CN108975367A - A kind of efficient method using high alumina coal gangue - Google Patents
A kind of efficient method using high alumina coal gangue Download PDFInfo
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- CN108975367A CN108975367A CN201810822655.5A CN201810822655A CN108975367A CN 108975367 A CN108975367 A CN 108975367A CN 201810822655 A CN201810822655 A CN 201810822655A CN 108975367 A CN108975367 A CN 108975367A
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- Prior art keywords
- coal gangue
- high alumina
- acid
- alumina coal
- gangue
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- 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 116
- 238000000034 method Methods 0.000 title claims abstract description 59
- 239000003245 coal Substances 0.000 title claims abstract description 48
- 239000002253 acid Substances 0.000 claims abstract description 54
- 239000010802 sludge Substances 0.000 claims abstract description 27
- 238000001354 calcination Methods 0.000 claims abstract description 22
- 239000002893 slag Substances 0.000 claims abstract description 22
- 229910052782 aluminium Inorganic materials 0.000 claims abstract description 21
- WNROFYMDJYEPJX-UHFFFAOYSA-K aluminium hydroxide Chemical compound [OH-].[OH-].[OH-].[Al+3] WNROFYMDJYEPJX-UHFFFAOYSA-K 0.000 claims abstract description 21
- 229910021502 aluminium hydroxide Inorganic materials 0.000 claims abstract description 21
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims abstract description 20
- 239000004411 aluminium Substances 0.000 claims abstract description 20
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 claims abstract description 20
- QAOWNCQODCNURD-UHFFFAOYSA-L Sulfate Chemical compound [O-]S([O-])(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-L 0.000 claims abstract description 18
- 239000006229 carbon black Substances 0.000 claims abstract description 13
- 238000005516 engineering process Methods 0.000 claims abstract description 8
- BAUYGSIQEAFULO-UHFFFAOYSA-L iron(2+) sulfate (anhydrous) Chemical compound [Fe+2].[O-]S([O-])(=O)=O BAUYGSIQEAFULO-UHFFFAOYSA-L 0.000 claims abstract 2
- QAOWNCQODCNURD-UHFFFAOYSA-N sulfuric acid Substances OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims description 54
- 238000005406 washing Methods 0.000 claims description 48
- 239000006210 lotion Substances 0.000 claims description 39
- 230000020477 pH reduction Effects 0.000 claims description 28
- 238000006243 chemical reaction Methods 0.000 claims description 27
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 claims description 23
- 238000004519 manufacturing process Methods 0.000 claims description 20
- DKFCNIGGENJIJN-UHFFFAOYSA-L aluminum;iron(2+);sulfate Chemical compound [Al+3].[Fe+2].[O-]S([O-])(=O)=O DKFCNIGGENJIJN-UHFFFAOYSA-L 0.000 claims description 19
- 239000001117 sulphuric acid Substances 0.000 claims description 18
- 235000011149 sulphuric acid Nutrition 0.000 claims description 18
- 239000006166 lysate Substances 0.000 claims description 15
- 229910052742 iron Inorganic materials 0.000 claims description 12
- 239000007788 liquid Substances 0.000 claims description 12
- 238000003756 stirring Methods 0.000 claims description 12
- 239000000126 substance Substances 0.000 claims description 12
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 12
- 238000009938 salting Methods 0.000 claims description 11
- 239000002994 raw material Substances 0.000 claims description 8
- 238000004064 recycling Methods 0.000 claims description 8
- 238000004131 Bayer process Methods 0.000 claims description 5
- 239000007789 gas Substances 0.000 claims description 5
- 230000003134 recirculating effect Effects 0.000 claims description 5
- 238000001914 filtration Methods 0.000 claims description 4
- 239000000843 powder Substances 0.000 claims description 4
- 238000002360 preparation method Methods 0.000 claims description 4
- 238000007711 solidification Methods 0.000 claims description 4
- 230000008023 solidification Effects 0.000 claims description 4
- 230000035484 reaction time Effects 0.000 claims description 3
- 238000001694 spray drying Methods 0.000 claims description 2
- 230000001502 supplementing effect Effects 0.000 claims description 2
- 229910052739 hydrogen Inorganic materials 0.000 claims 1
- 239000001257 hydrogen Substances 0.000 claims 1
- 125000004435 hydrogen atom Chemical class [H]* 0.000 claims 1
- 229910000358 iron sulfate Inorganic materials 0.000 claims 1
- 239000012266 salt solution Substances 0.000 claims 1
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 abstract description 5
- 239000002910 solid waste Substances 0.000 abstract description 5
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 abstract description 2
- 239000012535 impurity Substances 0.000 abstract description 2
- 229910052710 silicon Inorganic materials 0.000 abstract description 2
- 239000010703 silicon Substances 0.000 abstract description 2
- 239000007787 solid Substances 0.000 abstract description 2
- 229910052717 sulfur Inorganic materials 0.000 abstract 1
- 239000011593 sulfur Substances 0.000 abstract 1
- 239000000047 product Substances 0.000 description 26
- 238000004458 analytical method Methods 0.000 description 12
- 230000008569 process Effects 0.000 description 12
- 239000003513 alkali Substances 0.000 description 11
- 239000000463 material Substances 0.000 description 11
- 238000011084 recovery Methods 0.000 description 10
