CN102020299A - Method for producing industrial activated aluminum oxide from pulverized fuel ash - Google Patents
Method for producing industrial activated aluminum oxide from pulverized fuel ash Download PDFInfo
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- CN102020299A CN102020299A CN 201010601489 CN201010601489A CN102020299A CN 102020299 A CN102020299 A CN 102020299A CN 201010601489 CN201010601489 CN 201010601489 CN 201010601489 A CN201010601489 A CN 201010601489A CN 102020299 A CN102020299 A CN 102020299A
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- PNEYBMLMFCGWSK-UHFFFAOYSA-N Alumina Chemical compound [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 title claims abstract description 36
- 238000004519 manufacturing process Methods 0.000 title claims abstract description 23
- 239000000446 fuel Substances 0.000 title abstract 3
- 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 claims abstract description 201
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 claims abstract description 170
- 239000007788 liquid Substances 0.000 claims abstract description 134
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims abstract description 119
- 229910052742 iron Inorganic materials 0.000 claims abstract description 74
- 229910052782 aluminium Inorganic materials 0.000 claims abstract description 60
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 claims abstract description 57
- 238000000034 method Methods 0.000 claims abstract description 50
- 238000001354 calcination Methods 0.000 claims abstract description 29
- 229910052799 carbon Inorganic materials 0.000 claims abstract description 23
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 19
- 238000001035 drying Methods 0.000 claims abstract description 3
- 239000010881 fly ash Substances 0.000 claims description 149
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 107
- 239000000243 solution Substances 0.000 claims description 104
- 238000006243 chemical reaction Methods 0.000 claims description 57
- 238000001953 recrystallisation Methods 0.000 claims description 56
- 239000004411 aluminium Substances 0.000 claims description 55
- 238000001816 cooling Methods 0.000 claims description 54
- 238000002425 crystallisation Methods 0.000 claims description 49
- 230000008025 crystallization Effects 0.000 claims description 49
- 239000000706 filtrate Substances 0.000 claims description 39
- 238000007885 magnetic separation Methods 0.000 claims description 39
- 238000000926 separation method Methods 0.000 claims description 39
- 238000005188 flotation Methods 0.000 claims description 36
- 238000007670 refining Methods 0.000 claims description 35
- 239000013078 crystal Substances 0.000 claims description 34
- 239000002002 slurry Substances 0.000 claims description 34
- 238000001556 precipitation Methods 0.000 claims description 33
- 238000010438 heat treatment Methods 0.000 claims description 27
- 238000004137 mechanical activation Methods 0.000 claims description 25
- BUACSMWVFUNQET-UHFFFAOYSA-H dialuminum;trisulfate;hydrate Chemical compound O.[Al+3].[Al+3].[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O BUACSMWVFUNQET-UHFFFAOYSA-H 0.000 claims description 24
- 238000001704 evaporation Methods 0.000 claims description 21
- 230000008020 evaporation Effects 0.000 claims description 21
- 238000005119 centrifugation Methods 0.000 claims description 19
- UQSXHKLRYXJYBZ-UHFFFAOYSA-N iron oxide Inorganic materials [Fe]=O UQSXHKLRYXJYBZ-UHFFFAOYSA-N 0.000 claims description 19
- 230000003252 repetitive effect Effects 0.000 claims description 19
- 239000002253 acid Substances 0.000 claims description 17
- 239000012141 concentrate Substances 0.000 claims description 17
- NDLPOXTZKUMGOV-UHFFFAOYSA-N oxo(oxoferriooxy)iron hydrate Chemical compound O.O=[Fe]O[Fe]=O NDLPOXTZKUMGOV-UHFFFAOYSA-N 0.000 claims description 17
- 230000004044 response Effects 0.000 claims description 17
- 238000003756 stirring Methods 0.000 claims description 17
- 238000000967 suction filtration Methods 0.000 claims description 17
- 230000008569 process Effects 0.000 claims description 15
- SZVJSHCCFOBDDC-UHFFFAOYSA-N iron(II,III) oxide Inorganic materials O=[Fe]O[Fe]O[Fe]=O SZVJSHCCFOBDDC-UHFFFAOYSA-N 0.000 claims description 5
- 239000001117 sulphuric acid Substances 0.000 claims description 5
- 235000011149 sulphuric acid Nutrition 0.000 claims description 5
- 238000000227 grinding Methods 0.000 claims description 4
- 239000011259 mixed solution Substances 0.000 claims description 4
- 238000002791 soaking Methods 0.000 claims description 4
- 239000006229 carbon black Substances 0.000 claims description 3
- 230000035484 reaction time Effects 0.000 claims description 3
- 238000003837 high-temperature calcination Methods 0.000 claims description 2
- 238000003801 milling Methods 0.000 claims description 2
- TWNQGVIAIRXVLR-UHFFFAOYSA-N oxo(oxoalumanyloxy)alumane Chemical compound O=[Al]O[Al]=O TWNQGVIAIRXVLR-UHFFFAOYSA-N 0.000 abstract description 9
- 239000007787 solid Substances 0.000 abstract description 4
- 239000012535 impurity Substances 0.000 abstract description 3
- JEIPFZHSYJVQDO-UHFFFAOYSA-N iron(III) oxide Inorganic materials O=[Fe]O[Fe]=O JEIPFZHSYJVQDO-UHFFFAOYSA-N 0.000 abstract description 2
- 230000003213 activating effect Effects 0.000 abstract 1
- 229910052593 corundum Inorganic materials 0.000 abstract 1
- 229910001845 yogo sapphire Inorganic materials 0.000 abstract 1
- 238000004064 recycling Methods 0.000 description 31
- 238000002156 mixing Methods 0.000 description 30
- 238000000605 extraction Methods 0.000 description 18
- 239000003921 oil Substances 0.000 description 18
- 239000012452 mother liquor Substances 0.000 description 16
- 239000010413 mother solution Substances 0.000 description 16
- 238000005406 washing Methods 0.000 description 16
- 238000000498 ball milling Methods 0.000 description 15
- 238000011109 contamination Methods 0.000 description 15
- 238000010908 decantation Methods 0.000 description 15
- 239000012065 filter cake Substances 0.000 description 15
- 238000009413 insulation Methods 0.000 description 15
- 239000006227 byproduct Substances 0.000 description 14
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 10
- CPLXHLVBOLITMK-UHFFFAOYSA-N Magnesium oxide Chemical compound [Mg]=O CPLXHLVBOLITMK-UHFFFAOYSA-N 0.000 description 9
- 239000000843 powder Substances 0.000 description 7
- 239000010883 coal ash Substances 0.000 description 5
- 238000005265 energy consumption Methods 0.000 description 5
- 238000005554 pickling Methods 0.000 description 5
- 239000002994 raw material Substances 0.000 description 5
- 229910004298 SiO 2 Inorganic materials 0.000 description 4
- 230000008901 benefit Effects 0.000 description 4
- 239000004568 cement Substances 0.000 description 4
- 239000007789 gas Substances 0.000 description 4
- 239000000395 magnesium oxide Substances 0.000 description 4
- 238000002360 preparation method Methods 0.000 description 3
- 239000000047 product Substances 0.000 description 3
- 238000005245 sintering Methods 0.000 description 3
- 239000000126 substance Substances 0.000 description 3
- 238000004131 Bayer process Methods 0.000 description 2
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 2
- 239000002956 ash Substances 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 239000004574 high-performance concrete Substances 0.000 description 2
- IXCSERBJSXMMFS-UHFFFAOYSA-N hydrogen chloride Substances Cl.Cl IXCSERBJSXMMFS-UHFFFAOYSA-N 0.000 description 2
- 229910000041 hydrogen chloride Inorganic materials 0.000 description 2
- 229910052500 inorganic mineral Inorganic materials 0.000 description 2
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 description 2
- 239000011707 mineral Substances 0.000 description 2
- 229910052710 silicon Inorganic materials 0.000 description 2
- 239000010703 silicon Substances 0.000 description 2
- ZAMOUSCENKQFHK-UHFFFAOYSA-N Chlorine atom Chemical compound [Cl] ZAMOUSCENKQFHK-UHFFFAOYSA-N 0.000 description 1
- YCKRFDGAMUMZLT-UHFFFAOYSA-N Fluorine atom Chemical compound [F] YCKRFDGAMUMZLT-UHFFFAOYSA-N 0.000 description 1
- 229910007981 Si-Mg Inorganic materials 0.000 description 1
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 1
- 229910008316 Si—Mg Inorganic materials 0.000 description 1
- 239000002250 absorbent Substances 0.000 description 1
