CN101058432A - Method of preparing aluminum oxide from clay mine by citric acid extraction - Google Patents
Method of preparing aluminum oxide from clay mine by citric acid extraction Download PDFInfo
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- CN101058432A CN101058432A CN 200710099831 CN200710099831A CN101058432A CN 101058432 A CN101058432 A CN 101058432A CN 200710099831 CN200710099831 CN 200710099831 CN 200710099831 A CN200710099831 A CN 200710099831A CN 101058432 A CN101058432 A CN 101058432A
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- 239000004927 clay Substances 0.000 title claims abstract description 40
- KRKNYBCHXYNGOX-UHFFFAOYSA-N citric acid Chemical compound OC(=O)CC(O)(C(O)=O)CC(O)=O KRKNYBCHXYNGOX-UHFFFAOYSA-N 0.000 title claims description 155
- 238000000034 method Methods 0.000 title claims description 57
- 238000000605 extraction Methods 0.000 title claims description 40
- TWNQGVIAIRXVLR-UHFFFAOYSA-N oxo(oxoalumanyloxy)alumane Chemical compound O=[Al]O[Al]=O TWNQGVIAIRXVLR-UHFFFAOYSA-N 0.000 title claims description 33
- 238000002386 leaching Methods 0.000 claims abstract description 30
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 claims abstract description 18
- 238000001914 filtration Methods 0.000 claims abstract description 12
- 239000003795 chemical substances by application Substances 0.000 claims abstract description 5
- 238000001816 cooling Methods 0.000 claims abstract description 3
- 239000000706 filtrate Substances 0.000 claims description 20
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 14
- 150000002500 ions Chemical class 0.000 claims description 10
- 238000001556 precipitation Methods 0.000 claims description 10
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 9
- 239000002994 raw material Substances 0.000 claims description 8
- 238000000498 ball milling Methods 0.000 claims description 7
- YXFVVABEGXRONW-UHFFFAOYSA-N Toluene Chemical compound CC1=CC=CC=C1 YXFVVABEGXRONW-UHFFFAOYSA-N 0.000 claims description 6
- 239000000463 material Substances 0.000 claims description 6
- 239000000047 product Substances 0.000 claims description 6
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 claims description 5
- 239000011449 brick Substances 0.000 claims description 5
- 239000004568 cement Substances 0.000 claims description 5
- 239000002245 particle Substances 0.000 claims description 5
- 229910052710 silicon Inorganic materials 0.000 claims description 5
- 239000010703 silicon Substances 0.000 claims description 5
- KBPLFHHGFOOTCA-UHFFFAOYSA-N caprylic alcohol Natural products CCCCCCCCO KBPLFHHGFOOTCA-UHFFFAOYSA-N 0.000 claims description 4
- 239000006229 carbon black Substances 0.000 claims description 4
- 238000006243 chemical reaction Methods 0.000 claims description 4
- 239000003337 fertilizer Substances 0.000 claims description 4
- XTAZYLNFDRKIHJ-UHFFFAOYSA-N n,n-dioctyloctan-1-amine Chemical compound CCCCCCCCN(CCCCCCCC)CCCCCCCC XTAZYLNFDRKIHJ-UHFFFAOYSA-N 0.000 claims description 4
- 150000007524 organic acids Chemical class 0.000 claims description 4
- STCOOQWBFONSKY-UHFFFAOYSA-N tributyl phosphate Chemical compound CCCCOP(=O)(OCCCC)OCCCC STCOOQWBFONSKY-UHFFFAOYSA-N 0.000 claims description 4
- 238000000151 deposition Methods 0.000 claims description 3
- 238000004587 chromatography analysis Methods 0.000 claims description 2
- 239000008139 complexing agent Substances 0.000 claims description 2
- 230000001186 cumulative effect Effects 0.000 claims description 2
- 238000005242 forging Methods 0.000 claims description 2
- 239000003350 kerosene Substances 0.000 claims description 2
- 239000000203 mixture Substances 0.000 claims description 2
- TVMXDCGIABBOFY-UHFFFAOYSA-N n-Octanol Natural products CCCCCCCC TVMXDCGIABBOFY-UHFFFAOYSA-N 0.000 claims description 2
- 150000003141 primary amines Chemical class 0.000 claims description 2
- 125000005270 trialkylamine group Chemical group 0.000 claims description 2
- 229910052782 aluminium Inorganic materials 0.000 abstract description 12
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 abstract description 10