- 238000004090 dissolution Methods 0.000 description 9
- 238000000605 extraction Methods 0.000 description 9
- 230000003647 oxidation Effects 0.000 description 9
- 238000007254 oxidation reaction Methods 0.000 description 9
- 239000002195 soluble material Substances 0.000 description 9
- MHAJPDPJQMAIIY-UHFFFAOYSA-N Hydrogen peroxide Chemical compound OO MHAJPDPJQMAIIY-UHFFFAOYSA-N 0.000 description 8
- 230000008901 benefit Effects 0.000 description 8
- 239000011449 brick Substances 0.000 description 8
- 238000002386 leaching Methods 0.000 description 7
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 6
- 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 description 5
- 229910052708 sodium Inorganic materials 0.000 description 5
- 239000011734 sodium Substances 0.000 description 5
- 239000002699 waste material Substances 0.000 description 5
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 4
- UQSXHKLRYXJYBZ-UHFFFAOYSA-N Iron oxide Chemical compound [Fe]=O UQSXHKLRYXJYBZ-UHFFFAOYSA-N 0.000 description 4
- 239000005864 Sulphur Substances 0.000 description 4
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 description 4
- 239000000470 constituent Substances 0.000 description 4
- 238000007796 conventional method Methods 0.000 description 4
- 238000010438 heat treatment Methods 0.000 description 4
- 239000003921 oil Substances 0.000 description 4
- 239000000377 silicon dioxide Substances 0.000 description 4
- 239000007921 spray Substances 0.000 description 4
- 238000005507 spraying Methods 0.000 description 4
- 239000013589 supplement Substances 0.000 description 4
- 239000010936 titanium Substances 0.000 description 4
- 229910052719 titanium Inorganic materials 0.000 description 4
- 230000018044 dehydration Effects 0.000 description 3
- 238000006297 dehydration reaction Methods 0.000 description 3
- 239000000284 extract Substances 0.000 description 3
- 239000000706 filtrate Substances 0.000 description 3
- 238000000227 grinding Methods 0.000 description 3
- 239000003595 mist Substances 0.000 description 3
- 239000000203 mixture Substances 0.000 description 3
- 239000003002 pH adjusting agent Substances 0.000 description 3
- 239000004575 stone Substances 0.000 description 3
- 238000012546 transfer Methods 0.000 description 3
- BVKZGUZCCUSVTD-UHFFFAOYSA-L Carbonate Chemical compound [O-]C([O-])=O BVKZGUZCCUSVTD-UHFFFAOYSA-L 0.000 description 2
- UQZIWOQVLUASCR-UHFFFAOYSA-N alumane;titanium Chemical compound [AlH3].[Ti] UQZIWOQVLUASCR-UHFFFAOYSA-N 0.000 description 2
- 238000013459 approach Methods 0.000 description 2
- 229910052593 corundum Inorganic materials 0.000 description 2
- 238000001035 drying Methods 0.000 description 2
- 238000005265 energy consumption Methods 0.000 description 2
- 238000003912 environmental pollution Methods 0.000 description 2
- 229960005191 ferric oxide Drugs 0.000 description 2
- 238000002156 mixing Methods 0.000 description 2
- 238000006386 neutralization reaction Methods 0.000 description 2
- 230000003472 neutralizing effect Effects 0.000 description 2
- 230000035699 permeability Effects 0.000 description 2
- 238000007873 sieving Methods 0.000 description 2
- 238000005245 sintering Methods 0.000 description 2
- 229910001845 yogo sapphire Inorganic materials 0.000 description 2
- 239000005995 Aluminium silicate Substances 0.000 description 1
- OYPRJOBELJOOCE-UHFFFAOYSA-N Calcium Chemical compound [Ca] OYPRJOBELJOOCE-UHFFFAOYSA-N 0.000 description 1
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 1
- 235000008733 Citrus aurantifolia Nutrition 0.000 description 1
- 101100373011 Drosophila melanogaster wapl gene Proteins 0.000 description 1
- FYYHWMGAXLPEAU-UHFFFAOYSA-N Magnesium Chemical compound [Mg] FYYHWMGAXLPEAU-UHFFFAOYSA-N 0.000 description 1
- 235000011941 Tilia x europaea Nutrition 0.000 description 1
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 description 1
- 230000003213 activating effect Effects 0.000 description 1
- 235000012211 aluminium silicate Nutrition 0.000 description 1
- DIZPMCHEQGEION-UHFFFAOYSA-H aluminium sulfate (anhydrous) Chemical compound [Al+3].[Al+3].[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O DIZPMCHEQGEION-UHFFFAOYSA-H 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 239000002585 base Substances 0.000 description 1
- 239000006227 byproduct Substances 0.000 description 1
- 239000011575 calcium Substances 0.000 description 1
- 229910052791 calcium Inorganic materials 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 125000003636 chemical group Chemical group 0.000 description 1
- 239000004927 clay Substances 0.000 description 1
- 229910052681 coesite Inorganic materials 0.000 description 1
- 238000002485 combustion reaction Methods 0.000 description 1
- 230000002860 competitive effect Effects 0.000 description 1
- 238000009833 condensation Methods 0.000 description 1
- 230000005494 condensation Effects 0.000 description 1
- 229910052906 cristobalite Inorganic materials 0.000 description 1
- 238000000354 decomposition reaction Methods 0.000 description 1
- 238000013461 design Methods 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 238000001704 evaporation Methods 0.000 description 1
- 230000008020 evaporation Effects 0.000 description 1
- 239000000945 filler Substances 0.000 description 1
- 239000005431 greenhouse gas Substances 0.000 description 1
- 239000004615 ingredient Substances 0.000 description 1
- JEIPFZHSYJVQDO-UHFFFAOYSA-N iron(III) oxide Inorganic materials O=[Fe]O[Fe]=O JEIPFZHSYJVQDO-UHFFFAOYSA-N 0.000 description 1
