CN105776267A - Method for producing aluminum oxide by means of granulating and sintering of low-grade bauxite - Google Patents
Method for producing aluminum oxide by means of granulating and sintering of low-grade bauxite Download PDFInfo
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- CN105776267A CN105776267A CN201610083753.2A CN201610083753A CN105776267A CN 105776267 A CN105776267 A CN 105776267A CN 201610083753 A CN201610083753 A CN 201610083753A CN 105776267 A CN105776267 A CN 105776267A
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01F—COMPOUNDS OF THE METALS BERYLLIUM, MAGNESIUM, ALUMINIUM, CALCIUM, STRONTIUM, BARIUM, RADIUM, THORIUM, OR OF THE RARE-EARTH METALS
- C01F7/00—Compounds of aluminium
- C01F7/02—Aluminium oxide; Aluminium hydroxide; Aluminates
- C01F7/04—Preparation of alkali metal aluminates; Aluminium oxide or hydroxide therefrom
- C01F7/14—Aluminium oxide or hydroxide from alkali metal aluminates
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01F—COMPOUNDS OF THE METALS BERYLLIUM, MAGNESIUM, ALUMINIUM, CALCIUM, STRONTIUM, BARIUM, RADIUM, THORIUM, OR OF THE RARE-EARTH METALS
- C01F7/00—Compounds of aluminium
- C01F7/02—Aluminium oxide; Aluminium hydroxide; Aluminates
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Abstract
The invention provides a method for producing aluminum oxide by means of granulating and sintering of low-grade bauxite.The method comprises the following steps that sodium carbonate, coke powder and alkali liquor are added to bauxite and limestone for blending, all the materials are added into a blender mixer for granulation, the finished granule products are sintered on a sintering machine, water or correction liquor is added to pulverized clinker for dissolution, obtained slag is reversely washed 5-7 times with water, and washing liquor serves as the correction liquor; a solution and sodium aluminate crystals are mixed and dissolved, desilicication is conducted, aluminum hydroxide crystal seeds are added for seed precipitation decomposition, and a seed precipitation mother solution is subjected to evaporation and salt elimination in two steps.According to the method, for the defect that low-grade bauxite is difficult to refine, the sintering technology of the smelting field is combined and utilized, the whole seed precipitation technology is provided, the technological processes of a technological process is shortened by one third or above, the seed precipitation decomposition rate is comprehensively calculated and increased to 90% or above, the total recovery rate of aluminum oxide reaches 90% or above, the operation difficulty is reduced, the equipment and personnel investment is reduced, and the energy consumption is reduced.
Description
Technical field
The invention belongs to field of smelting, be specifically related to a kind of method that pelletizing method smelts bauxite.
Background technology
China's bauxite resource grade (alumina silica ratio) is relatively low, processes by the production technology of conventional sintering method, not only causes process for making alumina complicated, and adds difficulty and the production cost of alumina producing.Therefore, major part enterprise of current China is all only with bayer process, to middle and low grade bauxite, if directly processed by simple Bayer process, will result in alkaline consumption height, dissolution rate variance, cost sharply raise, particularly possibly together with silicon minerals such as illites in China's bauxite, can not being removed by simple pre-desiliconizing, these mineral are prone to react in ore pulp intensification warm, precipitated sodium white residue on heat-transfer surface, become and scab, make heat transfer coefficient decline rapidly.
On the other hand, aluminum i ndustry is the basic industry of China, economic construction being in great demand to bauxite, and China's great majority are the bauxite of middle-low grade.Along with bauxite increasingly sharpens for ore deposit grade downward trend, the many bauxite resources of China are difficult by because grade is low, it has to from external a large amount of imports, data shows, the external dependence degree of China's bauxite aluminium resource is up to 55% in recent years.The method of industrial treatment low-grade bauxite can only having traditional sintering process technology at present, but owing to its technological process is complicated, energy consumption is high, cause production cost to remain high, the sintering process production line of current China has been substantially at end-of-life state.