- 230000002745 absorbent Effects 0.000 description 1
- 230000009471 action Effects 0.000 description 1
- 239000003463 adsorbent Substances 0.000 description 1
- 239000003513 alkali Substances 0.000 description 1
- 229940037003 alum Drugs 0.000 description 1
- 238000004458 analytical method Methods 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 239000011575 calcium Substances 0.000 description 1
- 229910052791 calcium Inorganic materials 0.000 description 1
- 239000003054 catalyst Substances 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 239000000460 chlorine Substances 0.000 description 1
- 229910052801 chlorine Inorganic materials 0.000 description 1
- 239000004927 clay Substances 0.000 description 1
- 239000003245 coal Substances 0.000 description 1
- 238000002485 combustion reaction Methods 0.000 description 1
- 235000009508 confectionery Nutrition 0.000 description 1
- 238000007599 discharging Methods 0.000 description 1
- 229910000514 dolomite Inorganic materials 0.000 description 1
- 239000010459 dolomite Substances 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 239000003337 fertilizer Substances 0.000 description 1
- 238000001914 filtration Methods 0.000 description 1
- 239000011737 fluorine Substances 0.000 description 1
- 229910052731 fluorine Inorganic materials 0.000 description 1
- 238000005272 metallurgy Methods 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 239000003345 natural gas Substances 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 239000000049 pigment Substances 0.000 description 1
- 238000003672 processing method Methods 0.000 description 1
- 238000000746 purification Methods 0.000 description 1
- LIVNPJMFVYWSIS-UHFFFAOYSA-N silicon monoxide Chemical compound [Si-]#[O+] LIVNPJMFVYWSIS-UHFFFAOYSA-N 0.000 description 1
- 229910052814 silicon oxide Inorganic materials 0.000 description 1
- 239000002912 waste gas Substances 0.000 description 1
- 239000002699 waste material Substances 0.000 description 1
- 239000002351 wastewater Substances 0.000 description 1
Landscapes
- Compounds Of Alkaline-Earth Elements, Aluminum Or Rare-Earth Metals (AREA)
- Processing Of Solid Wastes (AREA)
Abstract
The invention discloses a method for producing industrial activated aluminum oxide from pulverized fuel ash, comprising the following steps: mechanically activating the pulverized fuel ash, floating and removing carbon, magnetically selecting and removing iron, impregnating in sulfuric acid to extract aluminum, separating solid and liquid, condensing rough liquid of aluminum sulfate, re-crystallizing aluminum sulfate, separating solid and liquid for the second time, dehydrating and drying aluminum sulfate, and calcining aluminum sulfate at a high temperature so as to obtain the industrial activated Al2O3 in which the content of Fe2O3 is lower than 0.5%; and the method completely meets the technical requirement of HG/T3927-2007 industrial activated aluminum oxide. The method is simple in technique, short in flow, easy to control production process, high in aluminum oxide extract rate, low in production cost, low in impurity content, and stable in quality.
Description
Technical field
The present invention relates to the resource utilization and the comprehensive utilization method of flyash, relate to a kind of method of flyash manufacture activated alumina specifically, promptly adopt finite concentration sulfuric acid heating and pressurizing to leach Tai-Ace S 150, after concentrating, adopt the method deironing of recrystallization, prepare Fe content and be lower than 0.02% industrial aluminum sulphate, the direct calcining of Tai-Ace S 150 obtains iron oxide content and is lower than 0.5% industrial active A l
2O
3
Background technology
Flyash is remaining solid residue behind coal-burning power plant's coal combustion, and China's flyash quantity discharged in 2007 reaches 2,500,000,000 tons, expects the year two thousand twenty whole nation flyash quantity discharged and will reach more than 5,000,000,000 tons.The level of comprehensive utilization of flyash and the raising of utilization ratio are related to the sound development of China's energy industry and the sustainable development of social environment.On chemical constitution, flyash is a kind of aluminium ore that is rich in the medium-grade of silico-aluminate, and along with the continuous exhaustion of China's alum clay resource, utilizes flyash to extract aluminium and have very wide application prospect.
The technical grade aluminum oxide has purposes very widely, is mainly used in industries such as oil refining, chemical fertilizer, petrochemical industry, Sweet natural gas, system oxygen and chemical industry, mainly as gas and liquid absorbent, fluorine adsorbent, the agent of suction chlorine, siccative and support of the catalyst etc.From flyash, extract aluminum oxide, mainly contain two kinds of methods at present, i.e. alkaline sintering method and pickling process.The patent of invention that adopts the alkaline sintering method to produce aluminum oxide has: Chinese invention patent application number 200710150915.0 discloses a kind of method of extracting high-purity ultra-fine alumina from flyash, 200710017304.9 disclose a kind of method of extracting aluminum oxide and producing cement from fag end thereof from aluminous fly-ash, 200410090949.1 disclose a kind of method of utilizing flyash and Wingdale combination producing aluminum oxide and cement etc., but, the energy consumption of alkaline sintering method is big, producing a large amount of secondaries piles up, 1 ton of flyash of every processing, will produce 10 tons residue, therefore, having limited it applies.
Production technique with pickling process extraction aluminum oxide from flyash is simple relatively, has reasonable handiness, its biggest advantage is aluminum oxide in the flyash and silicon oxide can be separated, and handle the quantity discharged that has reduced waste water, waste gas and waste residue in the process of flyash significantly, the residue that produces is rich in high silico-calcium, therefore can be directly as the active mineral admixture of high performance concrete etc.Common pickling process is divided hydrochloric acid pickling process and vitriol lixiviation method, owing to need to produce hydrogen chloride gas in the production process of hydrochloric acid pickling process, adopt water to absorb the concentration of making hydrochloric acid soln and be no more than 36%, need the extra moisture content of mass consumption, thoroughly will not cause hydrogen chloride gas to leak in case absorb, and hydrochloric acid has bigger action of rust to hardware, thereby influenced it and apply.Comparatively speaking, vitriol lixiviation is owned by France in a kind of more satisfactory method, for example: Chinese invention patent application number 200510048274.9 discloses a kind of method of alumina of extracting from flyash, 200610048295.5 disclose and a kind ofly produced method of alumina by flyash, 200710012997.2 disclose a kind of fly-ash Preparation method of alumina etc. of utilizing, but, these patented methods are to be used for the production metallurgy grade aluminum oxide mostly, and, because the intermediate Tai-Ace S 150 that obtains does not pass through the purification removal of impurities, but in follow-up process treatment process, adopt the energy consumption height, Bayer process backward in technique is purified, that is: the Tai-Ace S 150 crystal obtains foreign matter content than higher intermediate γ-Al through once calcining
2O
3, then molten through alkali, plant branch, filtration, washing, secondary clacining and obtain the lower Al of foreign matter content
2O
3, have that complex process, procedure links are many, energy consumption and shortcomings such as resource consumption is big, production cost height, be difficult to be applied.
Summary of the invention
The object of the invention is to provide the processing method of a kind of flyash manufacture activated alumina and comprehensive utilization thereof.The present invention has simplified purifying technique, has that technology is simple, flow process is short, production process is easy to control, alumina extraction ratio height, low, low, the stay-in-grade advantage of product foreign matter content of production cost, and is easy to utilize.