- NLYAJNPCOHFWQQ-UHFFFAOYSA-N kaolin Chemical compound O.O.O=[Al]O[Si](=O)O[Si](=O)O[Al]=O NLYAJNPCOHFWQQ-UHFFFAOYSA-N 0.000 description 1
- 239000004571 lime Substances 0.000 description 1
- 239000011777 magnesium Substances 0.000 description 1
- 229910052749 magnesium Inorganic materials 0.000 description 1
- 230000035800 maturation Effects 0.000 description 1
- 238000005065 mining Methods 0.000 description 1
- 238000005457 optimization Methods 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 210000004483 pasc Anatomy 0.000 description 1
- 150000004965 peroxy acids Chemical class 0.000 description 1
- 235000021110 pickles Nutrition 0.000 description 1
- 238000006116 polymerization reaction Methods 0.000 description 1
- 238000010248 power generation Methods 0.000 description 1
- 230000001681 protective effect Effects 0.000 description 1
- 239000000376 reactant Substances 0.000 description 1
- 230000009257 reactivity Effects 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 239000011435 rock Substances 0.000 description 1
- RMAQACBXLXPBSY-UHFFFAOYSA-N silicic acid Chemical compound O[Si](O)(O)O RMAQACBXLXPBSY-UHFFFAOYSA-N 0.000 description 1
- 235000012239 silicon dioxide Nutrition 0.000 description 1
- 239000002002 slurry Substances 0.000 description 1
- 239000002689 soil Substances 0.000 description 1
- 229910052682 stishovite Inorganic materials 0.000 description 1
- -1 through analyzing Substances 0.000 description 1
- OGIDPMRJRNCKJF-UHFFFAOYSA-N titanium oxide Inorganic materials [Ti]=O OGIDPMRJRNCKJF-UHFFFAOYSA-N 0.000 description 1
- 229910052905 tridymite Inorganic materials 0.000 description 1
- 239000002351 wastewater Substances 0.000 description 1
Classifications
-
- 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
- C01F7/20—Preparation of aluminium oxide or hydroxide from aluminous ores using acids or salts
- C01F7/26—Preparation of aluminium oxide or hydroxide from aluminous ores using acids or salts with sulfuric acids or sulfates
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B33/00—Silicon; Compounds thereof
- C01B33/113—Silicon oxides; Hydrates thereof
- C01B33/12—Silica; Hydrates thereof, e.g. lepidoic silicic acid
-
- 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
- C01F7/44—Dehydration of aluminium oxide or hydroxide, i.e. all conversions of one form into another involving a loss of water
- C01F7/441—Dehydration of aluminium oxide or hydroxide, i.e. all conversions of one form into another involving a loss of water by calcination
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G49/00—Compounds of iron
- C01G49/009—Compounds containing, besides iron, two or more other elements, with the exception of oxygen or hydrogen
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/12—Surface area
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/19—Oil-absorption capacity, e.g. DBP values
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/80—Compositional purity
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Life Sciences & Earth Sciences (AREA)
- Geology (AREA)
- General Life Sciences & Earth Sciences (AREA)
- Geochemistry & Mineralogy (AREA)
- Compounds Of Alkaline-Earth Elements, Aluminum Or Rare-Earth Metals (AREA)
- Processing Of Solid Wastes (AREA)
Abstract
The invention discloses a kind of methods that high alumina coal gangue efficiently utilizes, and belong to industrial solid castoff application technology as the second resource field；This method is will to solidify after gangue or slag acid adding, it is acidified again, dissolve out, be filtered, washed obtain sulfur acid aluminium based on sulfate liquor and Silicon-rich removal of impurities acid sludge, sulfate liquor is used to prepare aluminium hydroxide or aluminium oxide, polyaluminium sulfate iron product, and acid sludge produces white carbon black through calcining；This method utilization of resources is reasonable, and without new solid waste discharge, product market constant is big, and a kind of practicable method can be provided for the resource utilization of high alumina coal gangue.
Description
Technical field
The present invention discloses a kind of method for efficiently utilizing high alumina coal gangue, belong to industrial solid castoff resource utilization and
Technical field of resource comprehensive utilization.
Background technique
Currently, gangue is a kind of black rock in coalification course with coal seam association, it is to choose and exploit in coal
The waste generated in the process.The yield of the annual gangue in China reaches the 15%-20% of coal mining total amount, reaches national industry
Waste generates the 40% of total amount, but total utilization rate is not high, and by 2015, the utilization rate of gangue just reached 70%, from
The target that utilization of coal gangue utilization rate reaches 80% is far apart, and pressure is very huge.A large amount of Piling of Gangue is together not
A large amount of soil can be only occupied, the ecological environment on periphery can be also polluted, also will cause the waste of resource.It is asked to solve these
Topic, will not only reinforce the innovation and popularization of traditional technology, it is necessary to explore that other utilizations of resources are reasonable, environmentally friendly technique skill
Art, by all kinds of means, multipath reinforce utilization of coal gangue utilize.
