CN102351251B - Method for extracting ferrotitanium from aluminum oxide dissolution liquid extracted by low-temperature ammonium process - Google Patents

Method for extracting ferrotitanium from aluminum oxide dissolution liquid extracted by low-temperature ammonium process Download PDF

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CN102351251B
CN102351251B CN 201110208730 CN201110208730A CN102351251B CN 102351251 B CN102351251 B CN 102351251B CN 201110208730 CN201110208730 CN 201110208730 CN 201110208730 A CN201110208730 A CN 201110208730A CN 102351251 B CN102351251 B CN 102351251B
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ammonium
aluminum oxide
ferrotitanium
extracting
dissolution fluid
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CN102351251A (en
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张开元
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BEIJING SHIJIDIHE TECHNOLOGY Co Ltd
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BEIJING SHIJIDIHE TECHNOLOGY Co Ltd
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Abstract

The invention relates to a method for extracting ferrotitanium from an aluminum oxide dissolution liquid extracted by a low-temperature ammonium process, which comprises the following steps: cooling the dissolution liquid for crystallization to precipitate aluminum ammonium sulfate crystals, and filtering to obtain a crystalline filtrate and the aluminum ammonium sulfate crystals; while sufficiently stirring the crystalline filtrate, slowly adding ammonia water or introducing ammonia gas to precipitate TiO(OH)2, stopping stirring for sedimentation, and carrying out solid-liquid separation; washing the TiO(OH)2 precipitate with water; while sufficiently stirring the first washing liquid and first solution, continuing adding ammonia water or introducing ammonia gas to precipitate Fe(OH)3, stopping stirring for sedimentation, and carrying out solid-liquid separation; and washing the Fe(OH)3 precipitate with water. The method provided by the invention can be used for extracting iron and titanium from the dissolution liquid, and the other reaction product ammonium sulfate can be sintered together with fly ash, thereby implementing comprehensive utilization of fly ash. The invention hasobvious economic benefit, and implements zero pollutant discharge.