The method of flyash manufacture activated alumina is characterized in that comprising following step:
(1) mechanical activation: with flyash process mechanical activation;
(2) flotation de-carbon: will add water through the flyash of mechanical activation, and fully stir, and remove and do not fire clean carbon black;
(3) iron removal by magnetic separation: remove ferric oxide through magnetic separation;
(4) sulfuric acid lixiviate aluminium: will add the vitriol oil through the flyash raffinate after flotation carbon, the magnetic separation iron and carry out heating and pressurizing reaction 1～6h in acid tolerance response equipment, the top temperature of reaction is 200 ℃～240 ℃, and pressure is 0.1～0.5MPa;
(5) solid-liquid separation: after the reaction cooling, reaction solution adds water, and after the heated and boiled, suction filtration obtains the thick liquid of Tai-Ace S 150;
(6) the thick liquid of Tai-Ace S 150 concentrates: the thick liquid evaporation concentration of Tai-Ace S 150, and cooling obtains the Tai-Ace S 150 concentrated solution;
(7) Tai-Ace S 150 recrystallization: the heating of Tai-Ace S 150 concentrated solution is cooled off recrystallization with solution then, and precipitation separation and clear liquid obtain refining crystallization Tai-Ace S 150 slurries;
(8) secondary solid-liquid separation: gained refining crystallization Tai-Ace S 150 slurries are carried out solid-liquid separation, obtain low iron crystalline sulfuric acid aluminium filtrate;
(9) Tai-Ace S 150 dewatered drying: finally obtain low iron crystalline sulfuric acid aluminium filtrate oven dry, obtain Fe content and be lower than high-purity technical grade Tai-Ace S 150 of 0.02%;
(10) Tai-Ace S 150 high-temperature calcination: resulting high-purity industrial aluminum sulphate obtains Fe through the excess temperature calcining
2O
3Content is lower than 0.5% industrial active A l
2O
3
The method of aforesaid flyash manufacture activated alumina, the mechanical activation that it is characterized in that step (1) are that to adopt milling equipment to carry out levigate, and the grinding time is 0.5～6h;
In the step (2), be that 1:1～1:3 adds water according to the mass ratio of flyash and water;
In the step (4), the mass concentration scope of flyash sulfuric acid mixed solution is 30%～95%, and the solid-to-liquid ratio of flyash and sulphuric acid soln is 1:1～1:15 mass ratio;
In the step (5), after the reaction cooling, the mass ratio according to flyash and water in flyash is that 1:10～1:20 adds water;
In the step (6), the thick liquid of Tai-Ace S 150 is 90 ℃～130 ℃ evaporation concentration, and the crystal weight that control is separated out accounts for 40%～65% of the former weight of Tai-Ace S 150 liquid;
In the step (7), the Heating temperature of Tai-Ace S 150 concentrated solution is 40 ℃～70 ℃, and soaking time is 1～6h, recrystallization operation repetitive operation 2～6 times;
In the step (8), use centrifugation or vacuum belt filter;
In the step (9), the bake out temperature of low iron Tai-Ace S 150 filtrate is 70～100 ℃;
In the step (10), the calcining temperature of high-purity industrial aluminum sulphate is at 500 ℃～900 ℃, and calcination time is 1～5h.
The method of aforesaid flyash manufacture activated alumina is characterized in that the grinding time of step (1) mechanical activation is 1～3h;
In the step (4), the mass concentration scope of flyash sulfuric acid mixed solution is 40%～70%, and the solid-to-liquid ratio of flyash and sulphuric acid soln is 1:5～1:10 mass ratio, and the heating and pressurizing reaction times is 3～4h;
In the step (5), after the reaction cooling, the mass ratio according to flyash and water in flyash is that 1:12～1:18 adds water;
In the step (6), the thick liquid of Tai-Ace S 150 is 100～120 ℃ of evaporation concentration;
In the step (7), the Heating temperature of Tai-Ace S 150 concentrated solution is 50 ℃～60 ℃, and soaking time is 4～5h, recrystallization operation repetitive operation 2～6 times;
In the step (8), use centrifugation or vacuum belt filter;
In the step (9), the bake out temperature of low iron Tai-Ace S 150 filtrate is 80 ℃～90 ℃;
In the step (10), the calcining temperature of high-purity industrial aluminum sulphate is at 600 ℃～850 ℃, and calcination time is 2～4h.
The method of aforesaid flyash manufacture activated alumina is characterized in that flyash after the flotation de-carbon, adopts wet magnetic separation to remove magnetite.
The method of aforesaid flyash manufacture activated alumina is characterized in that the heating and pressurizing reaction times is 3～4h in the step (4).
The invention has the advantages that:
1, employing vitriol lixiviation method is extracted the aluminium in the flyash, and the process energy consumption of preparation Tai-Ace S 150 is low, simple to operate.
2, the method deironing of adopting magnetic separation and recrystallization to combine, operation steps is simple, and cost is lower, is easy to the industrialization deironing of Tai-Ace S 150.
3, the residue mother liquor in the secondary solid-liquid separation process turns back to Tai-Ace S 150 recrystallization operation and continues to extract Tai-Ace S 150.When Recycling Mother Solution surpassed 3～5 times, when foreign matter content was higher, through concentrating, precipitation was separated out in cooling, and oven dry can obtain the Aluminum Sulfate Solution crystal then.
3, high-purity industrial aluminum sulphate of preparing can directly be calcined and prepare industrial active A l
2O
3, need not that adopting process complexity, procedure links are many, energy consumption and resource consumption is big, production cost is high Bayer process circular treatment.
5, the present invention realizes 100% comprehensive utilization of fly ash when obtaining the higher aluminum extraction yield, has realized the resource utilization of flyash all the components, removes and can produce high-purity industrial aluminum sulphate and industrial active A l
2O
3Beyond the product, can also obtain not fire products such as clean carbon, magnetite powder, high ferro Tai-Ace S 150, high silicon ash, comprehensive utilization benefit is remarkable.
Embodiment
Further set forth the present invention by the following examples, these embodiment are only presented for purposes of illustration, do not limit the scope of the invention.The experimental technique of unreceipted actual conditions in the following example is usually according to normal condition.
Embodiment 1: the raw material powder coal ash consists of: Al
2O
3Content 37.7%, Fe
2O
3Content 4.38%, CaO content 3.74%, MgO content 0.54%, SiO
2Content 49.9%, loss on ignition 1.92%.The raw material powder coal ash also can adopt other compositions and corresponding amount thereof.
With flyash ball milling 1h in ball mill, carry out mechanical activation; Mass ratio according to flyash and water 1:3 adds water, fully stirs, and removes through flotation and does not fire clean deceiving, and it can be used for making carbon black or heat is produced in direct burning; Remove ferric oxide through magnetic separation again, the impurity magnetite powder that obtains is used to produce cement, makes iron oxide black pigment or ironmaking; To be made into h 2 so 4 concentration through the flyash raffinate after the flotation carbon, magnetic separation iron and the vitriol oil is 40% mixing solutions, the solid-to-liquid ratio (mass ratio) of control flyash and mixing solutions is 1:8, in acid tolerance response equipment, carry out heating and pressurizing reaction 3h, the top temperature of reaction is 240 ℃, and pressure is 0.5MPa; After the reaction cooling, be that 1:10 adds water according to the mass ratio of flyash and water, after the heated and boiled, suction filtration obtains filter cake, and is the water washing of 1:2 with the mass ratio of flyash and water, obtains the thick liquid of Tai-Ace S 150, and the extraction yield of analysis aluminium is 70%.This step is separated the SiO that obtains
2The solid residue that content is high after 70 ℃～120 ℃ oven dry, obtains high silicon ash, directly is mixed together as the active mineral admixture of high performance concrete or with light dolomite, light calcined magnesia and is mixed with novel Si-Mg cement.
100 ℃ of evaporation concentration, after the cooling, the crystal weight that control is separated out accounts for 40% of the former weight of Tai-Ace S 150 liquid, obtains the Tai-Ace S 150 concentrated solution with the thick liquid of Tai-Ace S 150; The Tai-Ace S 150 concentrated solution is heated to 50 ℃, and insulation 4h, then solution is cooled off recrystallization, make most of Tai-Ace S 150 crystallization separate out, adopt decantation that precipitation is separated with top clear liquid again, thereby obtain refining crystallization Tai-Ace S 150 slurries.With aforesaid recrystallization operation repetitive operation 3 times, to remove iron contamination to greatest extent; Gained refining crystallization Tai-Ace S 150 slurries are carried out solid-liquid separation, can use centrifugation or vacuum belt filter, obtain low iron crystalline sulfuric acid aluminium filtrate.The low iron crystalline sulfuric acid aluminium filtrate that finally obtains through 85 ℃ of oven dry, is obtained high-purity industrial aluminum sulphate, at 600 ℃ of calcining 3h, obtain industrial active A l then
2O
3, analyze Fe wherein
2O
3Content is 0.16%, meets the technical requirements of HG/T3927-2007 " industrial activated alumina " fully.The SO of calcination process discharging
3Gas, the filtrate of containing the finite concentration dilute sulphuric acid with the residue that reclaims Aluminum Sulfate Solution absorbs, and the preparation vitriol oil turns back to sulfuric acid lixiviate aluminium operation, realizes the vitriolic recycling.With the residue mother liquor in the secondary solid-liquid separation process, turn back to Tai-Ace S 150 recrystallization operation.When Recycling Mother Solution surpasses 3 times, when foreign matter content is higher, concentrate through 100 ℃, precipitation is separated out in cooling, and throw out after 100 ℃ of oven dry, is obtained the Aluminum Sulfate Solution crystal.