Extracting valuable element from gangue and producing related chemical products is a hot spot for efficiently utilizing gangue at present；
The gangue in China is in the majority with clay class, mostly contains aluminium element more, therefore extracting aluminium oxide from pelite gangue is in recent years
The research hotspot come.The method for extracting aluminium oxide from gangue at present mainly has acid system, alkaline process, sintering process, and alkaline process is due to alkali
Dosage is big, and aluminium recovery is low, level of residue it is big there are secondary pollution and the utilization of resources it is unreasonable, and sintering process energy consumption is high, is country
Provide the technical matters that should not be used, therefore the proper method of gangue synthetical recovery valuable element is acid system.
A kind of method that CN201310315648.3 has invented high efficiency extraction iron aluminium titanium from gangue, gangue is done
It is dry, crush after for neutralizing dry method acidleach, the acid sludge that pickle liquor is obtained by filtration is dry, and then acid adding mixes, through acidleach, molten
It solves, be filtered, washed, dry, and repeat above step, improve the dissolution rate of Iron in Coal Gangue aluminium titanium；The advantage of the invention is that
Most of carbonate, purifying mass in raw material, which are eliminated, using acid-soluble material improves the utilization rate of acid；Dissolution rate after acidleach
Height is conducive to the later use of acid sludge.
CN201610545655.6 proposes a kind of method for improving the leaching rate of aluminium in gangue, is existed with NaOH aqueous alkali
Efficient-decomposition gangue under atmospheric low-temperature improves the leaching rate of aluminium element；Advantages of the present invention: this method does not need high temperature dehydration
Roasting, reaction temperature is low, and the reaction time is short；Compared with traditional handicraft, operation of the present invention mild condition greatly reduces reaction temperature
Degree and reaction pressure, easy to operate and green high-efficient, low energy consumption, and environmental pollution is small, the dissolution rate of aluminium element can reach 60% with
On.
CN200510048215.1 is related to a kind of method for producing aluminium oxide using coal gangue as raw material, by smashed coal
Spoil is leached after high-temperature roasting with sodium hydroxide solution, filters residue, and filtrate is passed through CO2Gas makes Al (OH)3Precipitating, vacuum
Filtering, high temperature dehydration obtain Al2O3Product.Advantage of the invention is that reacting item using roasting salt-leaching combination method production technology
Part is mild, and production process is easy to control, and the waste water that technique generates can be recycled, and the waste residue generated after extraction can be used as rubber
The filler of product, environmentally protective, the recovery rate of aluminium oxide is also very high.
CN201010266645.1 is related to the side that a kind of coal gangue combustion lime-ash extracts aluminium oxide, silica and iron oxide
Method, gangue according to calorific value situation coal blending, realizes activating coal gangue while calcining power generation after pretreatment, generated
Electric power and steam are used for system；Lime-ash acidity extraction aluminium oxide, alkalinity extraction silica, and the comprehensive benefit for passing through by-product
With extraction iron oxide；Acid required for each process procedure, alkali, lime, extractant, CO2It is recycled in system.Bastard coal of the invention
The energy and chemical group Chengdu in stone are fully used, and drastically reduce the discharge amount of greenhouse gases and waste residue, improve
The economic benefit of system is that a kind of novel gangue greenization and high value added utilization technology, competitive advantage are obvious.
CN201310315648.3 discloses a kind of method of high efficiency extraction ferro-aluminum titanium in gangue, belongs to coal solid
Waste resource utilization technology field, gangue, for neutralizing the lysate of dry method acidleach clinker, neutralize after drying, grinding
Terminal acid concentration or pH value dissolve titanium oxide content in object out according to acidleach and determine；The filtered neutralization filtrate of neutralization reaction is used for
Aluminium, iron or aluminium, iron, titanium are separated, filter residue is neutralized and does not have to washing, directly acid adding mixing, carries out acid in chamber type electric resistance furnace after drying
Leaching reaction, is dissolved after reaction, is filtered, washed, filtrate is neutralized with fresh gangue, circulating repetition aforesaid operations, this hair
Bright method utilization rate is high, and the dissolution rates such as aluminium, iron, titanium are high, is aluminium, iron, titanium products open new raw material resources, it can be achieved that bastard coal
Stone high value added utilization.
Cheng Fangqin etc. has studied the influence factor that aluminium oxide is extracted from gangue, the results showed that, leaching time is to oxidation
The dissolution of aluminium influences maximum.The optimal conditions of dissolution be leaching time 3h, 650 DEG C of calcination temperature, hydrochloric acid acid amount 225mL(according to
Aluminium oxide and the molar ratio of hydrochloric acid reaction are 1:6 meter in gangue), solid-to-liquid ratio 1:3.
In conclusion researcher has done many work in terms of the efficient dissolution of gangue, especially in gangue
In terms of the high efficiency extraction of aluminium element and in terms of the preparation of related chemical products；But by reasonable process optimization and product design,
The method of polymeric aluminum sulfate iron, aluminium hydroxide (or further calcining production aluminium oxide) and white carbon black is produced also not using gangue
Appear in the newspapers announcement.
