CN104107676B - A kind of cinder of burned coal discarded object that utilizes prepares the method for aluminium for tobermorite sorbing material - Google Patents
A kind of cinder of burned coal discarded object that utilizes prepares the method for aluminium for tobermorite sorbing material Download PDFInfo
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- CN104107676B CN104107676B CN201410360318.0A CN201410360318A CN104107676B CN 104107676 B CN104107676 B CN 104107676B CN 201410360318 A CN201410360318 A CN 201410360318A CN 104107676 B CN104107676 B CN 104107676B
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- tobermorite
- aluminium
- lime
- cinder
- ash
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- MKTRXTLKNXLULX-UHFFFAOYSA-P pentacalcium;dioxido(oxo)silane;hydron;tetrahydrate Chemical compound [H+].[H+].O.O.O.O.[Ca+2].[Ca+2].[Ca+2].[Ca+2].[Ca+2].[O-][Si]([O-])=O.[O-][Si]([O-])=O.[O-][Si]([O-])=O.[O-][Si]([O-])=O.[O-][Si]([O-])=O.[O-][Si]([O-])=O MKTRXTLKNXLULX-UHFFFAOYSA-P 0.000 title claims abstract description 70
- 229910052782 aluminium Inorganic materials 0.000 title claims abstract description 68
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 title claims abstract description 67
- 239000004411 aluminium Substances 0.000 title claims abstract description 66
- 239000000463 material Substances 0.000 title claims abstract description 46
- 239000003245 coal Substances 0.000 title claims abstract description 38
- 239000003818 cinder Substances 0.000 title claims abstract description 37
- 238000000034 method Methods 0.000 title claims abstract description 17
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims abstract description 57
- 239000000843 powder Substances 0.000 claims abstract description 43
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 26
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims abstract description 24
- 239000000203 mixture Substances 0.000 claims abstract description 19
- 239000004744 fabric Substances 0.000 claims abstract description 17
- 235000013305 food Nutrition 0.000 claims abstract description 17
- 239000000376 reactant Substances 0.000 claims abstract description 17
- 229910001220 stainless steel Inorganic materials 0.000 claims abstract description 17
- 239000010935 stainless steel Substances 0.000 claims abstract description 17
- 238000006243 chemical reaction Methods 0.000 claims abstract description 12
- 238000001816 cooling Methods 0.000 claims abstract description 8
- 235000019353 potassium silicate Nutrition 0.000 claims abstract description 8
- 238000005096 rolling process Methods 0.000 claims abstract description 8
- NTHWMYGWWRZVTN-UHFFFAOYSA-N sodium silicate Chemical compound [Na+].[Na+].[O-][Si]([O-])=O NTHWMYGWWRZVTN-UHFFFAOYSA-N 0.000 claims abstract description 8
- 239000012798 spherical particle Substances 0.000 claims abstract description 8
- 239000007921 spray Substances 0.000 claims abstract description 8
- 238000000227 grinding Methods 0.000 claims abstract description 3
- 238000001354 calcination Methods 0.000 claims description 16
- 238000001027 hydrothermal synthesis Methods 0.000 claims description 10
- 239000007787 solid Substances 0.000 claims description 10
- 229910004298 SiO 2 Inorganic materials 0.000 claims description 9
- 238000010521 absorption reaction Methods 0.000 abstract description 9
- 230000000694 effects Effects 0.000 abstract description 2
- 239000002956 ash Substances 0.000 description 33
- 239000011575 calcium Substances 0.000 description 31
- 239000000047 product Substances 0.000 description 20
- 235000011121 sodium hydroxide Nutrition 0.000 description 16
- 239000010881 fly ash Substances 0.000 description 10
- 238000012360 testing method Methods 0.000 description 8
- 239000002351 wastewater Substances 0.000 description 8
- 239000004567 concrete Substances 0.000 description 7
- 238000002835 absorbance Methods 0.000 description 6
- 238000001179 sorption measurement Methods 0.000 description 6
