CN101607725B - Method for reclaiming alumina and sodium oxide in red mud of Bayer process - Google Patents
Method for reclaiming alumina and sodium oxide in red mud of Bayer process Download PDFInfo
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- CN101607725B CN101607725B CN200810115235XA CN200810115235A CN101607725B CN 101607725 B CN101607725 B CN 101607725B CN 200810115235X A CN200810115235X A CN 200810115235XA CN 200810115235 A CN200810115235 A CN 200810115235A CN 101607725 B CN101607725 B CN 101607725B
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- red mud
- leaching
- sodium aluminate
- bayer process
- alumina
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- 238000004131 Bayer process Methods 0.000 title claims abstract description 31
- 238000000034 method Methods 0.000 title claims abstract description 25
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 title claims abstract description 19
- KKCBUQHMOMHUOY-UHFFFAOYSA-N sodium oxide Chemical compound [O-2].[Na+].[Na+] KKCBUQHMOMHUOY-UHFFFAOYSA-N 0.000 title claims abstract description 17
- 229910001948 sodium oxide Inorganic materials 0.000 title claims abstract description 17
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims abstract description 60
- ANBBXQWFNXMHLD-UHFFFAOYSA-N aluminum;sodium;oxygen(2-) Chemical compound [O-2].[O-2].[Na+].[Al+3] ANBBXQWFNXMHLD-UHFFFAOYSA-N 0.000 claims abstract description 28
- 229910001388 sodium aluminate Inorganic materials 0.000 claims abstract description 28
- 238000002386 leaching Methods 0.000 claims abstract description 20
- 238000002425 crystallisation Methods 0.000 claims abstract description 13
- 230000008025 crystallization Effects 0.000 claims abstract description 13
- 238000004519 manufacturing process Methods 0.000 claims abstract description 13
- 239000003513 alkali Substances 0.000 claims abstract description 10
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 9
- BRPQOXSCLDDYGP-UHFFFAOYSA-N calcium oxide Chemical compound [O-2].[Ca+2] BRPQOXSCLDDYGP-UHFFFAOYSA-N 0.000 claims abstract description 8
- 239000000292 calcium oxide Substances 0.000 claims abstract description 8
- ODINCKMPIJJUCX-UHFFFAOYSA-N calcium oxide Inorganic materials [Ca]=O ODINCKMPIJJUCX-UHFFFAOYSA-N 0.000 claims abstract description 8
- 239000013078 crystal Substances 0.000 claims abstract description 8
- 239000007787 solid Substances 0.000 claims abstract description 8
- 238000001914 filtration Methods 0.000 claims abstract description 6
- 239000004568 cement Substances 0.000 claims abstract description 3
- 239000012452 mother liquor Substances 0.000 claims abstract 4
- 239000000243 solution Substances 0.000 claims description 12
- WNROFYMDJYEPJX-UHFFFAOYSA-K aluminium hydroxide Chemical compound [OH-].[OH-].[OH-].[Al+3] WNROFYMDJYEPJX-UHFFFAOYSA-K 0.000 claims description 5
- 239000007864 aqueous solution Substances 0.000 claims description 3
- 239000002994 raw material Substances 0.000 claims description 3
- 230000035484 reaction time Effects 0.000 claims description 2
- 238000004321 preservation Methods 0.000 claims 1
- 238000000926 separation method Methods 0.000 claims 1
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 abstract description 13
- 229910052708 sodium Inorganic materials 0.000 abstract description 13
- 239000011734 sodium Substances 0.000 abstract description 13
- 238000004090 dissolution Methods 0.000 abstract description 3
- 238000001354 calcination Methods 0.000 abstract description 2
- TWNQGVIAIRXVLR-UHFFFAOYSA-N oxo(oxoalumanyloxy)alumane Chemical compound O=[Al]O[Al]=O TWNQGVIAIRXVLR-UHFFFAOYSA-N 0.000 description 18
- 238000011084 recovery Methods 0.000 description 12
- 239000012670 alkaline solution Substances 0.000 description 9
- 239000007795 chemical reaction product Substances 0.000 description 8
- 239000000203 mixture Substances 0.000 description 8
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 6
- 150000004645 aluminates Chemical class 0.000 description 6
- 150000004677 hydrates Chemical class 0.000 description 6