Although the feature according to China's bauxite resource, some R&D institutions and enterprise have developed the technology such as series process and mixed combining method accordingly to reduce alkaline consumption, to improve the response rate of aluminium oxide, but both approaches is both needed to adopt sintering process, this causes, and production system complexity is huge, capital expenditure increases, energy consumption is high, be difficult to series of problems such as controlling, product quality is poor, economy is not good, is therefore progressively in the underproduction or end-of-life state yet.
How effectively to utilize the middle-low bauxite of alumina silica ratio less than 5, solve a difficult problem for China's bauxite resource relative deficiency, it has also become the task of top priority.
Summary of the invention
For the problems referred to above, the present invention provides a kind of granulation dry sintering, full kind to divide and spent liquor evaporation technology, it is achieved utilize the purpose of low-grade bauxite granulation SINTERING PRODUCTION aluminium oxide.
The technical scheme realizing the object of the invention is:
A kind of method utilizing low-grade bauxite granulation SINTERING PRODUCTION aluminium oxide, comprises the following steps:
(1) bauxite, limestone add soda, coke powder and alkali liquor carry out dispensing, described alkali liquor is circulation sodium aluminate solution, proportion scale is bauxite 35～45: limestone 26～35%: soda 5～15%: coke powder 8～12% (mass ratio of dry powder), after dispensing completes, moisture Control is 15～30%；
(2) together with the alkali liquor that volume is 85～90%, the material prepared is added batch mixer to be sufficiently mixed; granulate with roller granulating machine again; granulation liquid volume added is remaining 10～15%, and granulation particle diameter is 3～8mm, it is ensured that the permeability index after corning is at 40～60kPa.
(3) being sintered on sintering machine by finished product grain, sintering temperature 1400～1500 DEG C, the grog after burning till is levigate for grog powder；
(4) chamotte powder adding adjustment liquid and carries out dissolution, leaching condition is: liquid-solid ratio is 3～4:1, and dissolution time is 15～20 minutes, and temperature is 70～75 DEG C.
(5), after the slag hot water that step (4) obtains being carried out 5～7 back flush, washing liquid is as the adjustment liquid of step (4), and slag is stored up；
(6) desiliconization after the solution that step (4) is obtained and sodium aluminate crystallization mixed dissolution, the temperature of desiliconization 160～180 DEG C, 1～2 hour time；
(7) the solution hydrogenation alumina seed that step (6) obtains is carried out kind of a point decomposition, decompose and obtain Al (OH)3, then roasting obtains aluminium oxide；
(8) seed precipitation solution that step (7) obtains being undertaken in two steps evaporation and salt discharge, the first step adopts the evaporator evaporation of common material to be Na to concentration of lye2O280～300g/L, then carries out second step evaporation salt discharge again with nickel material vaporizer, and obtaining concentration of lye is Na2O500～600g/L；
(9) seed precipitation solution after being evaporated by second step carries out seed addition decrease temperature crystalline, obtains sodium aluminate crystal, and sodium aluminate crystal is then added in step (6) to carry out dissolving circulation；Crystallization condition is: first temperature 80～110 DEG C, end temperature 40～50 DEG C, 6～8 hours time；
(10) mother solution step (9) obtained obtains with step (8) salt and the white residue that step (6) obtains mix, and then return in step (1) as dispensing alkali liquor, it is achieved alkali liquor circulates.
Wherein, in described step (1), bauxite is the low-grade bauxite of alumina silica ratio less than 5.The used optional coal coke powder of coke powder, calorific value is more than 7000 kilocalories.
Wherein, in described step (1), bauxite and limestone mine are crushed to 2～below 5mm first respectively, then levigate account for more than 85% for-0.074mm to granularity.
Wherein, in described step (1), alkali liquor is circulation sodium aluminate solution, and concentration of lye is Na2O500～600g/L, α k=12～30 (causticization coefficient).After dispensing completes, moisture Control is 15～30%.
Wherein, in described step (2), granulation liquid volume added is remaining 10～15%, and liquid feeding is the alkali liquor same with step (1), and volume is the 10～20% of the same alkali liquor of step (1).
