CN104556175A - Method for preparing aluminum hydroxide from potash feldspar decomposition tailings - Google Patents
Method for preparing aluminum hydroxide from potash feldspar decomposition tailings Download PDFInfo
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- CN104556175A CN104556175A CN201510032486.1A CN201510032486A CN104556175A CN 104556175 A CN104556175 A CN 104556175A CN 201510032486 A CN201510032486 A CN 201510032486A CN 104556175 A CN104556175 A CN 104556175A
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Abstract
The invention relates to a method for preparing aluminum hydroxide from potash feldspar decomposition tailings, which comprises the following steps: 1) leaching of potash feldspar decomposition tailings: leaching the potash feldspar decomposition reaction tailings in an 8-10 vol% sulfuric acid solution; 2) preparation of iron-aluminum mixture: adding ammonia water, and controlling the end pH value of the dropwise addition at 8.0-10.0 to precipitate Fe<3+> and Al<3+>; 3) preparation of K-N compound fertilizer: concentrating the filtrate by evaporation, and crystallizing to obtain the K-N binary compound fertilizer potassium ammonium sulfate; 4) separation of iron and aluminum in iron-aluminum mixture: carrying out alkali leaching in a sodium hydroxide solution, and controlling the solid-to-liquid ratio and sodium hydroxide concentration to obtain ferric hydroxide and a sodium metalluminate solution; and 5) preparation of high-purity aluminum hydroxide by a carbonation process: introducing CO2 into the sodium metalluminate solution, controlling the reaction temperature, and regulating the pH value of the solution to 9.5-12.0 to precipitate the high-purity aluminum hydroxide.
Description
Technical field
The present invention relates to potassium feldspar decomposition tailings, particularly a kind of method of preparing hydrogen aluminum oxide from potassium feldspar decomposition tailings.
Background technology
In agriculture production, potassium is one of indispensable element, Shi Ge large agricultural country of China, but existing soluble potassium salt resource is difficult to meet Production requirement.Potassium felspar sand is the representative of insoluble potassium resource, and there are extremely abundant potassium felspar sand reserves Songxian County, Luoyang, and each component content of ore (massfraction) is: K
2o, 13.39%; SiO
2, 62.86%; Al
2o
3, 17.18%, contained K
2o and Al
2o
3grade all far away higher than industrial requirements grade, therefore will become the trend of Future Development to the research of potassium felspar sand.
China has the decomposition to potassium felspar sand of numerous colleges and universities and designing institute and studies, and its method is mostly attached most importance to the comprehensive utilization of potassium element, seldom has the processing method of the aluminium element decomposed in tailings being carried out to research and utilization, causes the waste of bauxite resource.For this present situation, Wuhan University of Technology professor Zhang Guangxu develops a kind of low temperature semidrying, the production technique of decomposing of potassium feldspar in rotary kiln.This technique, at comprehensive utilization potassium element, is effectively alleviated while soluble potassium salt demand, also recycles, have Great significance to a large amount of aluminium in decomposition tailings.
Summary of the invention
Problem to be solved by this invention is: a kind of method providing preparing hydrogen aluminum oxide from potassium feldspar decomposition tailings.Effectively make use of the aluminium contained in potassium feldspar decomposition tailings, preparing hydrogen aluminum oxide.