- 239000010413 mother solution Substances 0.000 description 6
- CDBYLPFSWZWCQE-UHFFFAOYSA-L Sodium Carbonate Chemical compound [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 description 4
- 229910021502 aluminium hydroxide Inorganic materials 0.000 description 4
- 229910052814 silicon oxide Inorganic materials 0.000 description 4
- 238000005245 sintering Methods 0.000 description 4
- 238000000967 suction filtration Methods 0.000 description 4
- 238000010792 warming Methods 0.000 description 4
- 229910001570 bauxite Inorganic materials 0.000 description 3
- 238000005265 energy consumption Methods 0.000 description 3
- 229910001648 diaspore Inorganic materials 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 238000000605 extraction Methods 0.000 description 2
- 235000017550 sodium carbonate Nutrition 0.000 description 2
- 229910000029 sodium carbonate Inorganic materials 0.000 description 2
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 description 1
- 235000011089 carbon dioxide Nutrition 0.000 description 1
- 230000007423 decrease Effects 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 230000002950 deficient Effects 0.000 description 1
- 238000001704 evaporation Methods 0.000 description 1
- 230000008020 evaporation Effects 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 238000001027 hydrothermal synthesis Methods 0.000 description 1
- 238000002955 isolation Methods 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 239000007791 liquid phase Substances 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 239000000047 product Substances 0.000 description 1
- 238000004064 recycling Methods 0.000 description 1
- 229910052710 silicon Inorganic materials 0.000 description 1
- 239000010703 silicon Substances 0.000 description 1
- 239000000377 silicon dioxide Substances 0.000 description 1
- 238000005406 washing Methods 0.000 description 1
Landscapes
- Compounds Of Alkaline-Earth Elements, Aluminum Or Rare-Earth Metals (AREA)
Abstract
一种回收拜尔法赤泥中氧化铝和氧化钠的方法，步骤为：将赤泥在30-70wt％NaOH溶液中行浸出反应，碱溶液与赤泥重量配比4∶1～8∶1，浸出温度180-250℃，浸出时间0.2-5h，浸出压力0.3-1.8MPa，过滤得含铝酸钠的碱液和脱铝赤泥；含铝酸钠的碱液50-100℃下结晶，得水合铝酸钠粗晶及结晶母液，结晶母液循环用于浸出反应；水合铝酸钠粗晶用水溶解返回拜尔法生产，经脱硅种分和煅烧得氧化铝；脱铝赤泥中加水和脱铝赤泥重量5-20％的氧化钙，液固比6∶1～10∶1，100-180℃下脱钠，脱钠后的赤泥用于水泥生产，NaOH溶液用于浸出反应。该方法溶出温度和压力较低，氧化铝溶出率高达90％。A method for recovering alumina and sodium oxide in Bayer process red mud, the steps are: leaching red mud in 30-70wt% NaOH solution, the weight ratio of alkali solution to red mud is 4:1-8:1, The leaching temperature is 180-250°C, the leaching time is 0.2-5h, and the leaching pressure is 0.3-1.8MPa, and the lye containing sodium aluminate and dealuminated red mud are obtained by filtration; the lye containing sodium aluminate is crystallized at 50-100°C to obtain Sodium aluminate hydrate coarse crystals and crystallization mother liquor, the crystallization mother liquor is recycled for leaching reaction; the hydrated sodium aluminate coarse crystals are dissolved in water and returned to Bayer process production, and alumina is obtained by desiliconization and calcination; adding water and The dealuminized red mud is 5-20% calcium oxide by weight, the liquid-solid ratio is 6:1-10:1, and the sodium is removed at 100-180°C. The de-sodiumized red mud is used for cement production, and NaOH solution is used for leaching reaction. The dissolution temperature and pressure of the method are relatively low, and the alumina dissolution rate is as high as 90%.
Description
Technical field
The present invention relates to the field of production of aluminum oxide and sodium oxide, the method for aluminum oxide and sodium oxide in particularly a kind of low-temp low-pressure recovery Bayer process red mud.
Background technology
At present, the worldwide basis industry all faces worldwide energy shortage, and resource is deficient day by day, and environment protection more and more is subjected to people's attention, and for aluminum oxide industry, these challenges are all the more sharp-pointed.