Description

From the aluminum oxide dissolution fluid that uses low temperature ammonium method to extract, extract the method for ferrotitanium
Technical field
The present invention relates to a kind of method of extracting ferrotitanium, relate in particular to a kind of method of from the aluminum oxide dissolution fluid that uses low temperature ammonium method to extract, extracting ferrotitanium.
Background technology
The energy structure of China is still based on coal at present, and the year ash discharge amount of thermal power plant reaches more than hundred million tons.Utilize flyash to extract aluminum oxide and not only meet comprehensive utilization of resources, reduce the environmental requirement of pollutant emission, and can reduce the needs of Nonrenewable resources bauxite.
Low temperature ammonium method is extracted from flyash in the dissolution fluid of aluminum oxide except exsiccated ammonium alum, also contains impurity such as ferric ammonium sulfate, titanyl sulfate.Existing manufacturing technique is not considered to remove these impurity, and the discharging of waste liquid that directly will contain metal ions such as iron, titanium that has has not only increased environmental protection pressure, and wasted useful resources.
Summary of the invention
The present invention is directed to low temperature ammonium method extracts from flyash in the dissolution fluid of aluminum oxide except exsiccated ammonium alum, also contain ferric ammonium sulfate, impurity such as titanyl sulfate, not only can increase environmental protection pressure, and wasted the deficiency of useful resources, a kind of method of extracting ferrotitanium from the aluminum oxide dissolution fluid that uses low temperature ammonium method to extract is provided.
The technical scheme that the present invention solves the problems of the technologies described above is as follows: a kind of method of extracting ferrotitanium from the aluminum oxide dissolution fluid that uses low temperature ammonium method to extract, described aluminum oxide dissolution fluid comprises exsiccated ammonium alum, ferric ammonium sulfate, titanyl sulfate and ammonium sulfate, and this method may further comprise the steps:
Step 1: with the dissolution fluid decrease temperature crystalline, separate out ammonium aluminum sulfate crystal, obtain crystallization filtrate and ammonium aluminum sulfate crystal after the filtration;
Step 2: described crystallization filtrate slowly adds ammoniacal liquor or feeds ammonia under well-beaten condition, and the crystallization pH value of filtrate is transferred to 1.0～2.0, separates out TiO (OH) 2, stop to stir, carry out solid-liquid separation behind sedimentation 0.1～30h, obtain TiO (OH) 2Precipitation and first solution;
Step 3: with described TiO (OH) 2After the precipitation water washs, the TiO (OH) after obtaining washing 2Precipitation and first washing lotion;
Step 4: first washing lotion and first solution under well-beaten condition, are continued to add ammoniacal liquor or feed ammonia, the pH value of first washing lotion and first solution is transferred to 2.8～3.5, separate out Fe (OH) 3, stop to stir, carry out solid-liquid separation behind sedimentation 0.1～30h, obtain Fe (OH) 3Precipitation and second solution;
Step 5: with described Fe (OH) 3After the precipitation water washs, the Fe (OH) after obtaining washing 3Precipitation and second washing lotion.
On the basis of technique scheme, the present invention can also do following improvement.
Further, crystallization filtrate temperature under well-beaten condition remains on 0 ℃～100 ℃ in the described step 2.
Further, the method for carrying out solid-liquid separation in the described step 2 is settling process or filtration method.
Further, the composition of first solution comprises ferric ammonium sulfate and ammonium sulfate in the described step 2.
Further, the composition of first washing lotion comprises ferric ammonium sulfate and ammonium sulfate in the described step 3.
Further, first washing lotion and first solution temperature under well-beaten condition remains on 0 ℃～100 ℃ in the described step 4.
Further, the method for carrying out solid-liquid separation in the described step 4 is settling process or filtration method.
Further, the composition of second solution is ammonium sulfate in the described step 4.
Further, the composition of second washing lotion is ammonium sulfate in the described step 5.