- 238000003756 stirring Methods 0.000 description 6
- 238000005406 washing Methods 0.000 description 6
- 238000002441 X-ray diffraction Methods 0.000 description 5
- 238000005341 cation exchange Methods 0.000 description 5
- 239000000919 ceramic Substances 0.000 description 5
- 239000000975 dye Substances 0.000 description 5
- 238000002360 preparation method Methods 0.000 description 5
- PYWVYCXTNDRMGF-UHFFFAOYSA-N rhodamine B Chemical compound [Cl-].C=12C=CC(=[N+](CC)CC)C=C2OC2=CC(N(CC)CC)=CC=C2C=1C1=CC=CC=C1C(O)=O PYWVYCXTNDRMGF-UHFFFAOYSA-N 0.000 description 5
- 229940043267 rhodamine b Drugs 0.000 description 5
- 229910004283 SiO 4 Inorganic materials 0.000 description 4
- 230000007613 environmental effect Effects 0.000 description 4
- 150000002500 ions Chemical class 0.000 description 4
- 239000002893 slag Substances 0.000 description 4
- PNEYBMLMFCGWSK-UHFFFAOYSA-N Alumina Chemical compound [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 3
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical group [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 3
- 239000004568 cement Substances 0.000 description 3
- 238000004042 decolorization Methods 0.000 description 3
- 229910001385 heavy metal Inorganic materials 0.000 description 3
- 238000005342 ion exchange Methods 0.000 description 3
- 238000004519 manufacturing process Methods 0.000 description 3
- 239000002994 raw material Substances 0.000 description 3
- 239000000126 substance Substances 0.000 description 3
- 235000008733 Citrus aurantifolia Nutrition 0.000 description 2
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical group O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 2
- 235000011941 Tilia x europaea Nutrition 0.000 description 2
- 238000011074 autoclave method Methods 0.000 description 2
- 230000015572 biosynthetic process Effects 0.000 description 2
- 238000009835 boiling Methods 0.000 description 2
- 239000011449 brick Substances 0.000 description 2
- AXCZMVOFGPJBDE-UHFFFAOYSA-L calcium dihydroxide Chemical compound [OH-].[OH-].[Ca+2] AXCZMVOFGPJBDE-UHFFFAOYSA-L 0.000 description 2
- 239000000292 calcium oxide Substances 0.000 description 2
- ODINCKMPIJJUCX-UHFFFAOYSA-N calcium oxide Inorganic materials [Ca]=O ODINCKMPIJJUCX-UHFFFAOYSA-N 0.000 description 2
- 239000010883 coal ash Substances 0.000 description 2
- 238000002485 combustion reaction Methods 0.000 description 2
- 239000013078 crystal Substances 0.000 description 2
- 238000011161 development Methods 0.000 description 2
- 230000018109 developmental process Effects 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 238000003912 environmental pollution Methods 0.000 description 2
- 238000002474 experimental method Methods 0.000 description 2
- 239000012535 impurity Substances 0.000 description 2
- 229910052500 inorganic mineral Inorganic materials 0.000 description 2
- 238000009413 insulation Methods 0.000 description 2
- 239000004571 lime Substances 0.000 description 2
- 235000010755 mineral Nutrition 0.000 description 2
- 239000011707 mineral Substances 0.000 description 2
- 230000035484 reaction time Effects 0.000 description 2
- 230000008929 regeneration Effects 0.000 description 2
- 238000011069 regeneration method Methods 0.000 description 2
- 238000011160 research Methods 0.000 description 2
- 239000010865 sewage Substances 0.000 description 2
- 229910052710 silicon Inorganic materials 0.000 description 2
- 239000010703 silicon Substances 0.000 description 2
- 238000003786 synthesis reaction Methods 0.000 description 2
- 239000002699 waste material Substances 0.000 description 2
- OYPRJOBELJOOCE-UHFFFAOYSA-N Calcium Chemical compound [Ca] OYPRJOBELJOOCE-UHFFFAOYSA-N 0.000 description 1
- VYZAMTAEIAYCRO-UHFFFAOYSA-N Chromium Chemical compound [Cr] VYZAMTAEIAYCRO-UHFFFAOYSA-N 0.000 description 1
- 229910018557 Si O Inorganic materials 0.000 description 1
- 229910052783 alkali metal Inorganic materials 0.000 description 1