Summary of the invention
The purpose of the present invention is to provide a kind of method for efficiently utilizing high alumina coal gangue, this method is original with high alumina spoil
Material adds according to its own calorific value directly using or by remake extraction valuable element raw material after recirculating fluidized bed recycling heat
98% industrial sulphuric acid of mass concentration is first solidified, then according to chemical composition supplement residual acid, then it is acidified reaction, dissolved out
Journey extracts acid-soluble material aluminium, iron etc., and acid sludge roasting direct produces white carbon black；Acid-soluble material prepares polymeric aluminum sulfate iron and aluminium hydroxide
(or aluminium oxide) product, calcining acid-soluble material tail gas recycle sulfuric acid be recycled, calcined material using Bayer process production aluminium hydroxide or
Aluminium oxide, alkaline residue are then used for polyaluminium sulfate pH adjuster；This method is high alumina coal gangue efficiently using providing one kind
New approaches, new technology, each element rate of recovery is high in gangue, and process is generated without new solid waste, will become the following high alumina bastard coal
Maximally efficient one of the approach of stone resource utilization.
For the high alumina coal gangue in terms of ash content quality, each quality accounting that forms is Al2O3> 30%, Fe2O3< 15%, CaO <
2%, MgO < 2%.
The above method of the present invention has achieved the purpose that efficient to utilize high alumina coal gangue, the specific steps are as follows:
(1) gangue met the requirements is taken, as its low heat valve >=800cal/kg, then using recirculating fluidized bed recycling heat
Amount obtains slag；If its low heat valve calorific value < 800cal/kg, then be used directly, properties of powder performace then with heat recovery with
No determination, when recycling heat, properties of powder performace was 80 mesh screen over-size < 10%, when not recycling heat, crossed 120 mesh screen over-sizes
< 5%；
(2) in the mass ratio of the industrial sulphuric acid of mass concentration 98% and raw material be 1.1~1.2 ratio, high alumina coal gangue or its
Industrial sulphuric acid is added in slag, is reacted at room temperature~50 DEG C, is transferred to after its solidification in vertical acidification kiln, is pressed again simultaneously
The ratio that the mass ratio of industrial sulphuric acid and raw material is 0.1~0.2 adds 98% industrial sulphuric acid, 2~3h of acidification reaction time, acidification
Kiln entrance heat source temperature is 180~190 DEG C；
(3) after being acidified, acidulants is transferred in the reactive tank with stirring, are 1 by acidulants quality and lysate mass ratio:
2~3 ratio adds lysate, and 1~1.5h of stirring and dissolving at 60~80 DEG C obtains sulfate liquor through filtering, and filter residue is washed
It washs to washing lotion pH > 3 and obtains acid sludge；
(4) the part of sulfuric acid salting liquid of step (3) is spray-dried, calcines acquisition aluminium oxide first product, and tail gas recycle sulfuric acid is used for
System circulation uses, and aluminium oxide first product further calcines production aluminium oxide using Bayer process production aluminium hydroxide or aluminium hydroxide,
It is used after the alkali of recycling is concentrated for system circulation, alkaline residue is then used as the pH regulator of production polymeric aluminum sulfate iron, uses simultaneously
In supplement source of iron；Residual sulfuric acid salting liquid is aoxidized, and pH value is adjusted, and produces polymeric aluminum sulfate iron；
(5) acid sludge is calcined through 900~1000 DEG C, must reach the white carbon black product of HG/T3068-2008 standard E class requirement.
Lysate is the first time washing lotion that clear water or step (1) wash filter residue in the step (3).
Sulfate calcination temperature after the step (4) spray drying is 900~1000 DEG C, 2~3h when calcining；Aluminum sulfate
Iron polymeric reaction temperature is 60~80 DEG C, and polymerization time is 4~6h, is conventional fabrication process.
The principle of the present invention:
In order to make in gangue acid is molten to dissolve out as far as possible, the removal of impurities of acid sludge Silicon-rich, the quality of gangue or slag and sulfuric acid are realized
Than generally requiring to be 1.2~1.4, but it is added at one time sulfuric acid, then will lead to subsequent acidification reaction material transfer difficulty, be acidified kiln
Poor air permeability, therefore, the present invention use at room temperature~50 DEG C, pass through reactant such as carbonate, reactivity easy in gangue
High part kaolin or unformed aluminium oxide and sulfuric acid reaction generate sulfate, and sulfate band under solidification temperature is recycled to crystallize
The characteristics of water, realizes that mixture facilitates material in acidification kiln internal mobility and gas permeability from slurry to solid-state in for 24 hours；In order to mention
The dissolution rate of acid-soluble material in high gangue, only solidification is unable to satisfy requirement with acid, and therefore, the present invention takes solidfied material transfer process
The mode of middle spray acid supplements residual sulfuric acid, to guarantee that the dosage of acid meets technique requirement.Acidification reaction itself is exothermic reaction, only
The progress of reaction can be maintained by suitably supplementing certain heat source, measured, properly increased to control final dissolution acidulants middle reaches from acid
Entrance heat source temperature, again in cold conditions solidfied material surface condensation, will then participate in reaction, improve acid after free acid carburation by evaporation
Utilization rate.Acidification realizes conversion of the acid-soluble material to sulfate in gangue, and wherein aoxidizes silicic acid obtained by pasc reaction finally
Dehydration forms unformed oxidation, can separate in subsequent process in leaching with sulfate, while being acid sludge baked for producing white carbon black
It creates conditions.Part acid-soluble material is spray-dried to obtain the mixture based on anhydrous slufuric acid aluminium, and oxygen can be able to after calcining
To change the unformed product based on aluminium, sodium metaaluminate is converted into after alkali soluble, i.e., available traditional handicraft kind point-score prepares aluminium hydroxide,
Aluminium hydroxide again through calcining can produce aluminium oxide, the insoluble matter during alkali soluble be mainly iron, calcium, magnesium etc. oxide or
Alkali is used for the pH adjuster preparation polymeric aluminum sulfate iron of acid-soluble material solution, passes through polymeric aluminum sulfate iron and aluminium hydroxide
Or the reasonable arrangement of alumina product yield, the new solid waste generated during utilization of coal gangue utilizes on the one hand can be eliminated, separately
On the one hand the iron content in polymeric aluminum sulfate iron also can be improved；Unformed silica (no ash base) content is 96% in acid sludge
More than, pass through roasting removal residual carbon and bright lost article, as white carbon black product.