- 239000004411 aluminium Substances 0.000 abstract description 9
- 239000002893 slag Substances 0.000 abstract description 9
- 238000004519 manufacturing process Methods 0.000 abstract description 8
- 238000005245 sintering Methods 0.000 abstract description 7
- 239000007788 liquid Substances 0.000 abstract description 5
- ZUGAOYSWHHGDJY-UHFFFAOYSA-K 5-hydroxy-2,8,9-trioxa-1-aluminabicyclo[3.3.2]decane-3,7,10-trione Chemical compound [Al+3].[O-]C(=O)CC(O)(CC([O-])=O)C([O-])=O ZUGAOYSWHHGDJY-UHFFFAOYSA-K 0.000 abstract description 3
- KRKNYBCHXYNGOX-UHFFFAOYSA-K Citrate Chemical compound [O-]C(=O)CC(O)(CC([O-])=O)C([O-])=O KRKNYBCHXYNGOX-UHFFFAOYSA-K 0.000 abstract 2
- 239000002253 acid Substances 0.000 description 14
- 229910001570 bauxite Inorganic materials 0.000 description 13
- 229910052500 inorganic mineral Inorganic materials 0.000 description 13
- 239000011707 mineral Substances 0.000 description 13
- 238000004131 Bayer process Methods 0.000 description 6
- 239000000377 silicon dioxide Substances 0.000 description 5
- 238000005516 engineering process Methods 0.000 description 4
- 238000003756 stirring Methods 0.000 description 4
- 239000000126 substance Substances 0.000 description 4
- 229910004298 SiO 2 Inorganic materials 0.000 description 3
- 238000004458 analytical method Methods 0.000 description 3
- 229910052681 coesite Inorganic materials 0.000 description 3
- 229910052593 corundum Inorganic materials 0.000 description 3
- 229910052906 cristobalite Inorganic materials 0.000 description 3
- 238000006460 hydrolysis reaction Methods 0.000 description 3
- 239000004615 ingredient Substances 0.000 description 3
- JEIPFZHSYJVQDO-UHFFFAOYSA-N iron(III) oxide Inorganic materials O=[Fe]O[Fe]=O JEIPFZHSYJVQDO-UHFFFAOYSA-N 0.000 description 3
- 238000001471 micro-filtration Methods 0.000 description 3
- 239000002244 precipitate Substances 0.000 description 3
- 235000012239 silicon dioxide Nutrition 0.000 description 3
- 229910052682 stishovite Inorganic materials 0.000 description 3
- 229910052905 tridymite Inorganic materials 0.000 description 3
- 229910001845 yogo sapphire Inorganic materials 0.000 description 3
- 229910018557 Si O Inorganic materials 0.000 description 2
- -1 aluminum ion Chemical class 0.000 description 2
- 230000000536 complexating effect Effects 0.000 description 2
- 150000001875 compounds Chemical class 0.000 description 2
- 230000007613 environmental effect Effects 0.000 description 2
- 239000012535 impurity Substances 0.000 description 2
- 238000004064 recycling Methods 0.000 description 2
- LIVNPJMFVYWSIS-UHFFFAOYSA-N silicon monoxide Inorganic materials [Si-]#[O+] LIVNPJMFVYWSIS-UHFFFAOYSA-N 0.000 description 2
- 239000002699 waste material Substances 0.000 description 2
- 229910018516 Al—O Inorganic materials 0.000 description 1
- 235000003140 Panax quinquefolius Nutrition 0.000 description 1
- 240000005373 Panax quinquefolius Species 0.000 description 1
- 230000002378 acidificating effect Effects 0.000 description 1
- 230000004913 activation Effects 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 238000009835 boiling Methods 0.000 description 1
- 238000001354 calcination Methods 0.000 description 1
- 238000011109 contamination Methods 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 238000004090 dissolution Methods 0.000 description 1
- 238000001035 drying Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000004134 energy conservation Methods 0.000 description 1
- 238000005265 energy consumption Methods 0.000 description 1
- 239000003344 environmental pollutant Substances 0.000 description 1
- 230000002349 favourable effect Effects 0.000 description 1
- 230000007062 hydrolysis Effects 0.000 description 1
- 230000014759 maintenance of location Effects 0.000 description 1
- 244000005700 microbiome Species 0.000 description 1
- 230000010287 polarization Effects 0.000 description 1
- 231100000719 pollutant Toxicity 0.000 description 1
- 238000010298 pulverizing process Methods 0.000 description 1
- 238000000746 purification Methods 0.000 description 1