- 150000001340 alkali metals Chemical class 0.000 description 1
- 229910052784 alkaline earth metal Inorganic materials 0.000 description 1
- 150000001342 alkaline earth metals Chemical class 0.000 description 1
- 238000004458 analytical method Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000004566 building material Substances 0.000 description 1
- 229910052791 calcium Inorganic materials 0.000 description 1
- 239000000920 calcium hydroxide Substances 0.000 description 1
- 229910001861 calcium hydroxide Inorganic materials 0.000 description 1
- BRPQOXSCLDDYGP-UHFFFAOYSA-N calcium oxide Chemical compound [O-2].[Ca+2] BRPQOXSCLDDYGP-UHFFFAOYSA-N 0.000 description 1
- 230000001413 cellular effect Effects 0.000 description 1
- 229910052804 chromium Inorganic materials 0.000 description 1
- 239000011651 chromium Substances 0.000 description 1
- 238000004140 cleaning Methods 0.000 description 1
- 239000002131 composite material Substances 0.000 description 1
- 239000000470 constituent Substances 0.000 description 1
- 238000002425 crystallisation Methods 0.000 description 1
- 230000008025 crystallization Effects 0.000 description 1
- 230000008030 elimination Effects 0.000 description 1
- 238000003379 elimination reaction Methods 0.000 description 1
- 238000004134 energy conservation Methods 0.000 description 1
- 229920006335 epoxy glue Polymers 0.000 description 1
- 238000001914 filtration Methods 0.000 description 1
- 239000012530 fluid Substances 0.000 description 1
- 239000011464 hollow brick Substances 0.000 description 1
- 239000012774 insulation material Substances 0.000 description 1
- 238000005192 partition Methods 0.000 description 1
- 239000010451 perlite Substances 0.000 description 1
- 235000019362 perlite Nutrition 0.000 description 1
- 239000002957 persistent organic pollutant Substances 0.000 description 1
- 238000005554 pickling Methods 0.000 description 1
- 238000007789 sealing Methods 0.000 description 1
- 239000000377 silicon dioxide Substances 0.000 description 1
- LIVNPJMFVYWSIS-UHFFFAOYSA-N silicon monoxide Inorganic materials [Si-]#[O+] LIVNPJMFVYWSIS-UHFFFAOYSA-N 0.000 description 1
- 241000894007 species Species 0.000 description 1
- 239000006228 supernatant Substances 0.000 description 1
- 238000010189 synthetic method Methods 0.000 description 1
- 239000003403 water pollutant Substances 0.000 description 1
- 238000005303 weighing Methods 0.000 description 1
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- Processing Of Solid Wastes (AREA)
Abstract
Utilize cinder of burned coal discarded object to prepare the method for aluminium for tobermorite sorbing material, cinder of burned coal calcined in electrothermal furnace and is cooled to grinding at room temperature, obtaining lime-ash fine powder; Then by the watery hydrochloric acid acidleach of lime-ash fine powder, then filter, wash, dry, obtain predecessor lime-ash powder; By lime-ash powder, Ca (OH)
2ground and mixed, then adds NaOH wherein and ground and mixed is even, obtains mixture; Spray water glass solution on mixture, and rotary rolling forms the aluminium of spherical particle for tobermorite reactant presoma; Aluminium is inserted in the stainless steel cloth food steamer of reactor for tobermorite reactant presoma, in 170 ~ 190 DEG C of hydro-thermal water proof steam pressure reaction 16 ~ 20h; Reacted rear cooling release, then isolate product dry namely obtain aluminium for tobermorite sorbing material.Resulting materials of the present invention has good absorption and clean effect, reaches comprehensive utilization cinder of burned coal and prepares the object had compared with high added value environmentally conscious materials.
Description
Technical field
The invention belongs to ecological environment material nd field, particularly relate to a kind of cinder of burned coal discarded object that utilizes and prepare the method for aluminium for tobermorite sorbing material.