China's alumina producing is a raw material with the diaspore type bauxite of indissoluble mainly, the ore of A/S＞10 only accounts for 10% according to statistics, A/S is that the ore of 7-10 accounts for 20%, and A/S to be the ore of 4-7 account for more than 60%, high alumina, high silicon, low alumina silica ratio are the valuable feature of China's bauxite.Handle A/S when the diaspore type bauxite of 4-7 with pure Bayer process, the alumina recovery rate is low, causes resource utilization low, and the economic and social benefits of aluminum oxide production process are seriously influenced.In order to improve the rate of recovery of aluminum oxide, USSR (Union of Soviet Socialist Republics) and China are devoted for years in adopting the technical study of Bayer sintering integrated process, have obtained significant achievement.But facts have proved that there is the energy consumption height to a certain extent in the integrated process Production Flow Chart, the not high drawback of Production Flow Chart complexity, production efficiency.
Alumina-producing method mainly is a sintering process in the existing recovery red mud, this method is mixed with Bayer process red mud and yellow soda ash, carrying out sintering more than 1000 ℃, obtain the solid sodium aluminate sintered product, just obtain sodium aluminate solution with the diluted alkaline stripping then, feed carbonic acid gas in the solution and promptly obtain aluminium hydroxide, (seeing Bi Shiwen " production technique of aluminum oxide " for details) used in the yellow soda ash recirculation that remains in the solution.The method that reclaims sodium oxide then is to carry out hydro-thermal reaction by add calcium oxide in red mud not reclaiming under the situation of aluminum oxide, allows sodium oxide enter liquid phase, and then reaches the purpose that reclaims sodium oxide.There are problems such as high energy consumption or the rate of recovery are low in above method, and the valuable metal that is seriously restricting red mud reclaims and comprehensive utilization.
Summary of the invention
The objective of the invention is deficiency at aluminum oxide and sodium oxide method existence in the above-mentioned existing recovery Bayer process red mud, a kind of production method that can reclaim aluminum oxide and sodium oxide in the Bayer process red mud under low-temp low-pressure is proposed, and then energy efficient and improve resource utilization effectively.
The objective of the invention is to realize by following technology.
The method of aluminum oxide and sodium oxide in the recovery Bayer process red mud provided by the invention, its step is as follows:
1) Bayer process red mud in being the NaOH aqueous solution of 30-70%, weight percent concentration is leached reaction, the weight part proportioning of described alkaline solution and Bayer process red mud is 4: 1～8: 1, the extraction temperature that leaches reaction is 180-250 ℃, leaching the reaction times is 0.2-5 hour, leaches to be incubated after reaction is finished and filters alkali lye and the dealuminzation red mud that obtains containing sodium aluminate;
2) alkali lye that contains sodium aluminate that step 1) is obtained carries out crystallization under 50-100 ℃, filter to obtain aluminate hydrates sodium coarse-grain and crystalline mother solution thereof, and the crystalline mother solution circulation is used for the leaching reaction of step 1); The aluminate hydrates sodium coarse-grain that obtains with water dissolution after, return bayer's process and produce main flow, after the desiliconization kind is divided operation aluminium hydroxide, after calcining, obtain aluminum oxide again;
3) in the dealuminzation red mud that step 1) obtains, add the calcium oxide of entry and dealuminzation red mud weight 5-20%, liquid-solid ratio is 6: 1～10: 1, sodium was taken off in reaction in 1-5 hour under temperature is 100-180 ℃, take off red mud behind the sodium is used to produce cement raw material again through washing whole mud, be circulated in step 1) in the NaOH aqueous solution that obtains and be used for leaching reaction;
The pressure of the leaching reaction of described step 1) is 0.3MPa-1.8MPa.
The method of aluminum oxide and sodium oxide has following obvious superiority in the recovery Bayer process red mud provided by the invention:
(1) extraction temperature of the present invention is 180-250 ℃, 700-800 ℃ of more traditional sintering process decline, make leaching process in, low pressure heating, can effectively cut down the consumption of energy.
(2) leaching pressure of the present invention leaches under the low pressure at 0.3MPa-1.8MPa, and it is big to have overcome facility investment, and life cycle is short, and shortcomings such as operational difficulty have reduced facility investment significantly, and make operating process be easy to carry out;
(3) dealumination process does not add any auxiliary material among the present invention, and the dealuminzation red mud amount that obtains is significantly reduced;
(4) circulation of high high alkali liquid of the present invention and isolation technique and whole process do not exist a large amount of concentration and evaporations to greatly reduce production energy consumption, have simplified production process, have reduced the equipment input, have improved industrial operability, have reduced production cost.