The invention has the following advantages over the prior art:
(1) by gangue curing mode, transfer and acidification reaction operational issue of the peracid cash than lower material are solved；
(2) Valuable Elements From Coal Gangue extracts product setting rationally, and added value is high, and process is generated without new solid waste；
(3) by way of secondary supplement acid, it ensure that acid amount needed for acid-soluble material reaction in gangue, by controlling entrance heat source
Temperature reduces acidulants free acid amount；
(4) alkaline residue is used for the pH adjuster of polymeric aluminum sulfate iron preparation, the ingredient in alkaline residue is not only taken full advantage of, also disappears
In addition to the problem of environmental pollution of alkaline residue；
(5) gangue valuable element extraction process is simple, technology maturation.
Detailed description of the invention
Fig. 1 is process flow diagram of the invention.
Specific embodiment
Below by embodiment, invention is further described in detail, but protection scope of the present invention be not limited to it is described
Content.
Embodiment 1
(1) as shown in Figure 1, coal shale in brick making and ash content analysis the results are shown in Table 1.1, as seen from table, this gangue has more high-incidence
Heat will should carry out again the utilization of slag after its heat recovery；
1.1 coal shale in brick making of table and ash content analysis
(2) by gangue crushed after being dried, being ground to 80 mesh screen over-sizes is 9.98%, recycles heat using recirculating fluidized bed
Obtain slag；
(3) by the gangue slag of step (2) in the industrial sulphur of the ratio addition mass concentration 98% of sour cash mass ratio 1:1.2
Acid solidifies at 50 DEG C；
(4) ratio for being 0.2 in industrial sulphuric acid and the mass ratio of slag, with spray after the gangue solidifying substance of step (3) is taken out
Mist form adds 98% industrial sulphuric acid, is transferred in vertical acidification kiln and carries out acidification reaction, and vertical acidification kiln entrance heating temperature is
180 DEG C, residence time 2.5h；
(5) after being acidified, acidification material is transferred in the reactive tank with stirring, is by acidulants quality and lysate mass ratio
The ratio of 1:2 adds clear water, stirs 1.5h at 60 DEG C, and dissolved matter is filtered to obtain sulfate liquor, filter residue with clear water wash to
PH > 3, first time washing lotion are used for the lysate of acidulants in next technique, and second of washing lotion is used for one of filter residue in next technique
Washing lotion, third time washing lotion then make two washing lotions of filter residue in next technique, and so on, last time washing is clear water；Table 1.2 is
Acid sludge chemical component；
The constituent analysis (wt%) of 1.2 acid sludge of table
(6) at the beginning of obtaining aluminium oxide after step (5) part of sulfuric acid salting liquid Direct spraying is dry, calcining (900 DEG C of calcining when 3h)
Product, aluminium oxide first product alkali soluble obtain sodium metaaluminate, prepare aluminium hydroxide or aluminium hydroxide through kind of a point-score and further calcine production oxidation
Aluminium, alkaline residue are then used as the pH regulator of production polymeric aluminum sulfate iron；Residual sulfuric acid salting liquid is adjusted through hydrogen peroxide oxidation with alkaline residue
PH value is 3, and polymeric aluminum sulfate iron is made according to a conventional method under the conditions of 60 DEG C of reaction 6h；
(7) step (5) acid sludge is calcined into obtain white carbon black product, through analyzing, SiO at 900 DEG C2For 97.48wt%, oil factor is
2.5, specific surface area 83m2/g。
Embodiment 2
(1) coal shale in brick making and ash content analysis the results are shown in Table 2.1, and as seen from table, this gangue low heat valve is 820cla/
Kg meets heat recovery requirement, and the utilization of slag will should be carried out again after its heat recovery；
2.1 coal shale in brick making of table and ash content analysis
(2) by gangue crushed after being dried, being ground to 80 mesh screen over-sizes is 6.23%, recycles heat using recirculating fluidized bed
Obtain slag；
(3) by the gangue slag of step (2) in the industrial sulphur of the ratio addition mass concentration 98% of sour cash mass ratio 1:1.1
Acid solidifies at normal temperature；
(4) ratio for being 0.1 in industrial sulphuric acid and the mass ratio of slag, with spray after the gangue solidifying substance of step (3) is taken out
Mist form adds 98% industrial sulphuric acid, is transferred in vertical acidification kiln and carries out acidification reaction, and vertical acidification kiln entrance heating temperature is
190 DEG C, residence time 3h；
(5) after being acidified, acidification material is transferred in the reactive tank with stirring, is by acidulants quality and lysate mass ratio
The first time washing lotion of the ratio addition embodiment 1 of 1:2.5, stirs 1h at 80 DEG C, dissolved matter is filtered to obtain sulfate liquor, filter
Slag circulation washing (successively use second of washing lotion of 1 step of embodiment (5) as a washing lotion, third time washing lotion as two washing lotions, clearly
Water), washing to pH > 3, first time washing lotion is used for the lysate of acidulants in next technique, and second of washing lotion is used for next technique