Background technology
Cinder of burned coal is the huge industrial residue of a class discharge capacity, mainly contains flyash, boiling furnace slag and fluid bed fluidized bed combustion coal ash/slag (abbreviation fluidized bed combustion coal ash/slag) etc.At present, in China's cinder of burned coal, flyash discharge capacity is maximum, and the flyash of annual discharge has reached more than 200,000,000 tons, and its accumulative heap is high-volume about 4,000,000,000 tons, take up an area 4 ~ 50,000 hectares, but utilization rate is less than 30%.Although boiling furnace slag discharge capacity in recent years has the trend reduced year by year, cinder of burned coal total release is growing on and on.Lime-ash is stacked and is not only taken a large amount of valuable land resource, and causes serious environmental pollution.A kind of conventional solid discarded object that cinder of burned coal Ye Shi steam power plant and coal-burning boiler produce is one of maximum environomental pollution source of society.The integrated treatment of industrial solid castoff is the important problem that annoying the whole world and even world industry and environmental harmony sustainable development always, therefore, find waste material regeneration very promising direction beyond doubt, higher economic worth can not only be produced, and there is great environment protection significance.Therefore, the regeneration having a higher-value to cinder of burned coal is the urgent need of current national environmental protection industry.
At present, domestic and international cinder of burned coal comprehensive Utilization Ways is summed up and mainly contains 7 kinds: 1. novel, that light thermal-insulation is energy-conservation materials for wall prepared by powder ash air-entrained concrete.2. coal powder concrete hollow brick, wherein flyash is admixture and fine aggregate, and volume is higher.3. cement, flyash expanded perlite concrete insulation blocks.4. with cement and flyash for epoxy glue ramming material prepares flyash concrete pavior brick.5. based on flyash, with cement, lime etc. for flyash brick prepared by cementitious matter.6. lytag and concrete product.7. flyash concrete light cellular partition board.As can be seen here, the utilization of the traditional cinder of burned coal mainly auxiliary material such as building concrete or repair the roads is worth less low side to utilize.
The general chemical composition range of cinder of burned coal is: SiO
2, 46 ~ 60%; Al
2o
3, 17 ~ 35%; Fe
2o
3, 2 ~ 15%; CaO, 1 ~ 10%; Other is 1 ~ 8% years old.From chemical composition range, cinder of burned coal main component is silica and aluminium oxide, also containing some calcium oxide.If these main components effectively utilized, the product that preparation added value is higher will be a kind of Land use systems having higher economy and environment and be worth.The research report of more existing this respects in recent years.
Tobermorite is also known as tobermorite (Tobermorite), and be a kind of afwillite mineral, desirable crystal-chemical formula is Ca
5si
6o
16(OH)
24H
2o.Because it has the performances such as thermal conductivity factor is little, intensity is high, high temperature resistant, mainly for the production of heat-insulation material and building materials in traditional industry.But research in recent years shows that tobermorite has better ion-exchange performance compared with conventional mineral sorbing material, to such as K
+, Na
+, Ba
2+, Cs
+, Rb
+and Sr
2+deng alkali metal, alkaline-earth metal and Cd
2+, Pb
2+, Hg
2+, Zn
2+, Co
2+and Ni
2+deng the heavy metal ion except 6 valency chromium, all there is good absorption and cation exchange capacity (CEC); To organic pollutants, also there is good adsorption capacity simultaneously.Thus, in heavy metal ion-containing waste water process and sealing nuke rubbish etc., there is higher application prospect, there is good environmental protection and be worth.
Comparatively speaking, pure tobermorite absorption and cation exchange capacity (CEC) relatively weak, to adulterate or ion exchange will greatly strengthen these performances.Aluminium is exactly that the silicon part in tobermorite is replaced a kind of aluminium doping type tobermorite obtained by aluminium for tobermorite.Because the non-equivalence of trivalent aluminium and tetravalence silicon is replaced, often introduce more constitution water, the absorption of tobermorite and cation exchange activity are greatly improved, thus enhances the ability of middle harmful ion of disposing of sewage.Therefore, find that a kind of to prepare aluminium very important for the method for tobermorite sorbing material.Although prepare aluminium existing numerous for the method for tobermorite sorbing material, method is complicated, and preparation cost is high, not easily promotes.