Embodiment 2: with the flyash that embodiment 1 uses, ball milling 2h in ball mill carries out mechanical activation; Mass ratio according to flyash and water is that 1:3 adds water, fully stirs, and removes through flotation and does not fire clean deceiving; Remove ferric oxide through magnetic separation again; To be made into sulfuric acid concentration through the flyash raffinate after the flotation carbon, magnetic separation iron and the vitriol oil is 50% mixing solutions, the solid-to-liquid ratio of control flyash and mixing solutions is 1:7, carry out heating and pressurizing reaction 4h in acid tolerance response equipment, the top temperature of reaction is 240 ℃, and pressure is 0.1MPa; After the reaction cooling, be that 1:15 adds water according to the mass ratio of flyash and water, after the heated and boiled, suction filtration obtains filter cake, and is the water washing of 1:1 with the mass ratio of flyash and water, obtains the thick liquid of Tai-Ace S 150.The extraction yield of analyzing aluminium is 75%.
110 ℃ of evaporation concentration, after the cooling, the crystal weight that control is separated out accounts for 65% of the former weight of Tai-Ace S 150 liquid, obtains the Tai-Ace S 150 concentrated solution with the thick liquid of Tai-Ace S 150; The Tai-Ace S 150 concentrated solution is heated to 60 ℃, and insulation 5h, then solution is cooled off recrystallization, make most of Tai-Ace S 150 crystallization separate out, adopt decantation that precipitation is separated with top clear liquid again, thereby obtain refining crystallization Tai-Ace S 150 slurries.With aforesaid recrystallization operation repetitive operation 5 times, to remove iron contamination to greatest extent; Gained refining crystallization Tai-Ace S 150 slurries are carried out solid-liquid separation, can use centrifugation or vacuum belt filter, obtain low iron crystalline sulfuric acid aluminium filtrate.The low iron crystalline sulfuric acid aluminium filtrate that finally obtains through 85 ℃ of oven dry, is obtained high-purity industrial aluminum sulphate, at 850 ℃ of calcining 2h, obtain industrial active A l then
2O
3, analyze Fe wherein
2O
3Content is 0.17%, meets the technical requirements of HG/T3927-2007 " industrial activated alumina " fully.
With the residue mother liquor in the secondary solid-liquid separation process, turn back to Tai-Ace S 150 recrystallization operation.When Recycling Mother Solution surpasses 5 times, when foreign matter content is higher, concentrate through 90 ℃, precipitation is separated out in cooling, and throw out after 80 ℃ of oven dry, is obtained the Aluminum Sulfate Solution crystal.SO
3Recycling in byproduct is identical with embodiment 1.
Embodiment 3: with the flyash among the embodiment 1, ball milling 3h in ball mill carries out mechanical activation; Mass ratio according to flyash and water is that 1:2 adds water, fully stirs, and removes through flotation and does not fire clean deceiving; Remove ferric oxide through magnetic separation again; To be made into sulfuric acid concentration through the flyash raffinate after the flotation carbon, magnetic separation iron and the vitriol oil is 80% mixing solutions, the solid-to-liquid ratio of control flyash and mixing solutions is 1:6, carry out heating and pressurizing reaction 5h in acid tolerance response equipment, the top temperature of reaction is 240 ℃, and pressure is 0.2MPa; After the reaction cooling, be that 1:10 adds water according to the mass ratio of flyash and water, after the heated and boiled, suction filtration obtains filter cake, and is the water washing of 1:2 with the mass ratio of flyash and water, obtains the thick liquid of Tai-Ace S 150.The extraction yield of analyzing aluminium is 72%.
100 ℃ of evaporation concentration, after the cooling, the crystal weight that control is separated out accounts for 45% of the former weight of Tai-Ace S 150 liquid, obtains the Tai-Ace S 150 concentrated solution with the thick liquid of Tai-Ace S 150; The Tai-Ace S 150 concentrated solution is heated to 55 ℃, and insulation 4h, then solution is cooled off recrystallization, make most of Tai-Ace S 150 crystallization separate out, adopt decantation that precipitation is separated with top clear liquid again, thereby obtain refining crystallization Tai-Ace S 150 slurries.With aforesaid recrystallization operation repetitive operation 4 times, to remove iron contamination to greatest extent; Gained refining crystallization Tai-Ace S 150 slurries are carried out solid-liquid separation, can use centrifugation or vacuum belt filter, obtain low iron crystalline sulfuric acid aluminium filtrate.The low iron crystalline sulfuric acid aluminium filtrate that finally obtains through 100 ℃ of oven dry, is obtained high-purity industrial aluminum sulphate, at 700 ℃ of calcining 3h, obtain industrial active A l then
2O
3, analyze Fe wherein
2O
3Content is 0.21%, meets the technical requirements of HG/T3927-2007 " industrial activated alumina " fully.
With the residue mother liquor in the secondary solid-liquid separation process, turn back to Tai-Ace S 150 recrystallization operation.When Recycling Mother Solution surpasses 5 times, when foreign matter content is higher, concentrate through 80 ℃, precipitation is separated out in cooling, and throw out after 90 ℃ of oven dry, is obtained the Aluminum Sulfate Solution crystal.SO
3Recycling in byproduct is identical with embodiment 1.
Embodiment 4: with the flyash among the embodiment 1, ball milling 4h in ball mill carries out mechanical activation; Mass ratio according to flyash and water is that 1:2 adds water, fully stirs, and removes through flotation and does not fire clean deceiving; Remove ferric oxide through magnetic separation again; To be made into sulfuric acid concentration through the flyash raffinate after the flotation carbon, magnetic separation iron and the vitriol oil is 95% mixing solutions, the solid-to-liquid ratio (mass ratio) of control flyash and mixing solutions is 1:4, in acid tolerance response equipment, carry out heating and pressurizing reaction 5h, the top temperature of reaction is 240 ℃, and pressure is 0.5MPa; After the reaction cooling, be that 1:20 adds water according to the mass ratio of flyash and water, after the heated and boiled, suction filtration obtains filter cake, and is the water washing of 1:1 with the mass ratio of flyash and water, obtains the thick liquid of Tai-Ace S 150.The extraction yield of analyzing aluminium is 80%.
110 ℃ of evaporation concentration, after the cooling, the crystal weight that control is separated out accounts for 50% of the former weight of Tai-Ace S 150 liquid, obtains the Tai-Ace S 150 concentrated solution with the thick liquid of Tai-Ace S 150; The Tai-Ace S 150 concentrated solution is heated to 50 ℃, and insulation 4h, then solution is cooled off recrystallization, make most of Tai-Ace S 150 crystallization separate out, adopt decantation that precipitation is separated with top clear liquid again, thereby obtain refining crystallization Tai-Ace S 150 slurries.With aforesaid recrystallization operation repetitive operation 4 times, to remove iron contamination to greatest extent; Gained refining crystallization Tai-Ace S 150 slurries are carried out solid-liquid separation, can use centrifugation or vacuum belt filter, obtain low iron crystalline sulfuric acid aluminium filtrate.The low iron crystalline sulfuric acid aluminium filtrate that finally obtains through 90 ℃ of oven dry, is obtained high-purity industrial aluminum sulphate, at 750 ℃ of calcining 3h, obtain industrial active A l then
2O
3, analyze Fe wherein
2O
3Content is 0.24%, meets the technical requirements of HG/T3927-2007 " industrial activated alumina " fully.
With the residue mother liquor in the secondary solid-liquid separation process, turn back to Tai-Ace S 150 recrystallization operation.When Recycling Mother Solution surpasses 5 times, when foreign matter content is higher, concentrate through 85 ℃, precipitation is separated out in cooling, and throw out after 100 ℃ of oven dry, is obtained the Aluminum Sulfate Solution crystal.SO
3Recycling in byproduct is identical with embodiment 1.
Embodiment 5: the raw material powder coal ash consist of Fe
2O
3Content is 3.66%, Al
2O
3Content is 40.88%, and CaO content is 2.96%, and MgO content is 0.36%, SiO
2Content is 42.7 %, loss on ignition 5.46%.