Further, also comprise step 6: second solution and second washing lotion are evaporated obtain ammonium sulfate and be used for flyash batching sintering.
The invention has the beneficial effects as follows: the method that the present invention extracts ferrotitanium can be extracted iron and the titanium in the dissolution fluid, obtains TiO (OH) 2, Fe (OH) 3Deng, another reaction product is ammonium sulfate, can be used for flyash batching sintering, thereby realize the comprehensive utilization of flyash, has tangible economic benefit, and has realized zero release of pollutant.
Description of drawings
Fig. 1 extracts the method flow diagram of the method for ferrotitanium from the aluminum oxide dissolution fluid that uses the extraction of low temperature ammonium method for the present invention.
Embodiment
Below in conjunction with accompanying drawing principle of the present invention and feature are described, institute gives an actual example and only is used for explaining the present invention, is not for limiting scope of the present invention.
The present invention is used for low temperature ammonium method is extracted ferrotitanium from the dissolution fluid of flyash extraction aluminum oxide method, mainly is based on the following principles of chemistry:
Carry titanium: TiOSO 4+ 2NH 3H 2O=TiO (OH) 2+ (NH 4) 2SO 4
Carry iron: NH 4Fe (SO 4) 2+ 3NH 3H 2O=Fe (OH) 3+ 2 (NH 4) 2SO 4
As shown in Figure 1, the raw material that the present invention extracts the method for ferrotitanium extracts the dissolution fluid of aluminum oxide for using low temperature ammonium method from flyash, and the main component of solute is exsiccated ammonium alum NH in this dissolution fluid 4Al (SO 4) 2, ferric ammonium sulfate NH 4Fe (SO 4) 2, titanyl sulfate TiOSO 4, ammonium sulfate (NH 4) 2SO 4Deng, this method may further comprise the steps:
Step 1: with the dissolution fluid decrease temperature crystalline, separate out ammonium aluminum sulfate crystal, obtain crystallization filtrate and ammonium aluminum sulfate crystal after the filtration, ammonium aluminum sulfate crystal is after purifying, for the production of aluminum oxide.
Step 2: crystallization filtrate slowly adds ammoniacal liquor or feeds ammonia under well-beaten condition, and the crystallization pH value of filtrate is transferred to 1.0～2.0, separates out TiO (OH) 2Stop to stir, carry out solid-liquid separation behind sedimentation 0.1～30h, obtain TiO (OH) 2Precipitation and first solution.
Step 3: with TiO (OH) 2After the precipitation water washs, the TiO (OH) after obtaining washing 2Precipitation and first washing lotion, the TiO after the washing (OH) 2Precipitation can be used for producing Chemicals such as titanium dioxide.
Step 4: first washing lotion and first solution under well-beaten condition, are continued to add ammoniacal liquor or feed ammonia, the pH value of first washing lotion and first solution is transferred to 2.8～3.5, separate out Fe (OH) 3Stop to stir, carry out solid-liquid separation behind sedimentation 0.1～30h, obtain Fe (OH) 3Precipitation and second solution.
Step 5:Fe (OH) 3After the precipitation water washs, the Fe (OH) after obtaining washing 3Precipitation and second washing lotion, the Fe after the washing (OH) 3Precipitate Chemicals such as can be used for producing iron oxide red or be used for iron and steel smelting.Second washing lotion and second solution can obtain ammonium sulfate through evaporation, return abovementioned steps and are used for the dissolution fluid of producing aluminum oxide behind the flyash batching sintering.
Embodiment 1
Flyash and ammonium sulfate mix sintering, the gained sintering solid carries out stripping, the dissolution fluid main component and separately concentration be the exsiccated ammonium alum NH of 205g/l 4Al (SO 4) 2, 23g/l ferric ammonium sulfate NH 4Fe (SO 4) 2, 15g/l titanyl sulfate TiOSO 4, the ammonium sulfate (NH of 130g/l 4) 2SO 4, dissolution fluid is cooled to 30 ℃, separate out ammonium aluminum sulfate crystal.Crystallization filtrate slowly adds ammoniacal liquor under 30 ℃ temperature under well-beaten condition, the pH value is transferred to 1.5, separates out TiO (OH) 2Stop to stir, carry out solid-liquid separation behind the sedimentation 2h, obtain TiO (OH) 2Precipitation and first solution.With TiO (OH) 2The precipitation water washs the TiO (OH) after obtaining washing 2Precipitation and first washing lotion, the TiO after the washing (OH) 2Precipitation is dried, wherein, and TiO (OH) 2Foreign