Summary of the invention
The object of the present invention is to provide a kind of cinder of burned coal discarded object that utilizes to prepare the method for aluminium for tobermorite sorbing material, the method can improve the comprehensive utilization value of cinder of burned coal, and be conducive to curbing environmental pollution, and preparation method is simple and convenient, cost is low.
In order to achieve the above object, the technical solution used in the present invention comprises the following steps:
1) cinder of burned coal is calcined in electrothermal furnace, be then cooled to room temperature, by the product grinding after calcining, obtain lime-ash fine powder;
2) by the watery hydrochloric acid acidleach of lime-ash fine powder, then filter, wash, dry, obtain predecessor lime-ash powder;
3) by lime-ash powder, Ca (OH)
2ground and mixed, then adds NaOH wherein and ground and mixed is even, obtains mixture; Spray water glass solution on mixture, and rotary rolling forms the aluminium of spherical particle for tobermorite reactant presoma; Wherein, Ca (OH)
2in Ca and lime-ash powder in SiO
2the mol ratio of contained Si is 5:6; Ca (OH)
2be 1:(1.0 ~ 1.5 with the mol ratio of NaOH);
4) in hydrothermal reaction kettle, add water, then on the water surface, set up stainless steel cloth food steamer, aluminium is inserted in stainless steel cloth food steamer for tobermorite reactant presoma, in 170 ~ 190 DEG C of hydro-thermal water proof steam pressure reaction 16 ~ 20h; React rear cooling release, then isolate product; Product is dried and namely obtains aluminium for tobermorite sorbing material.
Described step 1) in calcining carry out at 650 ~ 750 DEG C, calcination time is 1 ~ 1.5h.
Described step 2) in be (4.8 ~ 5.3) mL:1g by the liquid-solid ratio that adopts during the watery hydrochloric acid acidleach of lime-ash fine powder, the mass concentration of watery hydrochloric acid is 1.3 ~ 1.6%.
Described step 2) in acidleach time temperature be 70 ~ 80 DEG C, the time is 2 ~ 2.5h.
Compared with prior art, beneficial effect of the present invention is:
1, the present invention forms according to the physical chemistry of cinder of burned coal, with it for body material, and composite calcium hydroxide (Ca (OH)
2) and caustic soda (NaOH), adopt hydro-thermal autoclave method synthesis aluminium for tobermorite sorbing material.Obtained aluminium is for part Si in the crystal structure of tobermorite sorbing material
4+by Al
3+non-equivalence ionic compartmentation, thus there is stronger adsorptivity and cation exchange capacity (CEC), therefore in heavy metal ion-containing waste water process and Adsorption of Organic etc., there is higher application prospect, can be used as good ecological environment material nd, thus improve the comprehensive utilization value of cinder of burned coal, be conducive to environmental improvement.
2, Prof. Du Yucang tobermorite material generally adopts hydro-thermal method to prepare, but the shortcoming of hydro-thermal method also needs follow-up filter and cleaning process, more loaded down with trivial details.In order to overcome this shortcoming, present invention employs " hydro-thermal autoclave method ", its specific practice is, the pure water of a constant volume is added in hydrothermal reaction kettle, then use stainless steel cloth food steamer frame on the water surface, aluminium is inserted in stainless steel cloth food steamer for tobermorite reactant presoma, then according to hydrothermal condition water proof steam pressure.This method does not need subsequent filter to wash, simple convenience.
In addition, in cinder of burned coal of the present invention, main component is SiO
2, can be used for preparing the higher tobermorite sorbing material of added value; Also contain many Al in cinder of burned coal simultaneously
2o
3, this is a kind of desirable aluminium doped source not needing additionally to add.Thus utilize cinder of burned coal just directly can prepare absorption and the active higher aluminium of cation exchange for tobermorite, simply facilitate.
3, the present invention take cinder of burned coal as primary raw material, and preparation has sewage treating material-aluminium compared with high added value for tobermorite sorbing material, turns waste into wealth, has higher economy and environment and be worth.The present invention adopts cinder of burned coal discarded object directly to utilize aluminium matter composition wherein to prepare aluminium for tobermorite sorbing material, does not need to add other aluminium source raw material, with low cost.Hydro-thermal steam pressure synthetic method provided by the invention, eliminates the links such as filtration, washing, and production technology is simple, and easy control of reaction conditions, equipment investment is few, and production cost is lower.