With above-mentioned flyash ball milling 5h in ball mill, carry out mechanical activation; Mass ratio according to flyash and water is that 1:1 adds water, fully stirs, and removes through flotation and does not fire clean deceiving; Remove ferric oxide through magnetic separation again; To be made into sulfuric acid concentration through the flyash raffinate after the flotation carbon, magnetic separation iron and the vitriol oil is 30% mixing solutions, the solid-to-liquid ratio of control flyash and mixing solutions is 1:10, in acid tolerance response equipment, carry out heating and pressurizing reaction 1.5h, the top temperature of reaction is 200 ℃, pressure 0.3MPa; After the reaction cooling, be that 1:20 adds water according to the mass ratio of flyash and water, after the heated and boiled, suction filtration obtains filter cake, and is the water washing of 1:1 with the mass ratio of flyash and water, obtains the thick liquid of Tai-Ace S 150.The extraction yield of analyzing aluminium is 75%.
100 ℃ of evaporation concentration, after the cooling, the crystal weight that control is separated out accounts for 55% of the former weight of Tai-Ace S 150 liquid, obtains the Tai-Ace S 150 concentrated solution with the thick liquid of Tai-Ace S 150; The Tai-Ace S 150 concentrated solution is heated to 53 ℃, and insulation 5h, then solution is cooled off recrystallization, make most of Tai-Ace S 150 crystallization separate out, adopt decantation that precipitation is separated with top clear liquid again, thereby obtain refining crystallization Tai-Ace S 150 slurries.With aforesaid recrystallization operation repetitive operation 4 times, to remove iron contamination to greatest extent; Gained refining crystallization Tai-Ace S 150 slurries are carried out solid-liquid separation, can use centrifugation or vacuum belt filter, obtain low iron crystalline sulfuric acid aluminium filtrate.The low iron crystalline sulfuric acid aluminium filtrate that finally obtains through 88 ℃ of oven dry, is obtained high-purity industrial aluminum sulphate, at 800 ℃ of calcining 3h, obtain industrial active A l then
2O
3, analyze Fe wherein
2O
3Content is 0.21%, meets the technical requirements of HG/T3927-2007 " industrial activated alumina " fully.
With the residue mother liquor in the secondary solid-liquid separation process, turn back to Tai-Ace S 150 recrystallization operation.When Recycling Mother Solution surpasses 4 times, when foreign matter content is higher, concentrate through 100 ℃, precipitation is separated out in cooling, and throw out after 80 ℃ of ℃ of oven dry, is obtained the Aluminum Sulfate Solution crystal.SO
3Recycling in byproduct is identical with embodiment 1.
Embodiment 6: with the flyash among the embodiment 5, ball milling 2h in ball mill carries out mechanical activation; Mass ratio according to flyash and water is that 1:1 adds water, fully stirs, and removes through flotation and does not fire clean deceiving; Remove ferric oxide through magnetic separation again; To be made into sulfuric acid concentration through the flyash raffinate after the flotation carbon, magnetic separation iron and the vitriol oil is 60% mixing solutions, the solid-to-liquid ratio of control flyash and mixing solutions is 1:5, in acid tolerance response equipment, carry out heating and pressurizing reaction 1.4h, the top temperature of reaction is 240 ℃, and pressure is 0.4MPa; After the reaction cooling, be that 1:20 adds water according to the mass ratio of flyash and water, after the heated and boiled, suction filtration obtains filter cake, and is the water washing of 1:1 with the mass ratio of flyash and water, obtains the thick liquid of Tai-Ace S 150.The extraction yield of analyzing aluminium is 70%.
110 ℃ of evaporation concentration, after the cooling, the crystal weight that control is separated out accounts for 60% of the former weight of Tai-Ace S 150 liquid, obtains the Tai-Ace S 150 concentrated solution with the thick liquid of Tai-Ace S 150; The Tai-Ace S 150 concentrated solution is heated to 57 ℃, and insulation 5h, then solution is cooled off recrystallization, make most of Tai-Ace S 150 crystallization separate out, adopt decantation that precipitation is separated with top clear liquid again, thereby obtain refining crystallization Tai-Ace S 150 slurries.With aforesaid recrystallization operation repetitive operation 4 times, to remove iron contamination to greatest extent; Gained refining crystallization Tai-Ace S 150 slurries are carried out solid-liquid separation, can use centrifugation or vacuum belt filter, obtain low iron crystalline sulfuric acid aluminium filtrate.The low iron crystalline sulfuric acid aluminium filtrate that finally obtains through 100 ℃ of oven dry, is obtained high-purity industrial aluminum sulphate, at 680 ℃ of calcining 4h, obtain industrial active A l then
2O
3, analyze Fe wherein
2O
3Content is 0.15%, meets the technical requirements of HG/T3927-2007 " industrial activated alumina " fully.
With the residue mother liquor in the secondary solid-liquid separation process, turn back to Tai-Ace S 150 recrystallization operation.When Recycling Mother Solution surpasses 3 times, when foreign matter content is higher, concentrate through 95 ℃, precipitation is separated out in cooling, and throw out after 120 ℃ of oven dry, is obtained the Aluminum Sulfate Solution crystal.SO
3Recycling in byproduct is identical with embodiment 1.
Example 7: the raw material powder coal ash consist of Fe
2O
3Content is 2.72%, Al
2O
3Content is 41.67%, and CaO content is 2.39%, and MgO content is 0.43%, SiO
2Content is 46.21%, loss on ignition 3.07%.
With flyash ball milling 2h in ball mill, carry out mechanical activation; Mass ratio according to flyash and water is that 1:2 adds water, fully stirs, and removes through flotation and does not fire clean deceiving; Remove ferric oxide through magnetic separation again; To be made into sulfuric acid concentration through the flyash raffinate after the flotation carbon, magnetic separation iron and the vitriol oil is 70% mixing solutions, the solid-to-liquid ratio of control flyash and mixing solutions is 1:4, carry out heating and pressurizing reaction 3h in acid tolerance response equipment, the top temperature of reaction is 220 ℃, and pressure is 0.4MPa; After the reaction cooling, be that 1:15 adds water according to the mass ratio of flyash and water, after the heated and boiled, suction filtration obtains filter cake, and is the water washing of 1:2 with the mass ratio of flyash and water, obtains the thick liquid of Tai-Ace S 150.The extraction yield of analyzing aluminium is 75%.
100 ℃ of evaporation concentration, after the cooling, the crystal weight that control is separated out accounts for 47% of the former weight of Tai-Ace S 150 liquid, obtains the Tai-Ace S 150 concentrated solution with the thick liquid of Tai-Ace S 150; The Tai-Ace S 150 concentrated solution is heated to 52 ℃, and insulation 4.5h, then solution is cooled off recrystallization, make most of Tai-Ace S 150 crystallization separate out, adopt decantation that precipitation is separated with top clear liquid again, thereby obtain refining crystallization Tai-Ace S 150 slurries.With aforesaid recrystallization operation repetitive operation 5 times, to remove iron contamination to greatest extent; Gained refining crystallization Tai-Ace S 150 slurries are carried out solid-liquid separation, can use centrifugation or vacuum belt filter, obtain low iron crystalline sulfuric acid aluminium filtrate.The low iron crystalline sulfuric acid aluminium filtrate that finally obtains through 90 ℃ of oven dry, is obtained high-purity industrial aluminum sulphate, at 740 ℃ of calcining 3h, obtain industrial active A l then
2O
3, analyze Fe wherein
2O
3Content is 0.26%, meets the technical requirements of HG/T3927-2007 " industrial activated alumina " fully.
With the residue mother liquor in the secondary solid-liquid separation process, turn back to Tai-Ace S 150 recrystallization operation.When Recycling Mother Solution surpasses 4 times, when foreign matter content is higher, concentrate through 89 ℃, precipitation is separated out in cooling, and throw out after 105 ℃ of oven dry, is obtained the Aluminum Sulfate Solution crystal.SO
3Recycling in byproduct is identical with embodiment 1.
Example 8: with the flyash among the embodiment 7, ball milling 6h in ball mill carries out mechanical activation; Mass ratio according to flyash and water is that 1:1 adds water, fully stirs, and removes through flotation and does not fire clean deceiving; Remove ferric oxide through magnetic separation again; To be made into sulfuric acid concentration through the flyash raffinate after the flotation carbon, magnetic separation iron and the vitriol oil is 90% mixing solutions, the solid-to-liquid ratio of control flyash and mixing solutions is 1:3, carry out heating and pressurizing reaction 2h in acid tolerance response equipment, the top temperature of reaction is 240 ℃, and pressure is 0.1MPa; After the reaction cooling, be that 1:20 adds water according to the mass ratio of flyash and water, after the heated and boiled, suction filtration obtains filter cake, and is the water washing of 1:2 with the mass ratio of flyash and water, obtains the thick liquid of Tai-Ace S 150.The extraction yield of analyzing aluminium is 80%.