- 239000011819 refractory material Substances 0.000 description 1
- 238000007789 sealing Methods 0.000 description 1
- 238000002791 soaking Methods 0.000 description 1
- 239000002689 soil Substances 0.000 description 1
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Abstract
The invention discloses an alumina manufacturing method through leaching clay by citrate, which is characterized by the following: adopting organic citrate as leaching agent to leach the sintered aluminium in the clay; filtering to remove the leached slag; cooling and stewing the leached liquid; sedimenting the aluminium citrate; sintering the aluminium citrate through high temperature to produce the alumina product; circulating the leaching liquid with little polluting discharge.
Description
Technical field
A kind of method of preparing aluminum oxide from clay mine by citric acid extraction relates to a kind of acid system that utilizes and produces aluminum oxide, particularly utilizes the weak acid citric acid to leach and contains bauxite resource production method of alumina.
Background technology
It is abundant that China contains bauxite resource, and present proven reserve are up to several trillion tons, and are distributed more widely.The process for making alumina overwhelming majority commonly used at present is an alkaline process, comprises Bayer process, sintering process, mixed combining method, the less acid system of using, and what mainly consider is the acid system seriously corroded, the equipment acid resistance is required high.But bayer process requires the A/S of raw material greater than 8.0; Sintering process is less demanding to alumina silica ratio, but sintering process technology relative complex, the energy consumption height; The raw material that promptly is used in ore dressing-Bayer process also requires A/S greater than 2.0.So can be used for the raw material bauxite resource weight range of alumina producing dwindles greatly.What other can not be used for present alumina producing contains that bauxite resource ore deposit major part is the silicon height, aluminium is high or low, alumina silica ratio is low, with Bayer process or sintering process or integrated process or the materialization beneficiating method comes process for producing aluminum oxide cost height, the cycle is long, income is low, residue is difficult, big for environment pollution.Some is contained bauxite resource such as clay pit directly as raw materials such as refractory materials, brick material, cement, and does not calculate in the social economy in waste aluminium source.
Summary of the invention
Purpose of the present invention is exactly the deficiency that exists at above-mentioned prior art, provides a kind of and utilizes the less acid system leaching-out technique of corrodibility low-gradely in handling to contain the bauxite resource ore deposit, enlarges aluminiferous available stock amount, reduced social total cost of production, energy-saving and cost-reducing, leached mud, residual acid, backwater all can recyclings, pollute that discharge capacity is few, the method for eco-friendly preparing aluminum oxide from clay mine by citric acid extraction.
The objective of the invention is to be achieved through the following technical solutions.
A kind of method of preparing aluminum oxide from clay mine by citric acid extraction, it is characterized in that its process is to adopt the organic acid citric acid as leaching agent leaching calcining back clay pit, filter and remove leached mud, again the leach liquor cooling is staticly settled out Tiorco 677, Tiorco 677 obtains alumina product through high-temperature roasting.
The method of a kind of preparing aluminum oxide from clay mine by citric acid extraction of the present invention, it is characterized in that filtering-depositing after, contain remaining citric acid in the filtrate and return and do the leach liquor recycle, leached mud is as the raw material of biological silicon fertilizer, white carbon black, cement, brick material.
