CN102491346A - Method for preparing white carbon black from aluminum oxide red mud - Google Patents
Method for preparing white carbon black from aluminum oxide red mud Download PDFInfo
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- CN102491346A CN102491346A CN2011103948093A CN201110394809A CN102491346A CN 102491346 A CN102491346 A CN 102491346A CN 2011103948093 A CN2011103948093 A CN 2011103948093A CN 201110394809 A CN201110394809 A CN 201110394809A CN 102491346 A CN102491346 A CN 102491346A
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- leached mud
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- white carbon
- hydrochloric acid
- carbon black
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Abstract
The invention relates to a method for preparing white carbon black from aluminum oxide red mud and belongs to the technical field of white carbon block preparation. The invention aims at solving the technical problem to provide the method for effectively solving the recovery and utilization problem of the aluminum oxide red mud and reducing the solid pollutant discharge of the aluminum oxide red mud. The method adopts the technical scheme of comprising the following steps of: 1, preparing primary leaching solution and primary leaching slag; 2, preparing secondary leaching solution and secondary leaching slag; and 3, preparing the white carbon black. The method has the advantages that the leaching slag is effectively utilized, the aluminum oxide red mud is directly recovered and utilized, the solid pollutant discharge of the aluminum oxide red mud is reduced, and great social and economic benefits are realized.
Description
Technical field
A kind of method for preparing WHITE CARBON BLACK with alumina laterite of the present invention belongs to preparation WHITE CARBON BLACK technical field.
Background technology
Alumina laterite is the waste in the aluminum oxide production process.According to grade alumina silica ratio (A/S) difference of various places bauxite, 1 ton of aluminum oxide of every production does not wait with regard to 1.0～1.4 tons of red muds of by-product.About 6,000 ten thousand tons of the red mud of the annual generation in the whole world at present, according to annual statistics in 2010, China's aluminum oxide output was about 2,700 ten thousand tons, if calculate by 1.2 tons of red muds of aluminum oxide generation per ton, the annual red mud that produces of China is about 3,240 ten thousand tons.Red mud is an alkaline matter, is prone to the alkalization soil, polluted underground water, serious harm health of people.Simultaneously, contain valuable constituents such as rare metal, rare earth metal, aluminium, iron, silicon in the alumina laterite.Leaching with hydrochloric acid in the process of aluminium, iron, calcium, REE and yttrium in the red mud; Can obtain a large amount of leached muds; The staple of leached mud is a silicon-dioxide, just becomes an important problem so how can effectively recycle these leached muds.
Summary of the invention
A kind of method for preparing WHITE CARBON BLACK with alumina laterite of the present invention provides a kind of recycling of effective solution alumina laterite, reduces the method for alumina laterite solid pollutant discharging.
For solving the above problem, the technical scheme that the present invention adopts is to operate according to following steps:
The first step prepares a leach liquor and a leached mud
Alumina laterite is put into stirred autoclave, leach alumina laterite with hydrochloric acid soln, the leaching reaction conditions is:
Hydrochloric acid soln and red mud weight part ratio are 3-6:1, and the hydrochloric acid soln volumetric molar concentration is 4-8mol/L, and extraction temperature is 70-105 ℃, and extraction time is 60-360min;
Leaching slurry after leaching is carried out solid-liquid separation with pressure filter, obtain a leach liquor and a leached mud, and with leached mud of water washing, said water and a leached mud weight part ratio are 2-4:1;
Second step, preparation secondary leach liquor and secondary leached mud
A said leached mud is put into reaction kettle, add hydrochloric acid and leach; The secondary leaching condition is: extraction temperature is 70-105 ℃, and extraction time is 60-360min, and the hydrochloric acid soln volumetric molar concentration is 4-8mol/L, and hydrochloric acid and a leached mud weight part ratio are 3-6:1;
Secondary leaching slurry after leaching is carried out solid-liquid separation with pressure filter, obtain secondary leach liquor and secondary leached mud; And with water washing secondary leached mud twice, said water and secondary leached mud weight part ratio are 3:1;
The 3rd step, the preparation WHITE CARBON BLACK
Repeat above-mentioned second step operation, obtain leaching solid; Said leaching solid is dried to constant weight under 105-110 ℃ in loft drier; Leaching solid after will drying is then put into electric furnace, at temperature 200-500 ℃ of roasting 40-90min, makes WHITE CARBON BLACK after the pulverizing.