100 ℃ of evaporation concentration, after the cooling, the crystal weight that control is separated out accounts for 53% of the former weight of Tai-Ace S 150 liquid, obtains the Tai-Ace S 150 concentrated solution with the thick liquid of Tai-Ace S 150; The Tai-Ace S 150 concentrated solution is heated to 56 ℃, and insulation 5h, then solution is cooled off recrystallization, make most of Tai-Ace S 150 crystallization separate out, adopt decantation that precipitation is separated with top clear liquid again, thereby obtain refining crystallization Tai-Ace S 150 slurries.With aforesaid recrystallization operation repetitive operation 5 times, to remove iron contamination to greatest extent; Gained refining crystallization Tai-Ace S 150 slurries are carried out solid-liquid separation, can use centrifugation or vacuum belt filter, obtain low iron crystalline sulfuric acid aluminium filtrate.The low iron crystalline sulfuric acid aluminium filtrate that finally obtains through 90 ℃ of oven dry, is obtained high-purity industrial aluminum sulphate, at 660 ℃ of calcining 4h, obtain industrial active A l then
2O
3, analyze Fe wherein
2O
3Content is 0.14%, meets the technical requirements of HG/T3927-2007 " industrial activated alumina " fully.
With the residue mother liquor in the secondary solid-liquid separation process, turn back to Tai-Ace S 150 recrystallization operation.When Recycling Mother Solution surpasses 4 times, when foreign matter content is higher, concentrate through 90 ℃, precipitation is separated out in cooling, and throw out after 90 ℃ of oven dry, is obtained the Aluminum Sulfate Solution crystal.SO
3Recycling in byproduct is identical with embodiment 1.
Example 9: the raw material powder coal ash consist of Fe
2O
3Content is 4.39%, Al
2O
3Content is 28.7%, and CaO content is 5.38%, and MgO content is 1.28%, SiO
2Content is 52.51%, loss on ignition 4.29%.
With flyash ball milling 3h in ball mill, carry out mechanical activation; Mass ratio according to flyash and water is that 1:1 adds water, fully stirs, and removes through flotation and does not fire clean deceiving; Remove ferric oxide through magnetic separation again; To be made into sulfuric acid concentration through the flyash raffinate after the flotation carbon, magnetic separation iron and the vitriol oil is 50% mixing solutions, the solid-to-liquid ratio of control flyash and mixing solutions is 1:6, carry out heating and pressurizing reaction 2h in acid tolerance response equipment, the top temperature of reaction is 240 ℃, and pressure is 0.3MPa; After the reaction cooling, be that 1:20 adds water according to the mass ratio of flyash and water, after the heated and boiled, suction filtration obtains filter cake, and is the water washing of 1:1 with the mass ratio of flyash and water, obtains the thick liquid of Tai-Ace S 150.The extraction yield of analyzing aluminium is 72%.
100 ℃ of evaporation concentration, after the cooling, the crystal weight that control is separated out accounts for 61% of the former weight of Tai-Ace S 150 liquid, obtains the Tai-Ace S 150 concentrated solution with the thick liquid of Tai-Ace S 150; The Tai-Ace S 150 concentrated solution is heated to 60 ℃, and insulation 4h, then solution is cooled off recrystallization, make most of Tai-Ace S 150 crystallization separate out, adopt decantation that precipitation is separated with top clear liquid again, thereby obtain refining crystallization Tai-Ace S 150 slurries.With aforesaid recrystallization operation repetitive operation 5 times, to remove iron contamination to greatest extent; Gained refining crystallization Tai-Ace S 150 slurries are carried out solid-liquid separation, can use centrifugation or vacuum belt filter, obtain low iron crystalline sulfuric acid aluminium filtrate.The low iron crystalline sulfuric acid aluminium filtrate that finally obtains through 95 ℃ of oven dry, is obtained high-purity industrial aluminum sulphate, at 740 ℃ of calcining 3h, obtain industrial active A l then
2O
3, analyze Fe wherein
2O
3Content is 0.32%, meets the technical requirements of HG/T3927-2007 " industrial activated alumina " fully.
With the residue mother liquor in the secondary solid-liquid separation process, turn back to Tai-Ace S 150 recrystallization operation.When Recycling Mother Solution surpasses 5 times, when foreign matter content is higher, concentrate through 83 ℃, precipitation is separated out in cooling, and throw out after 110 ℃ of oven dry, is obtained the Aluminum Sulfate Solution crystal.SO
3Recycling in byproduct is identical with embodiment 1.
Example 10: with the flyash among the embodiment 9, ball milling 3h in ball mill carries out mechanical activation; Mass ratio according to flyash and water is that 1:2 adds water, fully stirs, and removes through flotation and does not fire clean deceiving; Remove ferric oxide through magnetic separation again; To be made into sulfuric acid concentration through the flyash raffinate after the flotation carbon, magnetic separation iron and the vitriol oil is 70% mixing solutions, the solid-to-liquid ratio of control flyash and mixing solutions is 1:5, carry out heating and pressurizing reaction 2h in acid tolerance response equipment, the top temperature of reaction is 240 ℃, and pressure is 0.2MPa; After the reaction cooling, be that 1:10 adds water according to the mass ratio of flyash and water, after the heated and boiled, suction filtration obtains filter cake, and is the water washing of 1:2 with the mass ratio of flyash and water, obtains the thick liquid of Tai-Ace S 150.The extraction yield of analyzing aluminium is 70%.
110 ℃ of evaporation concentration, after the cooling, the crystal weight that control is separated out accounts for 54% of the former weight of Tai-Ace S 150 liquid, obtains the Tai-Ace S 150 concentrated solution with the thick liquid of Tai-Ace S 150; The Tai-Ace S 150 concentrated solution is heated to 50 ℃, and insulation 4h, then solution is cooled off recrystallization, make most of Tai-Ace S 150 crystallization separate out, adopt decantation that precipitation is separated with top clear liquid again, thereby obtain refining crystallization Tai-Ace S 150 slurries.With aforesaid recrystallization operation repetitive operation 3 times, to remove iron contamination to greatest extent; Gained refining crystallization Tai-Ace S 150 slurries are carried out solid-liquid separation, can use centrifugation or vacuum belt filter, obtain low iron crystalline sulfuric acid aluminium filtrate.The low iron crystalline sulfuric acid aluminium filtrate that finally obtains through 100 ℃ of oven dry, is obtained high-purity industrial aluminum sulphate, at 840 ℃ of calcining 2h, obtain industrial active A l then
2O
3, analyze Fe wherein
2O
3Content is 0.22%, meets the technical requirements of HG/T3927-2007 " industrial activated alumina " fully.
With the residue mother liquor in the secondary solid-liquid separation process, turn back to Tai-Ace S 150 recrystallization operation.When Recycling Mother Solution surpasses 5 times, when foreign matter content is higher, concentrate through 100 ℃, precipitation is separated out in cooling, and throw out after 90 ℃ of oven dry, is obtained the Aluminum Sulfate Solution crystal.SO
3Recycling in byproduct is identical with embodiment 1.
Embodiment 11: with the flyash among the embodiment 1, ball milling 4h in ball mill carries out mechanical activation; Mass ratio according to flyash and water is that 1:2 adds water, fully stirs, and removes through flotation and does not fire clean deceiving; Remove ferric oxide through magnetic separation again; To be made into sulfuric acid concentration through the flyash raffinate after the flotation carbon, magnetic separation iron and the vitriol oil is 70% mixing solutions, the solid-to-liquid ratio of control flyash and mixing solutions is 1:6, carry out heating and pressurizing reaction 3h in acid tolerance response equipment, the top temperature of reaction is 220 ℃, and pressure is 0.3MPa; After the reaction cooling, be that 1:20 adds water according to the mass ratio of flyash and water, after the heated and boiled, suction filtration obtains filter cake, and is the water washing of 1:1 with the mass ratio of flyash and water, obtains the thick liquid of Tai-Ace S 150.The extraction yield of analyzing aluminium is 78%.