Wherein, in described step (3), the firing temperature of sintering machine sintering is 1050 DEG C, and igniting negative pressure is more than 4KPa, and sintering negative pressure is more than 8KPa；Grog after burning till adopts Vertical Mill to dry grind, and is milled down to-0.074mm and accounts for the grog powder of more than 90%.
Hot water temperature in step (5) can be 80～99 DEG C.
Preferably, in described step (6), add desiliconization seed and carry out desiliconization.Grain weight 40～the 60g/L of desiliconization.The solid that desiliconization seed and desiliconization step produce, it is possible to promote crystallization, be conducive to separating.Seed is not had at the operation initial stage.
Further, seed precipitation solution adds seed decrease temperature crystalline, and described seed is sodium aluminate crystal, grain weight 10～40g/L.
The present invention compared with prior art advantage is in that:
(1) method that the present invention proposes, the defect refined it is difficult to for low-grade bauxite, it is combined with the sintering technology of field of smelting, proposing full kind division technique technology, make sintering process technological process reduce more than 1/3rd, COMPREHENSIVE CALCULATING corrosion brings up to more than 90%, the overall recovery of aluminium oxide reaches more than 90%, reduce operation easier, reduce equipment and personnel put into, reduce energy consumption.
(2) present invention achieves the breakthrough of high concentration seed precipitation solution evaporation, evaporate salt discharge technology by two steps, solve the problem that tradition seed precipitation solution evaporation restricts evaporative concn because of salt discharge difficulty.
(3) calcined soda for industry cheap for part can be converted into the liquid caustic soda that added value is high by the present invention, falls below the cost of the major product of this technology further, and economic benefit is obvious.
In a word, the present invention technically achieves important breakthrough what conventional sintering method produced aluminium oxide, and production cost and investment of founding the factory all are greatly lowered, remarkably productive when processing low-grade bauxite, and integrated cost is close to Bayer process production cost.Simultaneously in lectotype selection, having the equipment choice of maturation at chemical industry and metallurgy industry, industrialization is very easy to feasible.
Accompanying drawing explanation
Fig. 1: granulation sintering process produces the flow chart of aluminium oxide.
Detailed description of the invention
Now with following most preferred embodiment, the present invention is described, but does not limit the scope of the present invention with this.
Following by different embodiments, the present invention is described.The present invention is not limited in these embodiments, it is possible to adjusted enforcement within the scope of afore mentioned chemical composition with manufacture method.
Raw material bauxite (A/S is 3.5) and limestone adopt ore deposit, From Xiaoyi, Shanxi area, and its composition is such as shown in table 1～table 4.
Embodiment 1
Table 1: bauxite composition
Table 2: limestone composition
First bauxite (composition is table 1 such as), limestone (composition is table 2 such as) are crushed to 2～5mm respectively, then it levigate are respectively accounted for more than 85% to granularity for-0.074mm, coke powder is crushed to 1～3mm.Then by bauxite powder, agstone, coke powder, light ash in dry powder quality ratio bauxite 35: limestone 26: soda 6: coke powder 8 is sufficiently mixed, being ready for alkali liquor, alkali liquor is circulation sodium aluminate solution, and concentration is Na2O510g/L, α k=14, the dispensing moisture 30% obtained, alkali ratio is 1, and calcium ratio is 2.
The material prepared adding batch mixer and carries out first time mixing, the material that has mixed enters rerolling machine, and rerolling machine machine sprays into alkali liquor simultaneously, and consumption is the 3/17 of dispensing consumption；Granulating in cartridge type granulator, particle size distribution is 3～8mm.
Being distributed on sintering machine by finished pellets and grate-layer material and rim charge to be sintered, control firing temperature 1050 DEG C, igniting negative pressure, more than 4KPa, sintering temperature 1400～1500 DEG C, sinters negative pressure 8～8.5KPa.Then agglomerate is milled down to-0.074mm and accounts for the grog grinding of more than 90%.
The chamotte powder ground adding adjustment liquid and carries out dissolution in dissolution groove, liquid-solid ratio is 3.5:1, the concentration Na of the dissolution fluid of configuration2O50g/L, α k=1.2, dissolution time is 20 minutes, and temperature is 75 DEG C.