In the said the first step, leached mud of water washing 1-3 time; A said leach liquor is used to extract REE, aluminium and iron.
In said the 3rd step, the number of times that repeats the operation of second step is 3-6 time.
The beneficial effect that the present invention has is: leaching with hydrochloric acid in the process of aluminium, iron, calcium, REE and yttrium in the alumina laterite; Can obtain a large amount of leached muds; The present invention has effectively utilized these leached muds; Directly recycle alumina laterite, reduced the discharging of alumina laterite solid pollutant, had important social and economic benefit.
Embodiment
Producing alumina laterite with middle aluminium Company Shanxi Branch alumina producing Bayer process is example, and chemical constitution is:
| Composition % | Al 2O 3 | SiO 2 | CaO | Fe 2O 3 | Na 2O | REO | Sc 2O 3 | TiO 2 | Alkali burns |
| Content % | 23.60 | 17.44 | 20.24 | 4.18 | 8.57 | 0.31 | 0.02 | 6.94 | 11.51 |
Ward off the glass stirred autoclave: Zibo China star chemical plant factory; Model, K10000
Chamber(filter)press: female source, Hangzhou filter ltd; Model, XMY60/800-UK
Acid: the special chemical pump industry of Anhui fluorine ltd; Model, the centrifugal acid of IHF65-40-250
Loft drier: go up seascape and step plant and instrument ltd; Model, 101A-4C
Cabinet-type electric furnace: the rich electric furnace of Yixing City space Manufacturing Co., Ltd; Model, RX3-30-9
Disintegrating apparatus: the big prosperous machinofacture in Zhengzhou ltd; Model, the 3R1510 Raymond mill
Embodiment 1
A kind ofly prepare the method for WHITE CARBON BLACK, operate according to following steps with alumina laterite:
The first step prepares a leach liquor and a leached mud
Alumina laterite is put into stirred autoclave, leach alumina laterite with hydrochloric acid soln, the leaching reaction conditions is:
Hydrochloric acid soln and red mud weight part ratio are 3.5:1, and the hydrochloric acid soln volumetric molar concentration is 7mol/L, and extraction temperature is 75 ℃, and extraction time is 250min;
Leaching slurry after leaching is carried out solid-liquid separation with pressure filter, obtain a leach liquor and a leached mud, and with leached mud of water washing 1 time, said water and a leached mud weight part ratio are 2.5:1; A said leach liquor is used to extract REE, aluminium and iron.
Second step, preparation secondary leach liquor and secondary leached mud
A said leached mud is put into reaction kettle, add hydrochloric acid and leach; The secondary leaching condition is: extraction temperature is 100 ℃, and extraction time is 80min, and the hydrochloric acid soln volumetric molar concentration is 7mol/L, and hydrochloric acid and a leached mud weight part ratio are 3.5:1;
Secondary leaching slurry after leaching is carried out solid-liquid separation with pressure filter, obtain secondary leach liquor and secondary leached mud; And with water washing secondary leached mud twice, said water and secondary leached mud weight part ratio are 3:1;
The 3rd step, the preparation WHITE CARBON BLACK
Repeat the above-mentioned second step operation 5 times, obtain leaching solid; Said leaching solid is dried to constant weight under 105-110 ℃ in loft drier; Leaching solid after will drying is then put into electric furnace, at 220 ℃ of roasting 85min of temperature, makes WHITE CARBON BLACK after the pulverizing.
Embodiment 2
A kind ofly prepare the method for WHITE CARBON BLACK, operate according to following steps with alumina laterite:
The first step prepares a leach liquor and a leached mud
Alumina laterite is put into stirred autoclave, leach alumina laterite with hydrochloric acid soln, the leaching reaction conditions is:
Hydrochloric acid soln and red mud weight part ratio are 5.5:1, and the hydrochloric acid soln volumetric molar concentration is 4.5mol/L, and extraction temperature is 100 ℃, and extraction time is 80min;
Leaching slurry after leaching is carried out solid-liquid separation with pressure filter, obtain a leach liquor and a leached mud, and with leached mud of water washing 2 times, said water and a leached mud weight part ratio are 3.2:1; A said leach liquor is used to extract REE, aluminium and iron.