120 ℃ of evaporation concentration, after the cooling, the crystal weight that control is separated out accounts for 62% of the former weight of Tai-Ace S 150 liquid, obtains the Tai-Ace S 150 concentrated solution with the thick liquid of Tai-Ace S 150; The Tai-Ace S 150 concentrated solution is heated to 60 ℃, and insulation 5h, then solution is cooled off recrystallization, make most of Tai-Ace S 150 crystallization separate out, adopt decantation that precipitation is separated with top clear liquid again, thereby obtain refining crystallization Tai-Ace S 150 slurries.With aforesaid recrystallization operation repetitive operation 5 times, to remove iron contamination to greatest extent; Gained refining crystallization Tai-Ace S 150 slurries are carried out solid-liquid separation, can use centrifugation or vacuum belt filter, obtain low iron crystalline sulfuric acid aluminium filtrate.The low iron crystalline sulfuric acid aluminium filtrate that finally obtains through 95 ℃ of oven dry, is obtained high-purity industrial aluminum sulphate, at 720 ℃ of calcining 3h, obtain industrial active A l then
2O
3, analyze Fe wherein
2O
3Content is 0.26%, meets the technical requirements of HG/T3927-2007 " industrial activated alumina " fully.
With the residue mother liquor in the secondary solid-liquid separation process, turn back to Tai-Ace S 150 recrystallization operation.When Recycling Mother Solution surpasses 5 times, when foreign matter content is higher, concentrate through 110 ℃, precipitation is separated out in cooling, and throw out after 80 ℃ of oven dry, is obtained the Aluminum Sulfate Solution crystal.SO
3Recycling in byproduct is identical with embodiment 1.
Embodiment 12: with the flyash among the embodiment 1, ball milling 3h in ball mill carries out mechanical activation; Mass ratio according to flyash and water is that 1:2 adds water, fully stirs, and removes through flotation and does not fire clean deceiving; Remove ferric oxide through magnetic separation again; To be made into sulfuric acid concentration through the flyash raffinate after the flotation carbon, magnetic separation iron and the vitriol oil is 80% mixing solutions, the solid-to-liquid ratio of control flyash and mixing solutions is 1:6, carry out heating and pressurizing reaction 5h in acid tolerance response equipment, the top temperature of reaction is 240 ℃, and pressure is 0.2MPa; After the reaction cooling, be that 1:10 adds water according to the mass ratio of flyash and water, after the heated and boiled, suction filtration obtains filter cake, and is the water washing of 1:2 with the mass ratio of flyash and water, obtains the thick liquid of Tai-Ace S 150.The extraction yield of analyzing aluminium is 82%.
100 ℃ of evaporation concentration, after the cooling, the crystal weight that control is separated out accounts for 49% of the former weight of Tai-Ace S 150 liquid, obtains the Tai-Ace S 150 concentrated solution with the thick liquid of Tai-Ace S 150; The Tai-Ace S 150 concentrated solution is heated to 57 ℃, and insulation 4h, then solution is cooled off recrystallization, make most of Tai-Ace S 150 crystallization separate out, adopt decantation that precipitation is separated with top clear liquid again, thereby obtain refining crystallization Tai-Ace S 150 slurries.With aforesaid recrystallization operation repetitive operation 4 times, to remove iron contamination to greatest extent; Gained refining crystallization Tai-Ace S 150 slurries are carried out solid-liquid separation, can use centrifugation or vacuum belt filter, obtain low iron crystalline sulfuric acid aluminium filtrate.The low iron crystalline sulfuric acid aluminium filtrate that finally obtains through 100 ℃ of oven dry, is obtained high-purity industrial aluminum sulphate, at 630 ℃ of calcining 4h, obtain industrial active A l then
2O
3, analyze Fe wherein
2O
3Content is 0.21%, meets the technical requirements of HG/T3927-2007 " industrial activated alumina " fully.
With the residue mother liquor in the secondary solid-liquid separation process, turn back to Tai-Ace S 150 recrystallization operation.When Recycling Mother Solution surpasses 4 times, when foreign matter content is higher, concentrate through 86 ℃, precipitation is separated out in cooling, and throw out after 90 ℃ of oven dry, is obtained the Aluminum Sulfate Solution crystal.SO
3Recycling in byproduct is identical with embodiment 1.
Embodiment 13: with the flyash among the embodiment 5, ball milling 2h in ball mill carries out mechanical activation; Mass ratio according to flyash and water is that 1:1 adds water, fully stirs, and removes through flotation and does not fire clean deceiving; Remove ferric oxide through magnetic separation again; To be made into sulfuric acid concentration through the flyash raffinate after the flotation carbon, magnetic separation iron and the vitriol oil is 60% mixing solutions, the solid-to-liquid ratio of control flyash and mixing solutions is 1:5, in acid tolerance response equipment, carry out heating and pressurizing reaction 1.4h, the top temperature of reaction is 240 ℃, and pressure is 0.1MPa; After the reaction cooling, be that 1:20 adds water according to the mass ratio of flyash and water, after the heated and boiled, suction filtration obtains filter cake, and is the water washing of 1:1 with the mass ratio of flyash and water, obtains the thick liquid of Tai-Ace S 150.The extraction yield of analyzing aluminium is 85%.
110 ℃ of evaporation concentration, after the cooling, the crystal weight that control is separated out accounts for 52% of the former weight of Tai-Ace S 150 liquid, obtains the Tai-Ace S 150 concentrated solution with the thick liquid of Tai-Ace S 150; The Tai-Ace S 150 concentrated solution is heated to 60 ℃, and insulation 5h, then solution is cooled off recrystallization, make most of Tai-Ace S 150 crystallization separate out, adopt decantation that precipitation is separated with top clear liquid again, thereby obtain refining crystallization Tai-Ace S 150 slurries.With aforesaid recrystallization operation repetitive operation 5 times, to remove iron contamination to greatest extent; Gained refining crystallization Tai-Ace S 150 slurries are carried out solid-liquid separation, can use centrifugation or vacuum belt filter, obtain low iron crystalline sulfuric acid aluminium filtrate.The low iron crystalline sulfuric acid aluminium filtrate that finally obtains through 100 ℃ of oven dry, is obtained high-purity industrial aluminum sulphate, at 825 ℃ of calcining 2h, obtain industrial active A l then
2O
3, analyze Fe wherein
2O
3Content is 0.34%, meets the technical requirements of HG/T3927-2007 " industrial activated alumina " fully.
With the residue mother liquor in the secondary solid-liquid separation process, turn back to Tai-Ace S 150 recrystallization operation.When Recycling Mother Solution surpasses 4 times, when foreign matter content is higher, concentrate through 95 ℃, precipitation is separated out in cooling, and throw out after 100 ℃ of oven dry, is obtained the Aluminum Sulfate Solution crystal.SO
3Recycling in byproduct is identical with embodiment 1.
Example 14: with the flyash among the embodiment 7, ball milling 6h in ball mill carries out mechanical activation; Mass ratio according to flyash and water is that 1:1 adds water, fully stirs, and removes through flotation and does not fire clean deceiving; Remove ferric oxide through magnetic separation again; To be made into sulfuric acid concentration through the flyash raffinate after the flotation carbon, magnetic separation iron and the vitriol oil is 90% mixing solutions, the solid-to-liquid ratio of control flyash and mixing solutions is 1:3, carry out heating and pressurizing reaction 2h in acid tolerance response equipment, the top temperature of reaction is 240 ℃, and pressure is 0.3MPa; After the reaction cooling, be that 1:20 adds water according to the mass ratio of flyash and water, after the heated and boiled, suction filtration obtains filter cake, and is the water washing of 1:2 with the mass ratio of flyash and water, obtains the thick liquid of Tai-Ace S 150.The extraction yield of analyzing aluminium is 82%.
100 ℃ of evaporation concentration, after the cooling, the crystal weight that control is separated out accounts for 48% of the former weight of Tai-Ace S 150 liquid, obtains the Tai-Ace S 150 concentrated solution with the thick liquid of Tai-Ace S 150; The Tai-Ace S 150 concentrated solution is heated to 54 ℃, and insulation 4h, then solution is cooled off recrystallization, make most of Tai-Ace S 150 crystallization separate out, adopt decantation that precipitation is separated with top clear liquid again, thereby obtain refining crystallization Tai-Ace S 150 slurries.With aforesaid recrystallization operation repetitive operation 4 times, to remove iron contamination to greatest extent; Gained refining crystallization Tai-Ace S 150 slurries are carried out solid-liquid separation, can use centrifugation or vacuum belt filter, obtain low iron crystalline sulfuric acid aluminium filtrate.The low iron crystalline sulfuric acid aluminium filtrate that finally obtains through 90 ℃ of oven dry, is obtained high-purity industrial aluminum sulphate, at 675 ℃ of calcining 3.5h, obtain industrial active A l then
2O
3, analyze Fe wherein
2O
3Content is 0.28%, meets the technical requirements of HG/T3927-2007 " industrial activated alumina " fully.