The method of a kind of preparing aluminum oxide from clay mine by citric acid extraction of the present invention, the clay pit that it is characterized in that being used to leach is for process is pulverized, ball milling to granularity is 833 μ m～74 μ m, the clay pit after forging under 200 ℃～900 ℃ behind roasting 1h～6h.
The method of a kind of preparing aluminum oxide from clay mine by citric acid extraction of the present invention, it is characterized in that the clay pit after the roasting descends to leach to forge the back clay pit at 50 ℃～150 ℃, leaching with citric acid concentration is 5g/l～80g/l, the dried ore deposit weight percent concentration of ore pulp is 5%～30%, pH value 0.5～5.0, the leached mud of the last period leaches 1～6 section as back one section solid-like continuously under same condition; Every section extraction time is 1h～8h.
The method of a kind of preparing aluminum oxide from clay mine by citric acid extraction of the present invention, it is characterized in that every section soak after, filtered while hot to soak the ore deposit solidliquid mixture, under 0 ℃～50 ℃, leach liquor was placed 1～48 hour again, refilter the precipitation that produces.
The method of a kind of preparing aluminum oxide from clay mine by citric acid extraction of the present invention, the throw out that it is characterized in that filtering out is under 800 ℃～1400 ℃ temperature, and roasting 0.5h～4h obtains alumina product.
The method of a kind of preparing aluminum oxide from clay mine by citric acid extraction of the present invention, it is characterized in that filtrate is residual has not the citric acid of the reaction participated in after chromatography of ions detects content, the citric acid that adds again after the calculating reaches to leach and requires citric acid concentration, turns back to and leaches the container recycle.
The method of a kind of preparing aluminum oxide from clay mine by citric acid extraction of the present invention, filtrate cumulative foreign ion after it is characterized in that extracting, utilize tributyl phosphate TBP, trialkylamine 7301, primary amine 1923, trioctylamine TOA to be complexing agent, adopt the filtrate after toluene, n-Octanol, kerosene repeatedly circulate as the thinner extraction respectively, continuous extraction 2 times～6 times, and use the hot water back extraction, back extraction is 1 time～4 times continuously; Anti-raffinate returns extraction section; Add citric acid to anti-stripping agent, reach and leach the citric acid concentration that requires, turn back to the leaching container.
Method of the present invention utilizes acid system to produce aluminum oxide, contain the bauxite resource ore deposit through pulverizing and ball milling after, 200 ℃～900 ℃ following roastings, make planar water, free water, lattice water remove, and the complete deshydroxy of mineral, hydrosilicate becomes metakaolinite, helps organic acid and leaches.In leaching process, citric acid mainly promotes the dissolving of mineral by the synergy of its ionized H+ and acid ion.Under this acidic conditions, H+ and mineral surface positively charged ion generation permutoid reaction, the hydrolysis reaction of Al-O and Si-O key has reduced the acidity in the system simultaneously in the promotion mineral.And the aluminum ion complexing in citrate part and the solution generates the influence that the Tiorco 677 complex compound reduces chemical affinity, promotes mineral dissolution again indirectly.The citrate part reduces the activation energy of mineral hydrolysis reaction again with the aluminum ion formation surface complexes of mineral surface, the surface complexes that generates destroys the stability of Si-O key by the bond polarization effect, thereby improved the mineral hydrolysis rate, caused the release of aluminium in the mineral structure.Aluminum citrate solution is unsaturation under extraction temperature, and after the filtered while hot slagging-off, temperature and pressure all descends, and solution reaches supersaturation, and the Tiorco 677 precipitation is separated out.Be placed on roasting under the comparatively high temps, the water that makes crystal water and reaction generate is emitted, and realizes the thing inversion of phases of aluminum oxide simultaneously.And Tiorco 677 is the bigger organoaluminum of molecular weight, forms the thinner extraordinary aluminum oxide of granularity after the roasting easily.
Method of the present invention at high, medium and low grade all can the bauxite resource ore deposit that contains carry out the weak acid citric acid and leach, comprise contain that the bauxite resource breeze is broken, the leaching of ball milling and roasting, roasting sample, separate that the precipitation of soaking in slag, the leach liquor is separated out and the recycling of filtration, sedimentary roasting, filtrate, extraction process cycle of treatment repeatedly impurity from more operations such as filtrate.