Second step, preparation secondary leach liquor and secondary leached mud
A said leached mud is put into reaction kettle, add hydrochloric acid and leach; The secondary leaching condition is: extraction temperature is 83 ℃, and extraction time is 190min, and the hydrochloric acid soln volumetric molar concentration is 4.5mol/L, and hydrochloric acid and a leached mud weight part ratio are 5.5:1;
Secondary leaching slurry after leaching is carried out solid-liquid separation with pressure filter, obtain secondary leach liquor and secondary leached mud; And with water washing secondary leached mud twice, said water and secondary leached mud weight part ratio are 3:1;
The 3rd step, the preparation WHITE CARBON BLACK
Repeat the above-mentioned second step operation 4 times, obtain leaching solid; Said leaching solid is dried to constant weight under 105-110 ℃ in loft drier; Leaching solid after will drying is then put into electric furnace, at 270 ℃ of roasting 76min of temperature, makes WHITE CARBON BLACK after the pulverizing.
Embodiment 3
A kind ofly prepare the method for WHITE CARBON BLACK, operate according to following steps with alumina laterite:
The first step prepares a leach liquor and a leached mud
Alumina laterite is put into stirred autoclave, leach alumina laterite with hydrochloric acid soln, the leaching reaction conditions is:
Hydrochloric acid soln and red mud weight part ratio are 4.5:1, and the hydrochloric acid soln volumetric molar concentration is 5mol/L, and extraction temperature is 90 ℃, and extraction time is 150min;
Leaching slurry after leaching is carried out solid-liquid separation with pressure filter, obtain a leach liquor and a leached mud, and with leached mud of water washing 3 times, said water and a leached mud weight part ratio are 4:1; A said leach liquor is used to extract REE, aluminium and iron.
Second step, preparation secondary leach liquor and secondary leached mud
A said leached mud is put into reaction kettle, add hydrochloric acid and leach; The secondary leaching condition is: extraction temperature is 78 ℃, and extraction time is 270min, and the hydrochloric acid soln volumetric molar concentration is 5mol/L, and hydrochloric acid and a leached mud weight part ratio are 4.5:1;
Secondary leaching slurry after leaching is carried out solid-liquid separation with pressure filter, obtain secondary leach liquor and secondary leached mud; And with water washing secondary leached mud twice, said water and secondary leached mud weight part ratio are 3:1;
The 3rd step, the preparation WHITE CARBON BLACK
Repeat the above-mentioned second step operation 6 times, obtain leaching solid; Said leaching solid is dried to constant weight under 105-110 ℃ in loft drier; Leaching solid after will drying is then put into electric furnace, at 300 ℃ of roasting 68min of temperature, makes WHITE CARBON BLACK after the pulverizing.
Embodiment 4
A kind ofly prepare the method for WHITE CARBON BLACK, operate according to following steps with alumina laterite:
The first step prepares a leach liquor and a leached mud
Alumina laterite is put into stirred autoclave, leach alumina laterite with hydrochloric acid soln, the leaching reaction conditions is:
Hydrochloric acid soln and red mud weight part ratio are 4:1, and the hydrochloric acid soln volumetric molar concentration is 6mol/L, and extraction temperature is 82 ℃, and extraction time is 180min;
Leaching slurry after leaching is carried out solid-liquid separation with pressure filter, obtain a leach liquor and a leached mud, and with leached mud of water washing 2 times, said water and a leached mud weight part ratio are 2.1:1; A said leach liquor is used to extract REE, aluminium and iron.