matter content be Fe 2O 3: 0.12%, Al 2O 3: 0.04%.First washing lotion and first solution under well-beaten condition, are continued to add ammoniacal liquor under 35 ℃ temperature, the pH value of first washing lotion and first solution is transferred to 3.0, separate out Fe (OH) 3Stop to stir, carry out solid-liquid separation behind the sedimentation 2h, obtain Fe (OH) 3Precipitation and second solution.Fe (OH) 3The precipitation water washs the Fe (OH) after obtaining washing 3Precipitation and second washing lotion, the Fe after the washing (OH) 3Precipitation is dried, wherein, and Fe (OH) 3Foreign matter content be TiO 2: 0.06%, Al 2O 3: 0.61%.Second washing lotion and second solution obtain ammonium sulfate through evaporation, are used for flyash batching sintering.
Embodiment 2
Flyash and ammonium sulfate mix sintering, the gained sintering solid carries out stripping, the dissolution fluid main component and separately concentration be the exsiccated ammonium alum NH of 245g/l 4Al (SO 4) 2, 22g/l ferric ammonium sulfate NH 4Fe (SO 4) 2, 13g/l titanyl sulfate TiOSO 4, the ammonium sulfate (NH of 160g/l 4) 2SO 4, dissolution fluid is cooled to 27 ℃, separate out ammonium aluminum sulfate crystal.Crystallization filtrate slowly feeds ammonia under 45 ℃ temperature under well-beaten condition, the pH value is transferred to 1.8, separates out TiO (OH) 2Stop to stir, carry out solid-liquid separation behind the sedimentation 4h, obtain TiO (OH) 2Precipitation and first solution.With TiO (OH) 2The precipitation water washs the TiO (OH) after obtaining washing 2Precipitation and first washing lotion, the TiO after the washing (OH) 2Precipitation is dried, wherein, and TiO (OH) 2Foreign matter content be Fe 2O 3: 0.09%, Al 2O 3: 0.05%.First washing lotion and first solution under well-beaten condition, are continued to feed ammonia under 45 ℃ temperature, the pH value of first washing lotion and first solution is transferred to 3.4, separate out Fe (OH) 3Stop to stir, carry out solid-liquid separation behind the sedimentation 5h, obtain Fe (OH) 3Precipitation and second solution.Fe (OH) 3The precipitation water washs the Fe (OH) after obtaining washing 3Precipitation and second washing lotion, the Fe after the washing (OH) 3The precipitation oven dry, wherein, Fe (OH) 3Foreign matter content be TiO 2: 0.04%, Al 2O 3: 0.84%.Second washing lotion and second solution obtain ammonium sulfate through evaporation, are used for flyash batching sintering.
Embodiment 3
Flyash and ammonium sulfate mix sintering, the gained sintering solid carries out stripping, the dissolution fluid main component and separately concentration be the exsiccated ammonium alum NH of 235g/l 4Al (SO 4) 2, 26g/l ferric ammonium sulfate NH 4Fe (SO 4) 2, 12g/l titanyl sulfate TiOSO 4, the ammonium sulfate (NH of 143g/l 4) 2SO 4, dissolution fluid is cooled to 35 ℃, separate out ammonium aluminum sulfate crystal.Crystallization filtrate slowly adds ammoniacal liquor under 65 ℃ temperature under well-beaten condition, the pH value is transferred to 1.7, separates out TiO (OH) 2Stop to stir, carry out solid-liquid separation behind the sedimentation 7h, obtain TiO (OH) 2Precipitation and first solution.With TiO (OH) 2The precipitation water washs the TiO (OH) after obtaining washing 2Precipitation and first washing lotion, the TiO after the washing (OH) 2Precipitation is dried, wherein, and TiO (OH) 2Foreign matter content be Fe 2O 3: 0.07%, Al 2O 3: 0.04%.First washing lotion and first solution under well-beaten condition, are continued to feed ammonia under 60 ℃ temperature, the pH value of first washing lotion and first solution is transferred to 3.2, separate out Fe (OH) 3Stop to stir, carry out solid-liquid separation behind the sedimentation 10h and obtain Fe (OH) 3Precipitation and second solution.Fe (OH) 3The precipitation water washs the Fe (OH) after obtaining washing 3Precipitation and second washing lotion, the Fe after the washing (OH) 3Precipitation is dried, wherein, and Fe (OH) 3Foreign matter content be TiO 2: 0.05%, Al 2O 3: 0.70%.Second washing lotion and second solution obtain ammonium sulfate through evaporation, are used for flyash batching sintering.
The above only is preferred embodiment of the present invention, and is in order to limit the present invention, within the spirit and principles in the present invention not all, any modification of doing, is equal to replacement, improvement etc., all should be included within protection scope of the present invention.