One washing lotion of middle filter residue, and clear water washing lotion then makees two washing lotions of filter residue in next technique；Table 2.2 is acid sludge chemical component；
The constituent analysis (wt%) of 2.2 acid sludge of table
(6) at the beginning of obtaining aluminium oxide after step (5) part of sulfuric acid salting liquid Direct spraying is dry, calcining (1000 DEG C of calcining when 2h)
Product, aluminium oxide first product alkali soluble obtain sodium metaaluminate, prepare aluminium hydroxide or aluminium hydroxide through kind of a point-score and further calcine production oxidation
Aluminium, alkaline residue are then used as the pH regulator of production polymeric aluminum sulfate iron；Residual sulfuric acid salting liquid is adjusted through hydrogen peroxide oxidation with alkaline residue
PH value is 4, and polymeric aluminum sulfate iron is made according to a conventional method under the conditions of 70 DEG C of reaction 5h；
(7) step (5) acid sludge is calcined into obtain white carbon black product, through analyzing, SiO at 1000 DEG C2For 96.09wt%, oil factor is
2.3, specific surface area 81m2/g。
Embodiment 3
(1) coal shale in brick making and ash content analysis the results are shown in Table 3.1, and as seen from table, this gangue low heat valve is 452cla/
Kg does not have heat recovery requirement, and gangue is dry, broken, grinding directly uses；
3.1 coal shale in brick making of table and ash content analysis
(2) being ground to step (1) gangue and sieving with 100 mesh sieve screen over-size is 4.56%；
(3) by the gangue slag of step (2) in the industrial sulphur of the ratio addition mass concentration 98% of sour cash mass ratio 1:1.2
Acid solidifies at 35 DEG C；
(4) ratio for being 0.15 in industrial sulphuric acid and the mass ratio of slag, after the gangue solidifying substance of step (3) is taken out with
Sprayable adds 98% industrial sulphuric acid, is transferred in vertical acidification kiln and carries out acidification reaction, and vertical acidification kiln entrance heating temperature is
185 DEG C, residence time 2.5h；
(5) after being acidified, acidification material is transferred in the reactive tank with stirring, is by acidulants quality and lysate mass ratio
The first time washing lotion of the ratio addition embodiment 2 of 1:3, stirs 1.2h at 70 DEG C, dissolved matter is filtered to obtain sulfate liquor, filter
Slag circulation washing (successively use (5) second of washing lotion of 2 step of embodiment as a washing lotion, third time washing lotion as two washing lotions, clearly
Water), washing to pH > 3, first time washing lotion is used for the lysate of acidulants in next technique, and second of washing lotion is used for next technique
One washing lotion of middle filter residue, and clear water washing lotion then makees two washing lotions of filter residue in next technique；Table 3.2 is acid sludge chemical component；
The constituent analysis (wt%) of 3.2 acid sludge of table
(6) aluminium oxide first product is obtained after step (5) part of sulfuric acid salting liquid Direct spraying is dry, calcining (950 DEG C of calcining when 2h),
Aluminium oxide first product alkali soluble obtains sodium metaaluminate, prepares aluminium hydroxide or aluminium hydroxide through kind of a point-score and further calcines production aluminium oxide,
Alkaline residue is then used as the pH regulator of production polymeric aluminum sulfate iron；Residual sulfuric acid salting liquid adjusts pH through hydrogen peroxide oxidation, with alkaline residue
Value is 3, and polymeric aluminum sulfate iron is made according to a conventional method under the conditions of 80 DEG C of reaction 4h；
(7) 1000 DEG C of acid sludge of step (5) are calcined into obtain white carbon black product, through analyzing, SiO2For 97.02wt%, oil factor 2.0,
Specific surface area is 75m2/g。
Embodiment 4
(1) coal shale in brick making and ash content analysis the results are shown in Table 4.1, and as seen from table, this gangue low heat valve is 639cla/
Kg does not have heat recovery requirement, and gangue is dry, broken, grinding directly uses；
4.1 coal shale in brick making of table and ash content analysis
(2) being ground to step (1) gangue and sieving with 100 mesh sieve screen over-size is 5.27%；
(3) by the gangue slag of step (2) in the industrial sulphur of the ratio addition mass concentration 98% of sour cash mass ratio 1:1.1
Acid solidifies at 40 DEG C；
(4) ratio for being 0.2 in industrial sulphuric acid and the mass ratio of slag, with spray after the gangue solidifying substance of step (3) is taken out
Mist form adds 98% industrial sulphuric acid, is transferred in vertical acidification kiln and carries out acidification reaction, and vertical acidification kiln entrance heating temperature is
180 DEG C, residence time 3h；
(5) after being acidified, acidification material is transferred in the reactive tank with stirring, is by acidulants quality and lysate mass ratio
The first time washing lotion of the ratio addition embodiment 3 of 1:2.5, stirs 1h at 75 DEG C, dissolved matter is filtered to obtain sulfate liquor, filter
The washing of slag circulation (successively use second of washing lotion in 3 step of embodiment (5) as a washing lotion, third time washing lotion as two washing lotions,
Clear water), washing to pH > 3, first time washing lotion is used for the lysate of acidulants in next technique, and second of washing lotion is used for next work
A washing lotion of filter residue in skill, and clear water washing lotion then makees two washing lotions of filter residue in next technique；Table 4.2 is acid sludge chemical component；