4, aluminium of the present invention is directly provided by cinder of burned coal for the silicon source in tobermorite sorbing material and aluminium source, and calcium hydroxide or white lime Ca (OH) are selected in calcium source
2.And the present invention to add caustic soda NaOH be to carry out siliceous raw material to process to rupture Si-O key, make it be easy to reconfigure, promote the forming reactions of tobermorite.In addition, because the source of cinder of burned coal and stacking condition alter a great deal, other impurity much can usually be brought into.The present invention takes the method for pre-pickling, to remove unnecessary impurity.
Accompanying drawing explanation
Fig. 1 is the XRD diffraction pattern of the obtained aluminium of embodiment 1 for tobermorite sorbing material; Wherein, * represents aluminium for tobermorite ,+represent Ca
3al
2(SiO
4)
1.53(OH)
5.88;
Fig. 2 is the XRD diffraction pattern of the obtained aluminium of embodiment 3 for tobermorite sorbing material; Wherein, wherein, * represents aluminium for tobermorite ,+represent Ca
3al
2(SiO
4)
1.53(OH)
5.88;
To be the obtained aluminium of embodiment 1 scheme for the SEM of tobermorite sorbing material Fig. 3;
Fig. 4 be the obtained aluminium of embodiment 1 for tobermorite for the adsorption curve figure containing rhodamine B organic dyestuff simulated wastewater.
Detailed description of the invention
Embodiment 1:
1) cinder of burned coal is placed in ceramic crucible, in 700 DEG C of calcining 1.5h in electrothermal furnace, is then cooled to room temperature, after fully being ground by the product after calcining, obtains lime-ash fine powder;
2) by mass concentration be 1.5% watery hydrochloric acid join in lime-ash fine powder according to the liquid-solid ratio of 5mL:1g, at 80 DEG C, heated at constant temperature stirs 2.0h to carry out acidleach, filters, washing, dry after acidleach, obtains predecessor lime-ash powder;
3) by lime-ash powder, Ca (OH)
2ground and mixed, then adds NaOH wherein and ground and mixed is even, obtains mixture; Spray water glass solution on mixture, and rotary rolling forms the aluminium of spherical particle for tobermorite reactant presoma; Wherein, Ca (OH)
2in Ca and lime-ash powder in SiO
2the mol ratio of contained Si is 5:6; Ca (OH)
2be 1:1 with the mol ratio of NaOH;
4) in hydrothermal reaction kettle, add water, then on the water surface, set up stainless steel cloth food steamer, aluminium is inserted in stainless steel cloth food steamer for tobermorite reactant presoma, in 180 DEG C of hydro-thermal water proof steam pressure reaction 18h; React rear cooling release, then isolate product; Product is dried and namely obtains aluminium for tobermorite sorbing material.
In order to verify the validity of above technical scheme, invention has been the checking of following test analysis.
1, X-ray diffraction (XRD) test
Fig. 1 is the XRD test result of the present embodiment gained aluminium for tobermorite sorbing material.As seen from Figure 1, embodiment 1 has synthesized the higher aluminium of purity for tobermorite sorbing material, and peak shape is sharp-pointed, and intensity is high.Cinder of burned coal aluminum content selected by this experiment is higher, has occurred minute quantity Ca in sample
3al
2(SiO
4)
1.53(OH)
5.88crystalline phase, but this crystalline phase of minute quantity can not have an impact to the performance of aluminium for tobermorite sorbing material.
2, SEM (SEM) test
Fig. 3 be in embodiment 1 gained aluminium for field emission scanning electron microscope (SEM) test result of tobermorite sorbing material.As seen from Figure 3, aluminium is good for tobermorite crystal development, and flakey aluminium, for the mesoporous shape skeleton structure of tobermorite Crystallization, has higher specific area, and this is the basic reason producing stronger absorption property and ion-exchange performance.