Method of the present invention is to soak aluminum technology in non-bauxite resource mineral Application for Field.In the production process research of aluminum oxide and aluminium, the alkaline process production technique of using the higher bauxite material of A/S to extract aluminum oxide is reported more, and the research report that the bauxite resource mineral extract aluminium that contains that utilizes A/S＜2.0 is seldom arranged; Studying more is technology-Bayer process, sintering process, the mixed combining method that alkaline process is produced aluminum oxide, because the corrodibility of misgivings acid, and few people study and use the acid system production technique.
Method of the present invention utilizes organic acid weak acid to produce aluminum oxide by the aluminium that complexing, sequestering action extract in the ore, both reduced the acidity of system, reduction is to the requirement of equipment corrosion resistance nature, the lower bauxite resource ore deposit that contains of grade is rationally utilized, enlarged alumina producing stock number scope, overcome the high requirement of alkaline process production, and technology realizes circulation ore grade, disposal of pollutants is few, and is environmentally friendly.
Method of the present invention, use baked at a lower temperature solid-like, at citric acid concentration that is lower than stoichiometric ratio and short extraction temperature, closed continuous leaching process through 2～4 sections, the aluminium of the overwhelming majority is extracted out in the mineral, the coarse filtration rear filtrate just can produce a large amount of Tiorco 677 precipitations at normal temperatures in the solution, and precipitation generates aluminum oxide through roasting.This is more energy-conservation than a series of processes that alkaline process complexity consumes energy again, consumption reduction, environmental protection, social production cycle short.And pressure constantly raises in the sealing leaching process, and the boiling point of water descends, and the solubleness of Tiorco 677 increases; Behind the heat filtering, filtrate enters open container, and pressure descends rapidly, makes Tiorco 677 natural subsidence speed and sinkability increase.
In the technological process of method of the present invention, the nubbin citric acid reaches other foreign ions that leached with aluminium in the filtering-depositing rear filtrate.But the foreign ion starting point concentration is very low in the filtrate, and filtrate can be replenished part citric acid fully in addition and be turned back to extracting stage and leach, and has realized technological cycle.After the circulation repeatedly, foreign ion runs up to finite concentration, with extraction process separating impurity ion and remaining citric acid, can reclaim most citric acid by extraction and reextraction.Strippant hot water has reduced crossed contamination, and backwater can utilize.Soak slag and can make the raw material of biological silicon fertilizer, white carbon black, cement, brick material etc.And can utilize and soak scoriaceous subacidity, to produce alkaline scrap material-red mud with Bayer process or alumina by sintering and mixes than row with suitable, creation soil microorganisms environment makes refuse utilized, and turns waste into wealth.
The processing condition of the inventive method are not harsh, and environmental friendliness is produced aluminum oxide for novel acid system and created favorable conditions.
Description of drawings
Fig. 1 is the technical matters technological line figure of method of the present invention;
Fig. 2 leaches clay pit kinetic curve figure for the 60g/l citric acid solution;
Fig. 3 is leach liquor precipitation XRD figure after roasting.
Embodiment
A kind of method of preparing aluminum oxide from clay mine by citric acid extraction is made the particle that granularity is 833 μ m～74 μ m with clay pit, and in 200 ℃～900 ℃ following calcined clay ore deposits, postcooling took out in 1～6 hour.Compound concentration is the citric acid solution of 5g/l～80g/l, doing ore deposit sirloin amount concentration by ore pulp is 5%～30% adding roasting sample, stirring intensity 100r/min～500r/min, pH value 0.5～5.0, the leached mud of the last period is as back one section solid-like, leach 1～6 section continuously under same condition, every section extraction time is 1h～8h.Leaching finishes, and separates slagging-off while hot.Place leach liquor, precipitation is separated out, and filters, and in 800 ℃～1400 ℃ following roasting 0.5h～4h precipitation, obtains aluminum oxide.Filtrate is returned extracting stage, and repeatedly round-robin filtrate is reclaimed available citric acid through extraction.Leached mud can be made the raw material of biological silicon fertilizer, white carbon black, cement, brick material etc.
