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Method for producing iron oxide black with fluorine-titanium mother liquor

A technology of iron oxide black and mother liquor, which is applied in the field of inorganic pigments, can solve the problems of wasting iron resources and environmental pollution, and achieve the effects of reducing energy consumption and production costs, increasing economic benefits, and good use effects

Active Publication Date: 2019-03-19
山东格林凯瑞精密仪器有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0003] At present, there is no effective method to reuse the fluorine-titanium mother liquor. Usually, the method of treating the fluoride-titanium mother liquor is to neutralize the storm gas, press filter the waste liquid and store it as waste residue, but this will pollute the environment. , and a waste of iron resources

Method used

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  • Method for producing iron oxide black with fluorine-titanium mother liquor
  • Method for producing iron oxide black with fluorine-titanium mother liquor

Examples

Experimental program
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Effect test

Embodiment 1

[0046] Take about 4000ml of fluorine-titanium mother liquor in a 5L beaker, add excess small iron pieces, heat to 50-60°C, react until the solution pH=4.0, filter with suction, and filter out the precipitated Ti(OH) 3 , and analyze ferrous chloride concentration (expressed as Fe) in the filtrate to be 86g / L; Get ferrous chloride solution 2090ml in 5L beaker, add water 910ml to adjust ferrous chloride concentration, stir, add concentration 15% ammoniacal liquor Neutralize and adjust to PH=10; heat to 90°C, slowly add 380ml of sodium chlorate solution with a concentration of 10%, keep the pH value in the range of 8.5-9.0 during the oxidation process, and the temperature is 90-95°C. After the sodium chlorate is added, the reaction is completed, the slurry is suction filtered, the filter cake is washed with water until the conductivity of the washing water is less than 1000 μs / cm, and then dried in an oven to obtain iron oxide black.

Embodiment 2

[0048] Take about 4000ml of fluoride-titanium mother liquor in a 5L beaker, add excess small iron pieces, heat to 60-70°C, react until the solution pH=4.5, filter with suction, and filter out the precipitated Ti(OH) 3, and analyze the ferrous chloride concentration (expressed as Fe) in the filtrate to be 89.2g / L; Get ferrous chloride solution 2180ml in the 5L beaker, add water 820ml to adjust the concentration of ferrous chloride, stir well, add concentration 15 Neutralize with % ammonia water and adjust to PH=9; heat to 93°C, slowly add 410ml of sodium chlorate solution with a concentration of 10%, keep the pH value in the range of 7.5 to 8.5 during the oxidation process, and the temperature is 93 to 95°C. After the sodium chlorate is added, the reaction is completed, the slurry is suction filtered, the filter cake is washed with water until the conductivity of the washing water is less than 1000 μs / cm, and then dried in an oven to obtain iron oxide black.

Embodiment 3

[0050] Take about 4000ml of fluorine-titanium mother liquor in a 5L beaker, add excess small iron pieces, heat to 70-80°C, react until the solution pH=4.5, filter with suction, and filter out the precipitated Ti(OH) 3 , and analyze ferrous chloride concentration (expressed as Fe) in the filtrate to be 88.5g / L; Get ferrous chloride solution 1865ml in 5L beaker, add water 1135ml to adjust filtrate concentration, stir, add concentration 15% ammoniacal liquor to neutralize , adjusted to PH=8.5; heated to 95°C, slowly adding 350ml of sodium chlorate solution with a concentration of 10%, keeping the pH value in the range of 7.0 to 8.0 during the oxidation process, and the temperature at 95 to 100°C. After the sodium chlorate is added, the reaction is completed, the slurry is suction filtered, the filter cake is washed with water until the conductivity of the washing water is less than 1000 μs / cm, and then dried in an oven to obtain iron oxide black.

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Abstract

The invention discloses a method for producing black iron oxide by adopting a fluorine titanium mother solution. The method comprises the following steps: adding an iron sheet into the fluorine titanium mother solution and reacting to obtain a ferrous chloride solution; neutralizing the acquired ferrous chloride solution with ammonium hydroxide to generate ferrous hydroxide gel; heating the acquired ferrous hydroxide gel and adding sodium chlorate for oxidizing, thus obtaining black iron oxide slurry; filtering, washing, drying and crushing the acquired black iron oxide slurry, thus obtaining the black iron oxide. According to the invention, the sodium chlorate is used as an oxidizing agent, so that a reaction endpoint can be easily judged, the product quality is higher, and the energy consumption and the production cost are both lower than those according to an air oxidation method; the oxidizing reaction is high in speed, so that the production capacity of the equipment can be greatly increased and the energy consumption and the production cost can be reduced; the blue phase value of the prepared black iron oxide is considerably higher than that of the traditional iron black product; the application of the black iron oxide to inner and outer wall coatings has a better use effect; tail gas is hardly generated; the environmental pollution is reduced; the economic benefit of the enterprise is increased.

Description

technical field [0001] The invention relates to the field of inorganic pigments, in particular to a method for producing iron oxide black by using titanium fluoride mother liquor. Background technique [0002] Potassium fluorotitanate is a colorless monoclinic flaky crystal or white powder, mainly used as a metallurgical additive for titanium alloys. At present, the main production process of potassium fluotitanate is that ilmenite is dissolved in hydrofluoric acid to generate ferrous fluotitanate solution, and the filtrate is filtered and then reacted with potassium chloride solution to obtain potassium fluotitanate. However, in the process of producing potassium fluorotitanate, fluoride titanium mother liquor will be produced, and the main components of fluoride titanium mother liquor are ferrous chloride and ferric chloride. [0003] At present, there is no effective method to reuse the fluorine-titanium mother liquor. Usually, the method of treating the fluoride-titaniu...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C01G49/08
CPCC01G49/08
Inventor 黄平峰张程程熬
Owner 山东格林凯瑞精密仪器有限公司
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