Claims (10)

1. method of from the aluminum oxide dissolution fluid that uses low temperature ammonium method to extract, extracting ferrotitanium, described aluminum oxide dissolution fluid comprises exsiccated ammonium alum, ferric ammonium sulfate, titanyl sulfate and ammonium sulfate, it is characterized in that, said method comprising the steps of:
Step 1: with the dissolution fluid decrease temperature crystalline, separate out ammonium aluminum sulfate crystal, obtain crystallization filtrate and ammonium aluminum sulfate crystal after the filtration;
Step 2: described crystallization filtrate slowly adds ammoniacal liquor or feeds ammonia under well-beaten condition, and the crystallization pH value of filtrate is transferred to 1.0～2.0, separates out TiO (OH) 2, stop to stir, carry out solid-liquid separation behind sedimentation 0.1～30h, obtain TiO (OH) 2Precipitation and first solution;
Step 3: with described TiO (OH) 2After the precipitation water washs, the TiO (OH) after obtaining washing 2Precipitation and first washing lotion;
Step 4: first washing lotion and first solution under well-beaten condition, are continued to add ammoniacal liquor or feed ammonia, the pH value of first washing lotion and first solution is transferred to 2.8～3.5, separate out Fe (OH) 3, stop to stir, carry out solid-liquid separation behind sedimentation 0.1～30h, obtain Fe (OH) 3Precipitation and second solution;
Step 5: with described Fe (OH) 3After the precipitation water washs, the Fe (OH) after obtaining washing 3Precipitation and second washing lotion.
2. the method for extracting ferrotitanium from the aluminum oxide dissolution fluid that uses low temperature ammonium method to extract according to claim 1 is characterized in that crystallization filtrate temperature under well-beaten condition remains on 0 ℃～100 ℃ in the described step 2.
3. the method for extracting ferrotitanium from the aluminum oxide dissolution fluid that uses low temperature ammonium method to extract according to claim 1 is characterized in that the method for carrying out solid-liquid separation in the described step 2 is settling process or filtration method.
4. the method for extracting ferrotitanium from the aluminum oxide dissolution fluid that uses low temperature ammonium method to extract according to claim 1 is characterized in that the composition of first solution comprises ferric ammonium sulfate and ammonium sulfate in the described step 2.
5. the method for extracting ferrotitanium from the aluminum oxide dissolution fluid that uses low temperature ammonium method to extract according to claim 1 is characterized in that the composition of first washing lotion comprises ferric ammonium sulfate and ammonium sulfate in the described step 3.
6. the method for extracting ferrotitanium from the aluminum oxide dissolution fluid that uses low temperature ammonium method to extract according to claim 1 is characterized in that first washing lotion and first solution temperature under well-beaten condition remains on 0 ℃～100 ℃ in the described step 4.
7. the method for extracting ferrotitanium from the aluminum oxide dissolution fluid that uses low temperature ammonium method to extract according to claim 1 is characterized in that the method for carrying out solid-liquid separation in the described step 4 is settling process or filtration method.
8. the method for extracting ferrotitanium from the aluminum oxide dissolution fluid that uses low temperature ammonium method to extract according to claim 1 is characterized in that the composition of second solution is ammonium sulfate in the described step 4.
9. the method for extracting ferrotitanium from the aluminum oxide dissolution fluid that uses low temperature ammonium method to extract according to claim 1 is characterized in that the composition of second washing lotion is ammonium sulfate in the described step 5.
10. according to the arbitrary described method of from the aluminum oxide dissolution fluid that uses low temperature ammonium method to extract, extracting ferrotitanium of claim 1 to 9, it is characterized in that, also comprise step 6: second solution and second washing lotion are evaporated obtain ammonium sulfate and be used for flyash batching sintering.
CN 201110208730 2011-07-25 2011-07-25 Method for extracting ferrotitanium from aluminum oxide dissolution liquid extracted by low-temperature ammonium process Active CN102351251B (en)

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US4159310A (en) * 1978-01-30 1979-06-26 Public Service Company Of New Mexico Process for recovering aluminum and other metal values from fly ash
CN100572279C (en) * 2007-07-12 2009-12-23 中国铝业股份有限公司 A kind of method of alumina of from flyash, extracting
CN101157456A (en) * 2007-09-11 2008-04-09 李禹� Comprehensive utilization method of ammonium sulfate and pulverized coal ash produced by thermal power plant ammonia process
CN102120600B (en) * 2010-01-08 2012-11-07 北京世纪地和科技有限公司 Method for purifying aluminum ammonium sulfate

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