The present invention is described further below in conjunction with embodiment.
With 1
#Sample ore is through broken, ball milling, clay pit is made the particle that granularity is 833 μ m～74 μ m, place retort furnace 625 ℃ of following roastings 3 hours, with mass concentration is that 6% citric acid solution leaches, stirring intensity is 300r/min, and ore pulp is done mineral amount concentration 10%, and the treatment time is 6 hours, continuously leach four sections, the last period soak the back slag as back one section leaching sample ore.Every section leaching finishes, while hot coarse filtration.Get four sections and soak back slag analysis Al2O3, SiO2, Fe2O3 content.Coarse filtration liquid was put 12 hours, had a large amount of white precipitates to generate, carry out micro-filtration.Micro-filtrate turns back to extracting stage and recycles.
Table 11
#Main component compared (leaching yield %) before and after sample ore leached
| Chemical ingredients | Al 2O 3 | SiO 2 | Fe 2O 3 |
| % soaks and removes back % leaching yield % before leaching | 48.38 6.97 93.05 | 45.05 91.81 1.71 | 0.84 1.21 30.3 |
With 2
#Sample ore is through broken, ball milling, clay pit is made the particle that granularity is 833 μ m～74 μ m, place retort furnace 575 ℃ of following roastings 2.5 hours, with mass concentration is that 4% citric acid solution leaches, stirring intensity is 200r/min, pulp density 15%, and the treatment time is 4 hours, continuously leach three sections, the last period soak the back slag as back one section leaching sample ore.Every section leaching finishes, while hot coarse filtration.Get two sections and soak back slag analysis Al2O3, SiO2, Fe2O3 content.Coarse filtration liquid put under the normal temperature placed 12 hours, have a large amount of white precipitates to generate, carry out micro-filtration.Micro-filtrate turns back to extracting stage and recycles.
Table 22
#Main component compared (leaching yield %) before and after sample ore leached
| Chemical ingredients | Al 2O 3 | SiO 2 | Fe 2O 3 |
| % soaks and removes back % leaching yield % before leaching | 47.85 16.24 81.80 | 44.60 82.45 0.89 | 0.86 1.31 18.31 |
Embodiment 3
With 3
#Sample ore is through broken, ball milling, clay pit is made the particle that granularity is 833 μ m～74 μ m, placing retort furnace 675 ℃ of following roastings 3.5 hours, is that 4% citric acid solution leaches with mass concentration, and stirring intensity is 300r/min, pulp density 10%, treatment time is 5 hours, leaches three sections continuously, the last period soak the back slag as back one section leaching sample ore.Every section leaching finishes, while hot coarse filtration.Get three sections and soak back slag analysis Al2O3, SiO2, Fe2O3 content.Coarse filtration liquid put under the normal temperature placed 12 hours, have a large amount of white precipitates to generate, carry out micro-filtration.Micro-filtrate turns back to extracting stage and recycles.
Table 33
#Main component compared (leaching yield %) before and after sample ore leached
| Chemical ingredients | Al 2O 3 | SiO 2 | Fe 2O 3 |
| % soaks and removes back % leaching yield % before leaching | 48.06 11.50 87.86 | 44.98 87.28 1.62 | 0.85 1.21 27.87 |
The collecting precipitation thing after the purification drying, is placed on 1050 ℃ of following roasting 1h, obtains alumina product, and its product is XRD and is seen accompanying drawing 3, and the overwhelming majority of Sheng Chenging is α-Al as can be known
2O
3
Claims (8)
1. the method for a preparing aluminum oxide from clay mine by citric acid extraction, it is characterized in that its process is to adopt the organic acid citric acid to leach as leaching agent to forge the back clay pit, filter and remove leached mud, again the leach liquor cooling is staticly settled out Tiorco 677, Tiorco 677 obtains alumina product through high-temperature roasting.