The present invention solves its technical problem and adopts following technical scheme:
The method of preparing hydrogen aluminum oxide from potassium feldspar decomposition tailings provided by the invention, comprises the following steps:
(1) leaching of potassium feldspar decomposition tailings:
Tailings potassium feldspar decomposition reacted is at 90 ~ 110 DEG C, and be the sulphuric acid soln leaching of 8 ~ 10% by volume fraction, the slurries obtained after stirring, by Filter Press, obtain leaching liquid;
(2) preparation of iron aluminium miscellany:
Leaching liquid is heated to 80 ~ 120 DEG C, slowly adds ammoniacal liquor, controlling to drip terminal is pH=8.0 ~ 10.0, filters after stirring, and reusable heat water washing is to neutral, dry, grinds;
(3) preparation of K, N composite fertilizer:
The filtrate evaporation concentration obtained after step (2) is filtered, crystallization ammonium-potassium sulfate, then spray granulating, drying, obtain K, N binary compound fertilizer ammonium-potassium sulfate;
(4) separation of iron aluminium in iron aluminium mixture:
The sodium hydroxide solution of the iron aluminium mixture 100 ~ 140g/L ground is carried out alkali according to the solid-to-liquid ratio of 1g solid/20 ~ 40ml liquid molten, alkali solubility temperature is 80 ~ 120 DEG C, reaction 0.8 ~ 1.2h, then filters, washs, dry, obtains ironic hydroxide and sodium aluminate solution;
(5) carbon method prepares high-purity hydrogen aluminum oxide:
CO is passed into by sodium aluminate solution
2, pH to 9.5 ~ 12.0 of adjustment solution, control temperature of reaction≤40 DEG C, and reaction 28 ~ 32min, then filters, and washing is to neutral, and dry, roasting, obtains high-purity hydrogen aluminum oxide.
In above-mentioned steps (1), low whipping speed is under 30 ~ 80r/min, can make that K, Al, Fe in tailings are as much as possible to be entered in slurries.
In above-mentioned steps (2), when adding ammoniacal liquor process, should avoid adding the too fast aluminium hydroxide that makes and being wrapped up in a large number.
In above-mentioned steps (2), ultra-fine lamination grinding machine dried filtrate is adopted to be milled to 180 ~ 220 orders.
In above-mentioned steps (4), the molten reactional equation of described alkali is: Al
3++ 4OH
-=AlO
2-+ 2H
2o.
In the molten process of above-mentioned steps (4) described alkali, timely make up water or condensing reflux, evaporate in a large number to prevent the high liquid that causes of temperature.
Above-mentioned steps passes into CO described in (5)
2in process, its reactional equation is: 2AlO
2-+ CO
2+ 3H
2o=CO
3 2-+ 2Al (OH)
3↓.
Above-mentioned steps passes into CO described in (5)
2in process, should control CO
2the speed that passes into be 2.5 ~ 3.5L/min, to avoid the speed that passes into too fast, the aluminium hydroxide crystal seed of formation is excessive, too fast, is mingled with basic metal.
In aforesaid method provided by the invention, the purity of the aluminium hydroxide obtained can reach 99%.
The present invention compared with prior art has following main advantage:
1, the method for the present invention's preparing hydrogen aluminum oxide from potassium feldspar decomposition tailings, makes the effective constituent of potassium felspar sand be fully used, the rate of recovery >=86% of aluminium, the perfect comprehensive utilization technique of potassium felspar sand.Described processing method is that the sulphuric acid soln being 8 ~ 10% by potassium feldspar decomposition tailings employing volume fraction leaches, and temperature controls at 90 ~ 110 DEG C, obtains mainly containing K
+, Al
3+and Fe
3+leaching liquid, ammonification precipitation taps a blast furnace the filtrate after aluminium mixture for the preparation of ammonium-potassium sulfate, thus manufactures N, K composite fertilizer.
2, the method for the present invention's preparing hydrogen aluminum oxide from potassium feldspar decomposition tailings, adopt the technique of alkali solution technique separation of iron aluminium mixture, temperature of reaction is at 80 ~ 120 DEG C, and solid-to-liquid ratio is 1g solid/20 ~ 40ml liquid, reactional equation: Al
3++ 4OH
-=AlO
2-+ 2H
2o, compared with adopting the technique of extraction process separation of iron aluminium, reaction conditions easily reaches, and lower to the requirement of equipment, operational condition easily controls, and subsequent treatment process is simple and easy to do.
