claims
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Problems solved by technology

However, the process is complex and requires nearly 20 process steps. Each process step must be strictly controlled in order to produce the best quality titanium dioxide products and meet the optimal performance of the pigment.
Because the traditional sulfuric acid method uses sulfuric acid with a high concentration, it discharges a lot of waste and causes serious pollution, and the treatment of the three wastes costs a lot

Method used

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  • Method for preparing rutile type titanium dioxide by using ilmenite as raw material
  • Method for preparing rutile type titanium dioxide by using ilmenite as raw material
  • Method for preparing rutile type titanium dioxide by using ilmenite as raw material

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Effect test

Embodiment 1

[0029] Such as figure 1 As shown, the ilmenite is ground and pulverized through a 300 mesh sieve, and the raw material with a mass of 75.00 g is pressed by m (ilmenite): m ((NH4) 2 SO 4 ):m(K 2 S 2 o 7 ) = 1:4:0.5, grind evenly, put it into the calciner, the reaction temperature is 360°C, and the holding time is 1h. Ammonia gas absorption is 18-20% ammonia water. Take the roasted ilmenite, put it into a three-necked flask after grinding, add 300ml of 30% dilute sulfuric acid for leaching, the leaching temperature is 65°C, and the leaching time is 10h, then add about 2.50g of iron filings to reduce for 4 hours. Under these conditions, the leaching rate of titanium reaches 96.82%. Concentrate the titanium solution, the volume ratio before and after concentration is 0.73, and then remove iron by freezing, the iron removal temperature is -15 °C, and the iron removal rate can reach 50.64% when the time is more than 15 hours. Ferrous sulfate is neutralized with ammonia water...

Embodiment 2

[0031] The ilmenite is crushed through a 350 mesh sieve, and the raw material with a quality of 75.05g is pressed by m (ilmenite): m ((NH4) 2 SO 4 ):m(K 2 S 2 o 7)=1:5:0.5 calcined. The calcination temperature is 400° C., the holding time is 30 minutes, and the ammonia gas absorption is 18-20% ammonia water. Add 300ml, 20% dilute sulfuric acid for leaching, the leaching temperature is 60°C, the leaching time is 8h, and then add about 2.50g of iron filings for reduction for 4 hours. Under these conditions, the leaching rate of titanium reaches 96.82%. Concentrate the titanium solution to 0.5 times the original volume, then the iron can be removed by freezing. The iron removal temperature is -16°C, and the iron removal rate can reach 50.64% when the time is more than 15 hours. The titanium solution is concentrated at about 65°C, and the concentration ratio is 0.55. 7% by weight of the concentrated titanium liquid is used as the raw material for producing rutile-type seed ...

Embodiment 3

[0033] When calcining, the raw material is m (ilmenite): m ((NH4) 2 SO 4 ):m(K 2 S 2 o 7 )=1:6:0.5, the total mineral mass is 75.00g, the reaction temperature is 450°C, the holding time is 1.5h, and the ammonia gas absorption is 18-20% ammonia water. Add 300ml, 30% dilute sulfuric acid for leaching, the leaching temperature is 70°C, the leaching time is 10h, and then add about 2.50g of iron filings for reduction for 4 hours. After suction filtration, the leaching solution is concentrated, with a concentration ratio of 0.7; then, iron removal is performed by freezing at a temperature of -18°C, and the iron removal rate can reach 46.23% when the time is more than 16 hours. After removing iron, concentrate the titanium liquid at about 65°C, and the concentration ratio is 0.6. 7% by weight of the concentrated titanium liquid is used as the raw material for producing rutile-type seed crystals, zinc oxide is added to the seed crystal raw material, the pH value is adjusted at 2....

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Abstract

The invention discloses a method for preparing rutile type titanium dioxide by using ilmenite as a raw material. The method comprises the steps of grinding ilmenite, calcining, extracting, freezing to remove iron, concentrating titaniferous solution, hydrolyzing titaniferous solution, rinsing, treating with salt and calcining. The method has the beneficial effects that: (1) high equipment cost generated by using high-concentration sulfuric acid is reduced by means of the process; (2) temperature for calcining is reduced by adding potassium pyrosulfate, and the extraction rate of titanium dioxide is greatly improved; (3) ammonium sulfate is generated from ammonia generated in calcining and waste acid generated in hydrolyzing and is recycled, the important problem of 'three wastes' is solved, and environmental friendliness is achieved; (4) a proper amount of rutile seed crystal is added under a certain condition in the hydrolyzing process, the yield of rutile type titanium dioxide is greatly increased; and (5) the temperature of crystal form transformation is reduced, rutile type crystal phase transformation can be obtained at 110 DEG C, and the calcining time is shortened to 2 hours.

Description

technical field [0001] The invention relates to a method for preparing rutile titanium dioxide by extracting titanium from ilmenite, belonging to the production field of rutile titanium dioxide. Background technique [0002] Titanium dioxide is currently the best and irreplaceable white inorganic chemical pigment. It is widely used in coatings, rubber, plastics, papermaking, printing inks, daily chemicals and other fields. There are four processes for its production: sulfuric acid method, chlorination method, hydrochloric acid method, and alkali method. The production process of titanium dioxide by the chloride method is internationally recognized as a new generation of advanced technology that replaces the sulfuric acid method because of its environmental protection in the production process and high product quality. At present, the production capacity ratio of the global chloride titanium dioxide and sulfuric acid titanium dioxide is about 6:4. In developed countries in...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01G23/047
CPCC01G23/047
Inventor 徐树英张德拉张玉苍张永明陈亚楠卢春朗
Owner HAINAN UNIVERSITY
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