The constituent analysis (wt%) of 4.2 acid sludge of table
(6) at the beginning of obtaining aluminium oxide after step (5) part of sulfuric acid salting liquid Direct spraying is dry, calcining (1000 DEG C of calcining when 2h)
Product, aluminium oxide first product alkali soluble obtain sodium metaaluminate, prepare aluminium hydroxide or aluminium hydroxide through kind of a point-score and further calcine production oxidation
Aluminium, alkaline residue are then used as the pH regulator of production polymeric aluminum sulfate iron；Residual sulfuric acid salting liquid is adjusted through hydrogen peroxide oxidation with alkaline residue
PH value is 4, and polymeric aluminum sulfate iron is made according to a conventional method under the conditions of 65 DEG C of reaction 5h；
(7) step (5) acid sludge is calcined into obtain white carbon black product, through analyzing, SiO at 900 DEG C2For 97.42wt%, oil factor is
2.4, specific surface area is 81 m2/g。
Claims (8)
1. a kind of method for efficiently utilizing high alumina coal gangue, it is characterised in that: add quality in high alumina coal gangue or its slag
The industrial concentrated sulfuric acid of concentration 98% is first solidified, then it is acidified, dissolve out, be filtered, washed, obtain sulfate liquor and acid sludge；Portion
Point sulfate liquor is spray-dried, calcining, and aluminium hydroxide is made in Bayer process or aluminium hydroxide further calcine preparation and aoxidized
Aluminium, remainder sulfate liquor is for producing polymeric aluminum sulfate iron；Acid sludge produces white carbon black after calcining.
2. the efficient method using high alumina coal gangue according to claim 1, which is characterized in that specific step is as follows:
(1) in the mass ratio of the industrial sulphuric acid of mass concentration 98% and raw material be 1.1~1.2 ratio, high alumina coal gangue or its
Industrial sulphuric acid is added in slag, is reacted at room temperature~50 DEG C, is transferred to after its solidification in vertical acidification kiln, is pressed again simultaneously
The ratio that the mass ratio of industrial sulphuric acid and raw material is 0.1~0.2 adds 98% industrial sulphuric acid, 2~3h of acidification reaction time, acidification
Kiln entrance heat source temperature is 180~190 DEG C；After acidification, acidulants are transferred in the reactive tank with stirring, by acidifying substance
Amount adds lysate with the ratio that lysate mass ratio is 1:2~3, and 1~1.5h of stirring and dissolving at 60~80 DEG C is obtained through filtering
Sulfate liquor is obtained, residue washing to washing lotion pH > 3 obtains acid sludge；
(2) part of sulfuric acid salting liquid is spray-dried, calcines acquisition aluminium oxide first product, and tail gas recycle Sulphuric acid makes for recycling
With aluminium oxide first product further calcines production aluminium oxide using Bayer process production aluminium hydroxide or aluminium hydroxide；Residual sulfuric acid salt
Solution is aoxidized, and adjustment pH value is 3-4, produces polymeric aluminum sulfate iron；
(3) acid sludge produces white carbon black after calcining.
3. the efficient method using high alumina coal gangue according to claim 1 or 2, it is characterised in that: work as high alumina coal gangue
Low heat valve < 800cal/kg when, do not recycle heat and directly use；When high alumina coal gangue low heat valve >=
When 800cal/kg, then slag is obtained using recirculating fluidized bed recycling heat.
4. the efficient method using high alumina coal gangue according to claim 3, it is characterised in that: high alumina coal gangue does not recycle
When heat, properties of powder performace was 120 mesh screen over-size < 5%, and properties of powder performace was 80 mesh screen over-size < 10% when recycling heat.
5. the efficient method using high alumina coal gangue according to claim 2, it is characterised in that: lysate in step (1)
The first time washing lotion of filter residue is washed for clear water or step (1).
6. the efficient method using high alumina coal gangue according to claim 2, it is characterised in that: step (2) spray drying
Sulfate calcination temperature afterwards is 900~1000 DEG C, 2~3h when calcining；Aluminium iron sulfate polymeric reaction temperature is 60~80 DEG C, is gathered
The conjunction time is 4~6h.
7. the efficient method using high alumina coal gangue according to claim 1 or 2, it is characterised in that: Bayer process produces hydrogen
Alkaline residue in alumina technology is used as the pH regulator of production polymeric aluminum sulfate iron, while for supplementing source of iron.
8. the efficient method using high alumina coal gangue according to claim 1 or 2, it is characterised in that: acid sludge through 900~
1000 DEG C are calcined to obtain product white carbon black.
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| CN109835930A (en) * | 2019-02-19 | 2019-06-04 | 昆明理工大学 | A kind of production method of aluminium oxide |
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| CN113336253A (en) * | 2021-05-24 | 2021-09-03 | 昆明理工大学 | Method for extracting aluminum oxide from high-aluminum coal gangue by using high-concentration SO2 |
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| CN115340424A (en) * | 2022-08-15 | 2022-11-15 | 昌晖自动化科技(济南)有限公司 | Coal gangue magnetized soil conditioner and preparation method thereof |
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