3, the method for the present invention's preparing hydrogen aluminum oxide from potassium feldspar decomposition tailings, adopt the aluminium hydroxide of carbon method high-purity, purity can reach 99%, reactional equation: 2AlO
2-+ CO
2+ 3H
2o=CO
3 2-+ 2Al (OH)
3↓, compared with industrial conventional bayer process, operational condition is simple, only needs to control temperature of reaction≤40 DEG C, control CO
2the speed that passes into be 2.5 ~ 3.5L/min, the pH of terminal is 9.5 ~ 12.0, and the process time is short, contributes to economizing on resources, reduce waste and environment protection.It is promoted the use of, and will produce good society and economic implications.
Accompanying drawing explanation
Fig. 1 is the process flow sheet of preparing hydrogen aluminum oxide from potassium feldspar decomposition tailings.
In figure: 1. ammonification reactor; 2. plate-and-frame filter press; 3. alkali leaching still; 4. dioxide bottle; 5. carbon divides reactor; 6. moisture eliminator; 7. evaporative crystallization still; 8. compound fertilizer prilling tower.
Embodiment
Below in conjunction with embodiment, the invention will be further described, only for technical conceive of the present invention and feature are described, but do not form any limitation of the invention.
Embodiment 1: the method for preparing hydrogen aluminum oxide from potassium feldspar decomposition tailings
Get 200ml potassium feldspar decomposition tailings leaching liquid, at 80 DEG C, add ammoniacal liquor, the sodium hydroxide solution of the iron aluminium mixture 100 ~ 140g/L obtained is that 1g solid/20 ~ 40ml liquid carries out alkali leaching, passes into CO in leaching liquid according to solid-to-liquid ratio
2, control temperature of reaction≤40 DEG C, obtain product aluminium hydroxide 3.07g, yield 76.96%, purity 98.62%.
Embodiment 2: the method for preparing hydrogen aluminum oxide from potassium feldspar decomposition tailings
Get 200ml potassium feldspar decomposition tailings leaching liquid, at 100 DEG C, add ammoniacal liquor, the sodium hydroxide solution of the iron aluminium mixture 100 ~ 140g/L obtained is that 1g solid/20 ~ 40ml liquid carries out alkali leaching, passes into CO in leaching liquid according to solid-to-liquid ratio
2, control temperature of reaction≤40 DEG C, obtain product aluminium hydroxide 3.45g, yield 86.20%, purity 98.97%.
Embodiment 3: the method for preparing hydrogen aluminum oxide from potassium feldspar decomposition tailings
Get 200ml potassium feldspar decomposition tailings leaching liquid, at 120 DEG C, add ammoniacal liquor, the sodium hydroxide solution of the iron aluminium mixture 100 ~ 140g/L obtained is that 1g solid/20 ~ 40ml liquid carries out alkali leaching, passes into CO in leaching liquid according to solid-to-liquid ratio
2, control temperature of reaction≤40 DEG C, obtain product aluminium hydroxide 3.47g, yield 86.50%, purity 99.01%.
Embodiment 4: the method for preparing hydrogen aluminum oxide from potassium feldspar decomposition tailings
Get 200ml potassium feldspar decomposition tailings leaching liquid, at 80 ~ 120 DEG C, add ammoniacal liquor, the sodium hydroxide solution of the iron aluminium mixture 100 ~ 140g/L obtained is that 1g solid/20ml liquid carries out alkali leaching, passes into CO in leaching liquid according to solid-to-liquid ratio
2, control temperature of reaction≤40 DEG C, obtain product aluminium hydroxide 3.13g, yield 79.50%, purity 97.37%.
Embodiment 5: the method for preparing hydrogen aluminum oxide from potassium feldspar decomposition tailings
Get 200ml potassium feldspar decomposition tailings leaching liquid, at 80 ~ 120 DEG C, add ammoniacal liquor, the sodium hydroxide solution of the iron aluminium mixture 100 ~ 140g/L obtained is that 1g solid/30ml liquid carries out alkali leaching, passes into CO in leaching liquid according to solid-to-liquid ratio
2, control temperature of reaction≤40 DEG C, obtain product aluminium hydroxide 3.44g, yield 86.20%, purity 98.87%.