After slag water dissolution obtained carries out 7 back flush, washing liquid adjusts liquid (mix with chamotte powder and use) as dissolution, and slag is stored up.
After solution dissolution obtained and sodium aluminate crystallization mixed dissolution, dividing mother liquid evaporation to adjust α k by one section of kind is 1.5, AL2O3Concentration controls to be 120g/L, adds desiliconization seed and carries out desiliconization in desilicator.Desiliconization condition is: grain weight 60g/L, temperature 160 DEG C, and 1 hour time, after desiliconization completes, serosity leaf filter is refined, and seminal fluid carries out kind of a point decomposition, and desiliconization slag mixes later dispensing with circulating mother liquor.
The seminal fluid adding aluminum hydroxide crystal seed that desiliconization obtains carries out kind of a point decomposition, decomposes and obtains Al (OH)3, then roasting obtains aluminium oxide.
Decomposing the seed precipitation solution obtained and be undertaken in two steps evaporation and salt discharge, it is Na that the conventional six effect falling film evaporators of the first step are evaporated to concentration of lye2O280～300g/L, then carries out second step evaporation salt discharge with nickel material vaporizer again, and obtaining concentration of lye is Na2O510g/L。
Seed precipitation solution after being evaporated by second step carries out seed addition decrease temperature crystalline, obtains sodium aluminate crystal, and sodium aluminate crystal is then added in dissolution rough liquid to carry out dissolving circulation.Crystallization condition is: first temperature 80 DEG C, end temperature 50 DEG C, grain weight 20g/L, 6 hours time.
The white residue that circulating mother liquor crystallization obtained obtains with evaporation discharge salt and desiliconization mixes, and then comes back for dispensing as dispensing alkali liquor, it is achieved alkali liquor circulates.
By the Decomposition Cycle mother solution COMPREHENSIVE CALCULATING that kind point decomposition step and two steps evaporation salt discharge step obtain, corrosion can reach 95%.Alumina recovery rate reaches 93%.
Embodiment 2
Table 3: bauxite composition
First bauxite (composition is table 3 such as), limestone (composition is table 2 such as) are crushed to 2～5mm respectively, then it levigate are respectively accounted for more than 85% to granularity for-0.074mm, coke powder is crushed to 1～3mm.Then by bauxite powder, agstone, coke powder, light ash in dry powder quality ratio bauxite 40: limestone 30: soda 10: coke powder 10 ratio is sufficiently mixed, concentration of lye is Na2O550g/L, α k=20, the dispensing moisture 28% obtained, alkali ratio is 1, and calcium ratio is 2.
The material prepared adding batch mixer and carries out first time mixing, the material that has mixed enters rerolling machine, and rerolling machine machine sprays into the alkali liquor accounting for dispensing alkali liquor 13/87 simultaneously, granulates in rerolling machine, and distribution of particles is 3～8mm.
Being distributed on sintering machine by finished pellets and grate-layer material and rim charge to be sintered, control firing temperature 1050 DEG C, igniting negative pressure, more than 4KPa, sintering temperature 1400～1500 DEG C, sinters negative pressure 8～8.5KPa.Then agglomerate is milled down to-0.074mm and accounts for the grog grinding of more than 90%.
The chamotte powder ground adding adjustment liquid and carries out dissolution in dissolution groove, leaching condition is: concentration of lye Na2O50g/L, α k=1.2, liquid-solid ratio is 3:1, and dissolution time is 15 minutes, and temperature is 75 DEG C.
After slag water dissolution obtained carries out 6 back flush, washing liquid adjusts liquid as dissolution, and slag is stored up.
After solution dissolution obtained and sodium aluminate crystallization mixed dissolution, dividing mother liquid evaporation to adjust α k by one section of kind is 1.5, AL2O3Concentration controls to be 130g/L, adds desiliconization seed and carries out desiliconization in desilicator.Desiliconization condition is: grain weight 60g/L, temperature 160 DEG C, and 1 hour time, after desiliconization completes, serosity leaf filter is refined, and seminal fluid carries out kind of a point decomposition, and desiliconization slag mixes later dispensing with circulating mother liquor.