With the residue mother liquor in the secondary solid-liquid separation process, turn back to Tai-Ace S 150 recrystallization operation.When Recycling Mother Solution surpasses 4 times, when foreign matter content is higher, concentrate through 105 ℃, precipitation is separated out in cooling, and throw out after 90 ℃ of oven dry, is obtained the Aluminum Sulfate Solution crystal.SO
3Recycling in byproduct is identical with embodiment 1.
Example 15: with the flyash among the embodiment 9, ball milling 2h in ball mill carries out mechanical activation; Mass ratio according to flyash and water is that 1:2 adds water, fully stirs, and removes through flotation and does not fire clean deceiving; Remove ferric oxide through magnetic separation again; To be made into sulfuric acid concentration through the flyash raffinate after the flotation carbon, magnetic separation iron and the vitriol oil is 70% mixing solutions, the solid-to-liquid ratio of control flyash and mixing solutions is 1:5, carry out heating and pressurizing reaction 2h in acid tolerance response equipment, the top temperature of reaction is 220 ℃, and pressure is 0.5MPa; After the reaction cooling, be that 1:10 adds water according to the mass ratio of flyash and water, after the heated and boiled, suction filtration obtains filter cake, and is the water washing of 1:1 with the mass ratio of flyash and water, obtains the thick liquid of Tai-Ace S 150.The extraction yield of analyzing aluminium is 85%.
110 ℃ of evaporation concentration, after the cooling, the crystal weight that control is separated out accounts for 49% of the former weight of Tai-Ace S 150 liquid, obtains the Tai-Ace S 150 concentrated solution with the thick liquid of Tai-Ace S 150; The Tai-Ace S 150 concentrated solution is heated to 53 ℃, and insulation 4h, then solution is cooled off recrystallization, make most of Tai-Ace S 150 crystallization separate out, adopt decantation that precipitation is separated with top clear liquid again, thereby obtain refining crystallization Tai-Ace S 150 slurries.With aforesaid recrystallization operation repetitive operation 5 times, to remove iron contamination to greatest extent; Gained refining crystallization Tai-Ace S 150 slurries are carried out solid-liquid separation, can use centrifugation or vacuum belt filter, obtain low iron crystalline sulfuric acid aluminium filtrate.The low iron crystalline sulfuric acid aluminium filtrate that finally obtains through 100 ℃ of oven dry, is obtained high-purity industrial aluminum sulphate, at 725 ℃ of calcining 2.5h, obtain industrial active A l then
2O
3, analyze Fe wherein
2O
3Content is 0.19%, meets the technical requirements of HG/T3927-2007 " industrial activated alumina " fully.
With the residue mother liquor in the secondary solid-liquid separation process, turn back to Tai-Ace S 150 recrystallization operation.When Recycling Mother Solution surpasses 5 times, when foreign matter content is higher, concentrate through 110 ℃, precipitation is separated out in cooling, and throw out after 110 ℃ of oven dry, is obtained the Aluminum Sulfate Solution crystal.SO
3Recycling in byproduct is identical with embodiment 1.
Claims (4)
1. the method for flyash manufacture activated alumina is characterized in that comprising following step:
(1) mechanical activation: with flyash process mechanical activation;
(2) flotation de-carbon: will add water through the flyash of mechanical activation, and fully stir, and remove and do not fire clean carbon black;
(3) iron removal by magnetic separation: remove ferric oxide through magnetic separation;
(4) sulfuric acid lixiviate aluminium: will add the vitriol oil through the flyash raffinate after flotation carbon, the magnetic separation iron and carry out heating and pressurizing reaction 1～6h in acid tolerance response equipment, the top temperature of reaction is 200 ℃～240 ℃, and pressure is 0.1～0.5MPa;
(5) solid-liquid separation: after the reaction cooling, reaction solution adds water, and after the heated and boiled, suction filtration obtains the thick liquid of Tai-Ace S 150;
(6) the thick liquid of Tai-Ace S 150 concentrates: the thick liquid evaporation concentration of Tai-Ace S 150, and cooling obtains the Tai-Ace S 150 concentrated solution;
(7) Tai-Ace S 150 recrystallization: the heating of Tai-Ace S 150 concentrated solution is cooled off recrystallization with solution then, and precipitation separation and clear liquid obtain refining crystallization Tai-Ace S 150 slurries;
(8) secondary solid-liquid separation: gained refining crystallization Tai-Ace S 150 slurries are carried out solid-liquid separation, obtain low iron crystalline sulfuric acid aluminium filtrate;
(9) Tai-Ace S 150 dewatered drying: finally obtain low iron crystalline sulfuric acid aluminium filtrate oven dry, obtain Fe content and be lower than high-purity technical grade Tai-Ace S 150 of 0.02%;
(10) Tai-Ace S 150 high-temperature calcination: resulting high-purity industrial aluminum sulphate obtains Fe through the excess temperature calcining
2O
3Content is lower than 0.5% industrial active A l
2O
3
2. the method for flyash manufacture activated alumina according to claim 1, the mechanical activation that it is characterized in that step (1) are that to adopt milling equipment to carry out levigate, and the grinding time is 0.5～6h;
In the step (2), be that 1:1～1:3 adds water according to the mass ratio of flyash and water;
In the step (4), the mass concentration scope of flyash sulfuric acid mixed solution is 30%～95%, and the solid-to-liquid ratio of flyash and sulphuric acid soln is 1:1～1:15 mass ratio;
In the step (5), after the reaction cooling, the mass ratio according to flyash and water in flyash is that 1:10～1:20 adds water;
In the step (6), the thick liquid of Tai-Ace S 150 is 90 ℃～130 ℃ evaporation concentration, and the crystal weight that control is separated out accounts for 40%～65% of the former weight of Tai-Ace S 150 liquid;
In the step (7), the Heating temperature of Tai-Ace S 150 concentrated solution is 40 ℃～70 ℃, and soaking time is 1～6h, recrystallization operation repetitive operation 2～6 times;
In the step (8), use centrifugation or vacuum belt filter;
In the step (9), the bake out temperature of low iron Tai-Ace S 150 filtrate is 70～100 ℃;
In the step (10), the calcining temperature of high-purity industrial aluminum sulphate is at 500 ℃～900 ℃, and calcination time is 1～5h.
3. the method for flyash manufacture activated alumina according to claim 1 is characterized in that the grinding time of step (1) mechanical activation is 1～3h;
In the step (4), the concentration range of flyash sulfuric acid mixed solution is 40%～70%, and the solid-to-liquid ratio of flyash and sulphuric acid soln is 1:5～1:10, and the heating and pressurizing reaction times is 3～4h;
In the step (5), after the reaction cooling, the mass ratio according to flyash and water in flyash is that 1:12～1:18 adds water;
In the step (6), the thick liquid of Tai-Ace S 150 is 100～120 ℃ of evaporation concentration;
In the step (7), the Heating temperature of Tai-Ace S 150 concentrated solution is 50 ℃～60 ℃, and soaking time is 4～5h, recrystallization operation repetitive operation 2～6 times;
In the step (8), use centrifugation or vacuum belt filter;
In the step (9), the bake out temperature of low iron Tai-Ace S 150 filtrate is 80 ℃～90 ℃;
In the step (10), the calcining temperature of high-purity industrial aluminum sulphate is at 600 ℃～850 ℃, and calcination time is 2～4h.
4. the method for flyash manufacture activated alumina according to claim 1 is characterized in that flyash after the flotation de-carbon, adopts wet magnetic separation to remove magnetite.
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| CN102397820A (en) * | 2011-11-18 | 2012-04-04 | 中国铝业股份有限公司 | Method for utilizing bauxite dust |
| CN102557091A (en) * | 2011-12-30 | 2012-07-11 | 西安航天科技工业公司 | Method for subsequent treatment of aluminum sulfate generated in technical process of extracting alumina from fly ash |
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| CN105621489A (en) * | 2016-01-29 | 2016-06-01 | 卓达新材料科技集团有限公司 | Method for separating iron oxide in coal ash of circulating fluidized bed |
| CN105753061A (en) * | 2016-01-29 | 2016-07-13 | 卓达新材料科技集团有限公司 | Method for separating ferric oxide in coal-powder boiler fly ash |
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