Embodiment 6: the method for preparing hydrogen aluminum oxide from potassium feldspar decomposition tailings
Get 200ml potassium feldspar decomposition tailings leaching liquid, at 80 ~ 120 DEG C, add ammoniacal liquor, the sodium hydroxide solution of the iron aluminium mixture 100 ~ 140g/L obtained is that 1g solid/40ml liquid carries out alkali leaching, passes into CO in leaching liquid according to solid-to-liquid ratio
2, control temperature of reaction≤40 DEG C, obtain product aluminium hydroxide 3.35g, yield 83.69%, purity 98.95%.
Claims (9)
1. the method for preparing hydrogen aluminum oxide from potassium feldspar decomposition tailings, is characterized in that comprising the following steps:
(1) leaching of potassium feldspar decomposition tailings:
Tailings potassium feldspar decomposition reacted is at 90 ~ 110 DEG C, and be the sulphuric acid soln leaching of 8 ~ 10% by volume fraction, the slurries obtained after stirring, by Filter Press, obtain leaching liquid;
(2) preparation of iron aluminium miscellany:
Leaching liquid is heated to 80 ~ 120 DEG C, slowly adds ammoniacal liquor, controlling to drip terminal is pH=8.0 ~ 10.0, filters after stirring, and reusable heat water washing is to neutral, dry, grinds;
(3) preparation of K, N composite fertilizer:
The filtrate evaporation concentration obtained after step (2) is filtered, crystallization ammonium-potassium sulfate, then spray granulating, drying, obtain K, N binary compound fertilizer ammonium-potassium sulfate;
(4) separation of iron aluminium in iron aluminium mixture:
The sodium hydroxide solution of the iron aluminium mixture 100 ~ 140g/L ground is carried out alkali according to the solid-to-liquid ratio of 1g solid/20 ~ 40ml liquid molten, alkali solubility temperature is 80 ~ 120 DEG C, reaction 0.8 ~ 1.2h, then filters, washs, dry, obtains ironic hydroxide and sodium aluminate solution;
(5) carbon method prepares high-purity hydrogen aluminum oxide:
CO is passed into by sodium aluminate solution
2, pH to 9.5 ~ 12.0 of adjustment solution, control temperature of reaction≤40 DEG C, and reaction 28 ~ 32min, then filters, and washing is to neutral, and dry, roasting, obtains high-purity hydrogen aluminum oxide.
2. method according to claim 1, is characterized in that, in step (1), low whipping speed is under 30 ~ 80r/min, makes that K, Al, Fe in tailings are as much as possible to be entered in slurries.
3. method according to claim 1, is characterized in that in step (2), when adding ammoniacal liquor process, should avoid adding the too fast aluminium hydroxide that makes and being wrapped up in a large number.
4. method according to claim 1, is characterized in that in step (2), dried filtrate is adopted ultra-fine lamination grinding machine to be milled to 180 ~ 220 orders.
5. method according to claim 1, is characterized in that in step (4), and the molten reactional equation of described alkali is: Al
3++ 4OH
-=AlO
2-+ 2H
2o.
6. method according to claim 1, is characterized in that in the molten process of step (4) described alkali, timely make up water or condensing reflux, evaporates in a large number to prevent the high liquid that causes of temperature.
7. method according to claim 1, is characterized in that passing into CO described in step (5)
2in process, its reactional equation is: 2AlO
2-+ CO
2+ 3H
2o=CO
3 2-+ 2Al (OH)
3↓.
8. method according to claim 1, is characterized in that passing into CO described in step (5)
2in process, should control CO
2the speed that passes into be 2.5 ~ 3.5L/min, to avoid the speed that passes into too fast, the aluminium hydroxide crystal seed of formation is excessive, too fast, is mingled with basic metal.