Second step, preparation secondary leach liquor and secondary leached mud
A said leached mud is put into reaction kettle, add hydrochloric acid and leach; The secondary leaching condition is: extraction temperature is 90 ℃, and extraction time is 150min, and the hydrochloric acid soln volumetric molar concentration is 6mol/L, and hydrochloric acid and a leached mud weight part ratio are 4:1;
Secondary leaching slurry after leaching is carried out solid-liquid separation with pressure filter, obtain secondary leach liquor and secondary leached mud; And with water washing secondary leached mud twice, said water and secondary leached mud weight part ratio are 3:1;
The 3rd step, the preparation WHITE CARBON BLACK
Repeat the above-mentioned second step operation 3 times, obtain leaching solid; Said leaching solid is dried to constant weight under 105-110 ℃ in loft drier; Leaching solid after will drying is then put into electric furnace, at 350 ℃ of roasting 50min of temperature, makes WHITE CARBON BLACK after the pulverizing.
Embodiment 5
A kind ofly prepare the method for WHITE CARBON BLACK, operate according to following steps with alumina laterite:
The first step prepares a leach liquor and a leached mud
Alumina laterite is put into stirred autoclave, leach alumina laterite with hydrochloric acid soln, the leaching reaction conditions is:
Hydrochloric acid soln and red mud weight part ratio are 5:1, and the hydrochloric acid soln volumetric molar concentration is 5mol/L, and extraction temperature is 104 ℃, and extraction time is 75min;
Leaching slurry after leaching is carried out solid-liquid separation with pressure filter, obtain a leach liquor and a leached mud, and with leached mud of water washing 3 times, said water and a leached mud weight part ratio are 3:1; A said leach liquor is used to extract REE, aluminium and iron.
Second step, preparation secondary leach liquor and secondary leached mud
A said leached mud is put into reaction kettle, add hydrochloric acid and leach; The secondary leaching condition is: extraction temperature is 102 ℃, and extraction time is 75min, and the hydrochloric acid soln volumetric molar concentration is 5mol/L, and hydrochloric acid and a leached mud weight part ratio are 5:1;
Secondary leaching slurry after leaching is carried out solid-liquid separation with pressure filter, obtain secondary leach liquor and secondary leached mud; And with water washing secondary leached mud twice, said water and secondary leached mud weight part ratio are 3:1;
The 3rd step, the preparation WHITE CARBON BLACK
Repeat the above-mentioned second step operation 4 times, obtain leaching solid; Said leaching solid is dried to constant weight under 105-110 ℃ in loft drier; Leaching solid after will drying is then put into electric furnace, at 470 ℃ of roasting 45min of temperature, makes WHITE CARBON BLACK after the pulverizing.
The invention is not restricted to the foregoing description, in the ken that those of ordinary skills possessed, can also not break away under the prerequisite of aim of the present invention and make various variations.
Claims (3)
1. one kind prepares the method for WHITE CARBON BLACK with alumina laterite, it is characterized in that operating according to following steps:
The first step prepares a leach liquor and a leached mud
Alumina laterite is put into stirred autoclave, leach alumina laterite with hydrochloric acid soln, the leaching reaction conditions is:
Hydrochloric acid soln and red mud weight part ratio are 3-6:1, and the hydrochloric acid soln volumetric molar concentration is 4-8mol/L, and extraction temperature is 70-105 ℃, and extraction time is 60-360min;
Leaching slurry after leaching is carried out solid-liquid separation with pressure filter, obtain a leach liquor and a leached mud, and with leached mud of water washing, said water and a leached mud weight part ratio are 2-4:1;
Second step, preparation secondary leach liquor and secondary leached mud
A said leached mud is put into reaction kettle, add hydrochloric acid and leach; The secondary leaching condition is: extraction temperature is 70-105 ℃, and extraction time is 60-360min, and the hydrochloric acid soln volumetric molar concentration is 4-8mol/L, and hydrochloric acid and a leached mud weight part ratio are 3-6:1;
Secondary leaching slurry after leaching is carried out solid-liquid separation with pressure filter, obtain secondary leach liquor and secondary leached mud; And with water washing secondary leached mud twice, said water and secondary leached mud weight part ratio are 3:1;
The 3rd step, the preparation WHITE CARBON BLACK
Repeat above-mentioned second step operation, obtain leaching solid; Said leaching solid is dried to constant weight under 105-110 ℃ in loft drier; Leaching solid after will drying is then put into electric furnace, at temperature 200-500 ℃ of roasting 40-90min, makes WHITE CARBON BLACK after the pulverizing.