Embodiment
Embodiment 1
Reclaiming the Bayer process red mud aluminum oxide with method of the present invention, is example with Henan factory Bayer process red mud, and it is as follows that this Bayer process red mud is formed (wt%):
Its recycling step is:
With Bayer process red mud and weight percent concentration is that 30% NaOH solution mixes and is placed in the reactor, its weight part proportioning is Bayer process red mud: NaOH=1: 4, be warming up to 180 ℃, under 0.3MPa, react 1h, obtain containing alkali lye, the reaction product mixture of sodium aluminate and dealuminzation red mud, after reaction product to be mixed is cooled to 100 ℃, take out reactor and in 100 ℃ of baking ovens, be incubated suction filtration, separate the alkaline solution and the dealuminzation red mud that obtain containing sodium aluminate, (A is an alumina weight per-cent to A/S=0.49 in the dealuminzation red mud composition of this moment, S silicon oxide weight percent), the rate of recovery of the aluminum oxide of Bayer process red mud is 70.06%;
The alkaline solution that contains sodium aluminate (filtrated stock) that obtains is put into crystallization reactor, the causticity ratio of the crystalline mother solution that 6 hours after-filtration of crystallization obtain is elevated to 30, the causticity ratio of aluminate hydrates sodium crystal is 1.58, can make sandy alumina to sodium aluminate dissolving, desiliconization, kind branch then.
Add the calcium oxide of water and dealuminzation red mud weight 5% in the dealuminzation red mud again, its liquid-solid ratio is 6: 1, reacts 4h under 140 ℃ of conditions, and the sodium oxide concentration of whole mud is 0.6% behind the sodium for taking off of obtaining.
Embodiment 2
With Bayer process red mud and weight percent concentration is that 45% NaOH solution mixes and is placed in the reactor, its weight part proportioning is Bayer process red mud: NaOH=1: 4, be warming up to 240 ℃, under 1.3MPa, react 2h, obtain containing alkali lye, the reaction product mixture of sodium aluminate and dealuminzation red mud, after reaction product to be mixed is cooled to 100 ℃, take out reactor and in 100 ℃ of baking ovens, be incubated suction filtration, separate the alkaline solution and the dealuminzation red mud that obtain containing sodium aluminate, (A is an alumina weight per-cent to A/S=0.11 in the dealuminzation red mud composition of this moment, S silicon oxide weight percent), the rate of recovery of the aluminum oxide of Bayer process red mud is 93%;
The alkaline solution that contains sodium aluminate (filtrated stock) that obtains is put into crystallization reactor, the causticity ratio of the crystalline mother solution that 8 hours after-filtration of crystallization obtain is elevated to 32, the causticity ratio of aluminate hydrates sodium crystal is 1.65, can make sandy alumina to sodium aluminate dissolving, desiliconization, kind branch then.
Add the calcium oxide of water and dealuminzation red mud weight 10% in the dealuminzation red mud again, its liquid-solid ratio is 8: 1, reacts 3h under 150 ℃ of conditions, and the sodium oxide concentration of whole mud is 0.47% behind the sodium for taking off of obtaining.
Embodiment 3
With Bayer process red mud and weight percent concentration is that 50% NaOH solution mixes, and allocate a certain amount of aluminium hydroxide into, making the causticity ratio in the solution that obtains is 40, its weight part proportioning is Bayer process red mud: NaOH=1: 8, after insert and be warming up to 230 ℃ in the reactor, under 1.2MPa, react 2h, obtain containing alkali lye, the reaction product mixture of sodium aluminate and dealuminzation red mud, after reaction product to be mixed is cooled to 100 ℃, take out reactor and in 100 ℃ of baking ovens, be incubated suction filtration, separate the alkaline solution and the dealuminzation red mud that obtain containing sodium aluminate, (A is an alumina weight per-cent to A/S=0.49 in the dealuminzation red mud composition of this moment, S silicon oxide weight percent), the rate of recovery of the aluminum oxide of Bayer process red mud is 68.79%.
The alkaline solution that contains sodium aluminate (filtrated stock) that obtains is put into crystallization reactor, the causticity ratio of the crystalline mother solution that 16 hours after-filtration of crystallization obtain is elevated to 34, the causticity ratio of aluminate hydrates sodium crystal is 1.62, can make sandy alumina to sodium aluminate dissolving, desiliconization, kind branch then.
Add the calcium oxide of water and dealuminzation red mud weight 15% in the dealuminzation red mud again, its liquid-solid ratio is 8: 1, reacts 2h under 160 ℃ of conditions, and the sodium oxide concentration of whole mud is 0.8% behind the sodium for taking off of obtaining.