Repeat the decomposition in example 1, evaporation and crystallization mode, it is achieved process cycles.
By the Decomposition Cycle mother solution COMPREHENSIVE CALCULATING that kind point decomposition step and two steps evaporation salt discharge step obtain, corrosion reaches 94%.Alumina recovery rate reaches 92%
Embodiment 3
Table 4: bauxite composition
First bauxite (composition is table 4 such as), limestone (composition is table 2 such as) are crushed to 2～5mm respectively, then it levigate are respectively accounted for more than 85% to granularity for-0.074mm, coke powder is crushed to 1～3mm.Then by bauxite powder, agstone, coke powder, light ash in dry powder quality ratio bauxite 45: limestone 35: soda 15: coke powder 12% ratio is sufficiently mixed, and is ready for alkali liquor, concentration is Na2O550g/L, α k=20, and alkali liquor is by volume divided into two parts, allocation proportion is 90:10.Dispensing moisture 26%, alkali ratio is 1, and calcium ratio is 2, and coke powder ratio is 12%.
Expecting that adding batch mixer together with the alkali liquor of 90% carries out first time mixing by what prepare, the material that has mixed enters rerolling machine, and rerolling machine machine sprays the alkali liquor of people remaining 10% simultaneously, granulates in rerolling machine, and distribution of particles is 3～8mm.
Being distributed on sintering machine by finished pellets and grate-layer material and rim charge to be sintered, control firing temperature 1050 DEG C, igniting negative pressure, more than 4KPa, sintering temperature 1400～1500 DEG C, sinters negative pressure 8～8.5KPa.Then agglomerate is milled down to-0.074mm and accounts for the grog grinding of more than 90%.
The chamotte powder ground adding adjustment liquid and carries out dissolution in dissolution groove, leaching condition is: concentration of lye Na2O50g/L, α k=1.2, liquid-solid ratio is 4:1, and dissolution time is 20 minutes, and temperature is 75 DEG C.
After slag dissolution obtained carries out 7 back flush, washing liquid adjusts liquid as dissolution, and slag is stored up.
After solution dissolution obtained and sodium aluminate crystallization mixed dissolution, dividing mother liquid evaporation to adjust α k by one section of kind is 1.5, AL2O3Concentration controls to be 140g/L, adds desiliconization seed and carries out desiliconization in desilicator.Desiliconization condition is: grain weight 60g/L, temperature 160 DEG C, and 1 hour time, after desiliconization completes, serosity leaf filter is refined, and seminal fluid carries out kind of a point decomposition, and desiliconization slag mixes later dispensing with circulating mother liquor.
Repeat the decomposition in example 1, evaporation and crystallization mode, it is achieved process cycles.
By the Decomposition Cycle mother solution COMPREHENSIVE CALCULATING that kind point decomposition step and two steps evaporation salt discharge step obtain, corrosion reaches 93%.Alumina recovery rate reaches 90%
Those skilled in the art in the art will be appreciated that, above-described embodiment is intended merely to the explanation present invention, and it is not used as limitation of the invention, as long as in the spirit of the present invention, the conversion of above-described embodiment, modification all will be fallen within the scope of the claims.