2. the method for a kind of preparing aluminum oxide from clay mine by citric acid extraction according to claim 1, after it is characterized in that filtering-depositing, contain remaining citric acid in the filtrate and return and do the leach liquor recycle, leached mud is as the raw material of biological silicon fertilizer, white carbon black, cement, brick material.
3. the method for a kind of preparing aluminum oxide from clay mine by citric acid extraction according to claim 1, the clay pit that it is characterized in that being used to leach is for process is pulverized, ball milling to granularity is the particle of 833 μ m～74 μ m, the clay pit after forging under 200 ℃～900 ℃ behind roasting 1h～6h.
4. the method for a kind of preparing aluminum oxide from clay mine by citric acid extraction according to claim 1, it is characterized in that the clay pit after the roasting descends to leach to forge the back clay pit at 50 ℃～150 ℃, leaching with citric acid concentration is 5g/l～80g/l, the dried ore deposit weight percent concentration of ore pulp is 5%～30%, pH value 0.5～5.0, the leached mud of the last period leaches 1～6 section as back one section solid-like continuously under same condition; Every section extraction time is 1h～8h.
5. the method for a kind of preparing aluminum oxide from clay mine by citric acid extraction according to claim 1, it is characterized in that every section soak after, want filtered while hot to soak the ore deposit solidliquid mixture, under 0 ℃～50 ℃, leach liquor was placed 1～48 hour again, refilter the precipitation that produces.
6. the method for a kind of preparing aluminum oxide from clay mine by citric acid extraction according to claim 1, the throw out that it is characterized in that filtering out is under 800 ℃～1400 ℃ temperature, and roasting 0.5h～4h obtains alumina product.
7. the method for a kind of preparing aluminum oxide from clay mine by citric acid extraction according to claim 1, it is characterized in that filtrate is residual has not the citric acid of the reaction participated in after chromatography of ions detects content, the citric acid that adds again after the calculating reaches to leach and requires citric acid concentration, turns back to and leaches the container recycle.
8. the method for a kind of preparing aluminum oxide from clay mine by citric acid extraction according to claim 7, filtrate cumulative foreign ion after it is characterized in that extracting, utilize tributyl phosphate TBP, trialkylamine 7301, primary amine 1923, trioctylamine TOA to be complexing agent, adopt the filtrate after toluene, n-Octanol, kerosene repeatedly circulate as the thinner extraction respectively, continuous extraction 2 times～6 times, and use the hot water back extraction, back extraction is 1 time～4 times continuously; Anti-raffinate returns extraction section; Add citric acid to anti-stripping agent, leach the citric acid concentration that requires, turn back to the leaching container.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105498683A (en) * | 2015-12-01 | 2016-04-20 | 长江水资源保护科学研究所 | Preparation method of modified clay mineral material for purification of fluorine-containing sewage |
| CN106732787A (en) * | 2016-11-18 | 2017-05-31 | 福州大学化肥催化剂国家工程研究中心 | A kind of activation method of bauxite, bauxite catalyst and preparation method thereof |
| CN115109925A (en) * | 2022-06-20 | 2022-09-27 | 东北大学 | Method for treating transition metal oxide ore by citric acid system |
-
2007
- 2007-05-31 CN CN 200710099831 patent/CN101058432A/en active Pending
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105498683A (en) * | 2015-12-01 | 2016-04-20 | 长江水资源保护科学研究所 | Preparation method of modified clay mineral material for purification of fluorine-containing sewage |
| CN106732787A (en) * | 2016-11-18 | 2017-05-31 | 福州大学化肥催化剂国家工程研究中心 | A kind of activation method of bauxite, bauxite catalyst and preparation method thereof |
| CN106732787B (en) * | 2016-11-18 | 2019-07-26 | 福州大学化肥催化剂国家工程研究中心 | A kind of activation method of bauxite, bauxite catalyst and preparation method thereof |
| CN115109925A (en) * | 2022-06-20 | 2022-09-27 | 东北大学 | Method for treating transition metal oxide ore by citric acid system |
| CN115109925B (en) * | 2022-06-20 | 2024-05-17 | 东北大学 | Method for treating transition metal oxide ore by using citric acid system |
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