2. according to claim 1ly a kind ofly prepare the method for WHITE CARBON BLACK, it is characterized in that in the said the first step leached mud of water washing 1-3 time with alumina laterite; A said leach liquor is used to extract REE, aluminium and iron.
3. according to claim 1ly a kind ofly prepare the method for WHITE CARBON BLACK, it is characterized in that the number of times that repeats the operation of second step is 3-6 time in said the 3rd step with alumina laterite.
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| CN2011103948093A CN102491346A (en) | 2011-12-02 | 2011-12-02 | Method for preparing white carbon black from aluminum oxide red mud |
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| CN2011103948093A CN102491346A (en) | 2011-12-02 | 2011-12-02 | Method for preparing white carbon black from aluminum oxide red mud |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103952557A (en) * | 2014-03-20 | 2014-07-30 | 浙江大学 | Method for secondary acid leaching of alumina in coal ash residues |
| CN106116510A (en) * | 2016-07-01 | 2016-11-16 | 黑龙江大学 | A kind of red mud extracts silicon dioxide and prepares method and the application of ceramic element filler |
| CN106629757A (en) * | 2016-11-17 | 2017-05-10 | 黑龙江大学 | Method for removing nitrogen and phosphorus from water by using calcium silicate prepared from silicon recycled from red mud |
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| CN101148332A (en) * | 2007-09-12 | 2008-03-26 | 长安大学 | Method for increasing content of silicon dioxide in silicon ash and producing white carbon black |
| WO2010079369A1 (en) * | 2009-01-12 | 2010-07-15 | Nikolaos Papadopoulos | Valuable products obtained from red mud |
| CN101891224A (en) * | 2010-06-29 | 2010-11-24 | 河南煤业化工集团有限责任公司 | Method for producing alumina and white carbon black by utilizing red mud and flyash |
| CN102079525A (en) * | 2010-12-14 | 2011-06-01 | 广东石油化工学院 | Method for preparing white carbon black by taking rice hull ash as raw material |
| CN102127642A (en) * | 2011-03-26 | 2011-07-20 | 太原理工大学 | Method for enriching rare-earth elements from red mud |
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2011
- 2011-12-02 CN CN2011103948093A patent/CN102491346A/en active Pending
Patent Citations (6)
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| CN1164515A (en) * | 1996-05-07 | 1997-11-12 | 姚克瑜 | Red mud recovery and utilization technology |
| CN101148332A (en) * | 2007-09-12 | 2008-03-26 | 长安大学 | Method for increasing content of silicon dioxide in silicon ash and producing white carbon black |
| WO2010079369A1 (en) * | 2009-01-12 | 2010-07-15 | Nikolaos Papadopoulos | Valuable products obtained from red mud |
| CN101891224A (en) * | 2010-06-29 | 2010-11-24 | 河南煤业化工集团有限责任公司 | Method for producing alumina and white carbon black by utilizing red mud and flyash |
| CN102079525A (en) * | 2010-12-14 | 2011-06-01 | 广东石油化工学院 | Method for preparing white carbon black by taking rice hull ash as raw material |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103952557A (en) * | 2014-03-20 | 2014-07-30 | 浙江大学 | Method for secondary acid leaching of alumina in coal ash residues |
| CN106116510A (en) * | 2016-07-01 | 2016-11-16 | 黑龙江大学 | A kind of red mud extracts silicon dioxide and prepares method and the application of ceramic element filler |
| CN106629757A (en) * | 2016-11-17 | 2017-05-10 | 黑龙江大学 | Method for removing nitrogen and phosphorus from water by using calcium silicate prepared from silicon recycled from red mud |
| CN106629757B (en) * | 2016-11-17 | 2019-08-13 | 黑龙江大学 | Recycling silicon prepares the method that calcium silicates removes nitrogen phosphorus in water removal in a kind of red mud |
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Application publication date: 20120613 |