9. method according to claim 1, is characterized in that the purity of obtained aluminium hydroxide can reach 99%.
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105060350A (en) * | 2015-08-04 | 2015-11-18 | 贵州远盛钾业科技有限公司 | Production method of iron oxide by utilizing potassium-bearing rock |
| CN105107818A (en) * | 2015-08-20 | 2015-12-02 | 山东盛日环保工程技术有限公司 | Environment friendly treating process for alumina red mud tailings and feldspar tailing mixed materials |
| CN112126783A (en) * | 2020-08-25 | 2020-12-25 | 湖南邦普循环科技有限公司 | Recycling method of iron and aluminum in nickel-cobalt-manganese solution |
| CN113121334A (en) * | 2020-01-15 | 2021-07-16 | 中蓝长化工程科技有限公司 | Method for producing potassium oxalate and aluminum hydroxide by using potassium feldspar |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1160019A (en) * | 1997-02-25 | 1997-09-24 | 中国科学院化工冶金研究所 | Ammonium sulfate method for extracting alumina from low-grade aluminium-contg. ore |
| CN101450811A (en) * | 2008-10-23 | 2009-06-10 | 长春市超威新材料科技有限公司 | Method for extracting alumina from coal gangue |
| CN103539177A (en) * | 2013-10-31 | 2014-01-29 | 洛阳氟钾科技有限公司 | Technology for preparing aluminum hydroxide by use of potassium feldspar |
| CN103539162A (en) * | 2013-10-31 | 2014-01-29 | 洛阳氟钾科技有限公司 | Process method for preparing ammonium-potassium sulfate from potassium feldspar |
-
2015
- 2015-01-22 CN CN201510032486.1A patent/CN104556175B/en not_active Expired - Fee Related
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1160019A (en) * | 1997-02-25 | 1997-09-24 | 中国科学院化工冶金研究所 | Ammonium sulfate method for extracting alumina from low-grade aluminium-contg. ore |
| CN101450811A (en) * | 2008-10-23 | 2009-06-10 | 长春市超威新材料科技有限公司 | Method for extracting alumina from coal gangue |
| CN103539177A (en) * | 2013-10-31 | 2014-01-29 | 洛阳氟钾科技有限公司 | Technology for preparing aluminum hydroxide by use of potassium feldspar |
| CN103539162A (en) * | 2013-10-31 | 2014-01-29 | 洛阳氟钾科技有限公司 | Process method for preparing ammonium-potassium sulfate from potassium feldspar |
Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105060350A (en) * | 2015-08-04 | 2015-11-18 | 贵州远盛钾业科技有限公司 | Production method of iron oxide by utilizing potassium-bearing rock |
| CN105107818A (en) * | 2015-08-20 | 2015-12-02 | 山东盛日环保工程技术有限公司 | Environment friendly treating process for alumina red mud tailings and feldspar tailing mixed materials |
| CN113121334A (en) * | 2020-01-15 | 2021-07-16 | 中蓝长化工程科技有限公司 | Method for producing potassium oxalate and aluminum hydroxide by using potassium feldspar |
| CN113121334B (en) * | 2020-01-15 | 2022-05-20 | 中蓝长化工程科技有限公司 | Method for producing potassium oxalate and aluminum hydroxide by using potassium feldspar |
| CN112126783A (en) * | 2020-08-25 | 2020-12-25 | 湖南邦普循环科技有限公司 | Recycling method of iron and aluminum in nickel-cobalt-manganese solution |
| CN112126783B (en) * | 2020-08-25 | 2022-06-14 | 湖南邦普循环科技有限公司 | Recycling method of iron and aluminum in nickel-cobalt-manganese solution |
| US11760655B2 (en) | 2020-08-25 | 2023-09-19 | Hunan Brunp Recycling Technology Co., Ltd. | Method for recycling iron and aluminum in nickel-cobalt-manganese solution |
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