Embodiment 4
With Bayer process red mud and weight percent concentration is that 70% NaOH solution mixes, and allocate a certain amount of aluminium hydroxide into, making the causticity ratio in the solution that obtains is 40, its weight part proportioning is Bayer process red mud: NaOH=1: 5, after insert and be warming up to 250 ℃ in the reactor, under 1.7MPa, react 3h, obtain containing alkali lye, the reaction product mixture of sodium aluminate and dealuminzation red mud, after reaction product to be mixed is cooled to 100 ℃, take out reactor and in 100 ℃ of baking ovens, be incubated suction filtration, separate the alkaline solution and the dealuminzation red mud that obtain containing sodium aluminate, (A is an alumina weight per-cent to A/S=0.23 in the dealuminzation red mud composition of this moment, S silicon oxide weight percent), the rate of recovery of the aluminum oxide of Bayer process red mud is 85.31%.
The alkaline solution that contains sodium aluminate (filtrated stock) that obtains is put into crystallization reactor, the causticity ratio of the crystalline mother solution that 16 hours after-filtration of crystallization obtain is elevated to 35, the causticity ratio of aluminate hydrates sodium crystal is 1.672, can make sandy alumina to sodium aluminate dissolving, desiliconization, kind branch then.
Add the calcium oxide of water and dealuminzation red mud weight 15% in the dealuminzation red mud again, its liquid-solid ratio is 10: 1, reacts 2h under 180 ℃ of conditions, and the sodium oxide concentration of whole mud is 0.27% behind the sodium for taking off of obtaining.
Claims (1)
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| CN101607725A CN101607725A (en) | 2009-12-23 |
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Families Citing this family (13)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN102502731A (en) * | 2011-10-13 | 2012-06-20 | 河津市晋铝大株化工有限公司 | Method for manufacturing superfine aluminum hydroxide micropowder |
| CN102627305B (en) * | 2012-03-28 | 2014-05-07 | 中国铝业股份有限公司 | Method using alkaline process to extract alumina in coal ash |
| CN103030162B (en) * | 2012-12-11 | 2015-08-19 | 中国科学院过程工程研究所 | A kind of method preparing sodium aluminate solid from Bayer process red mud |
| CN103030160B (en) * | 2012-12-11 | 2014-11-05 | 中国科学院过程工程研究所 | Method for recycling alumina and sodium oxide from bayer process red mud |
| CN106319218B (en) | 2015-06-16 | 2019-12-24 | 有研稀土新材料股份有限公司 | Method for recovering rare earth, aluminum and silicon from rare earth-containing aluminum-silicon waste |
| CN105039714A (en) * | 2015-08-26 | 2015-11-11 | 攀钢集团攀枝花钢铁研究院有限公司 | Processing method for sodium treatment vanadium and chromium extracting residues and method for extracting vanadium and chromium through sodium salt roasting of vanadium and chromium residues |
| CN106086411A (en) * | 2016-08-01 | 2016-11-09 | 江苏省冶金设计院有限公司 | Red mud is utilized to prepare the method and system of ferrosilicon |
| CN107758714B (en) * | 2016-08-17 | 2020-12-01 | 中国科学院过程工程研究所 | A method for synergistic extraction of aluminum-silicon-lithium-gallium in fly ash by combined method |
| CN106319226A (en) * | 2016-08-22 | 2017-01-11 | 中国铝业股份有限公司 | Method for comprehensively recycling aluminium oxide, sodium oxide and ferric oxide from red mud |
| CN110540225B (en) * | 2019-09-17 | 2020-05-08 | 昆明理工大学 | Recycling treatment process for red mud roasted by waste mushroom sticks |
| CN113105282B (en) * | 2021-04-28 | 2022-09-27 | 东北大学 | Method for preparing silicon-potassium-calcium compound fertilizer by using calcium-containing red mud |
| CN113371743B (en) * | 2021-05-28 | 2023-05-30 | 昆明理工大学 | A method for producing chemical alumina by two-step alkali dissolution method |
| CN114195196A (en) * | 2022-01-11 | 2022-03-18 | 凯里市鑫泰熔料有限公司 | A kind of method for preparing easily soluble aluminum hydroxide with red mud as raw material |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN101058431A (en) * | 2007-01-26 | 2007-10-24 | 长安大学 | Method of extracting aluminum oxide |
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