Claims (8)
1. the method utilizing low-grade bauxite granulation SINTERING PRODUCTION aluminium oxide, it is characterised in that comprise the following steps:
(1) bauxite, limestone add soda, coke powder and alkali liquor carry out dispensing, described alkali liquor is circulation sodium aluminate solution, proportion scale is bauxite 35～45: limestone 26～35%: soda 5～15%: coke powder 8～12%, and after dispensing completes, moisture Control is 15～30%；
(2) together with the alkali liquor that volume is 85～90%, the material prepared is added batch mixer to be sufficiently mixed; granulate with roller granulating machine again; granulation liquid volume added is remaining 10～15%, and granulation particle diameter is 3～8mm, it is ensured that the permeability index after corning is at 40～60kPa；
(3) being sintered on sintering machine by finished product grain, sintering temperature 1400～1500 DEG C, the grog after burning till is levigate for grog powder；
(4) chamotte powder adding adjustment liquid and carries out dissolution, liquid-solid ratio is 3～4:1, and dissolution time is 15～20 minutes, and temperature is 70～75 DEG C；
(5), after the slag hot water that step (4) obtains being carried out 5～7 back flush, washing liquid is as the adjustment liquid of step (4), and slag is stored up；
(6) desiliconization after the solution that step (4) is obtained and sodium aluminate crystallization mixed dissolution, the temperature of desiliconization 160～180 DEG C, 1～2 hour time；
(7) the solution hydrogenation alumina seed that step (6) obtains is carried out kind of a point decomposition, decompose and obtain Al (OH)3, then roasting obtains aluminium oxide；
(8) seed precipitation solution that step (7) obtains being undertaken in two steps evaporation and salt discharge, the first step adopts the evaporator evaporation of carbon steel material to be Na to concentration of lye2O280～300g/L, then carries out second step evaporation salt discharge again with nickel material vaporizer, and obtaining concentration of lye is Na2O500～600g/L；
(9) seed precipitation solution after being evaporated by second step carries out seed addition decrease temperature crystalline, obtains sodium aluminate crystal, and sodium aluminate crystal is then added in step (6) to carry out dissolving circulation；Crystallization condition is: first temperature 80～110 DEG C, end temperature 40～50 DEG C, 6～8 hours time；
(10) mother solution step (9) obtained obtains with step (8) salt and the white residue that step (6) obtains mix, and then return in step (1) as dispensing alkali liquor, it is achieved alkali liquor circulates.
2. method according to claim 1, it is characterised in that in described step (1), bauxite is the low-grade bauxite of alumina silica ratio less than 5.
3. method according to claim 1, it is characterised in that in described step (1), bauxite and limestone mine are crushed to 2～below 5mm first respectively, then levigate account for more than 85% for-0.074mm to granularity.
4. method according to claim 1, it is characterised in that in described step (1), alkali liquor is circulation sodium aluminate solution, and concentration of lye is Na2O500～600g/L, α k=12～30, after dispensing completes, moisture Control is 15～30%.
5. method according to claim 1, it is characterized in that, in described step (2), granulation liquid volume added is remaining 10～15%, liquid feeding is the alkali liquor same with step (1), and volume is the 10～20% of the same alkali liquor of step (1).
6. method according to claim 1, it is characterised in that in described step (3), the firing temperature of sintering machine sintering is 1050 DEG C, and igniting negative pressure is more than 4KPa, and sintering negative pressure is more than 8KPa；Grog after burning till adopts Vertical Mill to dry grind, and is milled down to-0.074mm granule and accounts for the grog powder of more than 90%.
7., according to the arbitrary described method of claim 1～6, it is characterised in that in described step (6), add desiliconization seed and carry out desiliconization, the grain weight 40～60g/L of desiliconization.
8. according to the arbitrary described method of claim 1～6, it is characterised in that in described step (9), seed precipitation solution adds seed decrease temperature crystalline, and described seed is sodium aluminate crystal, grain weight 10～40g/L.
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| CN108609641A (en) * | 2018-07-09 | 2018-10-02 | 中铝集团山西交口兴华科技股份有限公司 | A kind of production system and its production technology producing low sodium alumina using low-grade bauxite |
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| CN102583477A (en) * | 2012-03-16 | 2012-07-18 | 东北大学 | Comprehensive utilization method of high-ferrum and low-grade bauxite |
| CN104609451A (en) * | 2015-01-30 | 2015-05-13 | 魏子贺 | Process for preparing aluminum oxide by virtue of dry-sintering method |
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| CN101434403A (en) * | 2008-12-16 | 2009-05-20 | 重庆市博赛矿业（集团）有限公司 | Novel method for processing calx sodica sintered alumina by dry method |
| CN102249274A (en) * | 2011-06-20 | 2011-11-23 | 中国铝业股份有限公司 | Method for producing aluminum oxide with alumyte |
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| CN108609641A (en) * | 2018-07-09 | 2018-10-02 | 中铝集团山西交口兴华科技股份有限公司 | A kind of production system and its production technology producing low sodium alumina using low-grade bauxite |
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