3, the absorption property test of rhodamine B organic dyestuff simulated wastewater
First with rhodamine B organic dyestuff preparation simulated wastewater, again according to adding the aluminium of 0.1g synthesis in every 10ml simulated wastewater for tobermorite sorbing material, stirring and adsorbing reaction 0 ~ 60min, centrifugal elimination solid constituent, after detecting absorption with supernatant, the absorbance of solution changes.Namely 0min is the absorbance of rhodamine B organic dyestuff simulated wastewater, can be used as standard, is used for representing the change of absorbance under different sorption reaction time.Namely the reduced value of absorbance represents the value added of percent of decolourization, is used for weighing the size of species adsorbs ability.
Fig. 4 be in embodiment 1 aluminium for the absorption property test result of tobermorite sorbing material.As seen from Figure 4, if with the absorbance of rhodamine B organic dyestuff simulated wastewater for standard, along with the increase of sorption reaction time, each sample constantly declines in the absorbance at 554nm place, percent of decolourization constantly increases in other words, and 60min adsorption reaction percent of decolourization can reach 87.6%.As can be seen here, the aluminium prepared by the present invention has stronger water pollutant for tobermorite sorbing material and removes ability.
Embodiment 2:
1) cinder of burned coal is placed in ceramic crucible, in 650 DEG C of calcining 1.5h in electrothermal furnace, is then cooled to room temperature, after fully being ground by the product after calcining, obtains lime-ash fine powder;
2) by mass concentration be 1.6% watery hydrochloric acid join in lime-ash fine powder according to the liquid-solid ratio of 4.8mL:1g, at 70 DEG C, heated at constant temperature stirs 2.5h to carry out acidleach, filters, washing, dry after acidleach, obtains predecessor lime-ash powder;
3) by lime-ash powder, Ca (OH)
2ground and mixed, then adds NaOH wherein and ground and mixed is even, obtains mixture; Spray water glass solution on mixture, and rotary rolling forms the aluminium of spherical particle for tobermorite reactant presoma; Wherein, Ca (OH)
2in Ca and lime-ash powder in SiO
2the mol ratio of contained Si is 5:6; Ca (OH)
2be 1:1.5 with the mol ratio of NaOH;
4) in hydrothermal reaction kettle, add water, then on the water surface, set up stainless steel cloth food steamer, aluminium is inserted in stainless steel cloth food steamer for tobermorite reactant presoma, in 170 DEG C of hydro-thermal water proof steam pressure reaction 20h; React rear cooling release, then isolate product; Product is dried and namely obtains aluminium for tobermorite sorbing material.
Embodiment 3:
1) cinder of burned coal is placed in ceramic crucible, in 750 DEG C of calcining 1.0h in electrothermal furnace, is then cooled to room temperature, after fully being ground by the product after calcining, obtains lime-ash fine powder;
2) by mass concentration be 1.3% watery hydrochloric acid join in lime-ash fine powder according to the liquid-solid ratio of 5.3mL:1g, at 75 DEG C, heated at constant temperature stirs 2.2h to carry out acidleach, filters, washing, dry after acidleach, obtains predecessor lime-ash powder;
3) by lime-ash powder, Ca (OH)
2ground and mixed, then adds NaOH wherein and ground and mixed is even, obtains mixture; Spray water glass solution on mixture, and rotary rolling forms the aluminium of spherical particle for tobermorite reactant presoma; Wherein, Ca (OH)
2in Ca and lime-ash powder in SiO
2the mol ratio of contained Si is 5:6; Ca (OH)
2be 1:1.2 with the mol ratio of NaOH;
4) in hydrothermal reaction kettle, add water, then on the water surface, set up stainless steel cloth food steamer, aluminium is inserted in stainless steel cloth food steamer for tobermorite reactant presoma, in 190 DEG C of hydro-thermal water proof steam pressure reaction 16h; React rear cooling release, then isolate product; Product is dried and namely obtains aluminium for tobermorite sorbing material.
Fig. 2 is the XRD test result of the present embodiment gained aluminium for tobermorite sorbing material.As seen from Figure 2, embodiment 2-in-1 become the higher aluminium of purity for tobermorite sorbing material, peak shape is sharp-pointed, and intensity is high.Cinder of burned coal aluminum content selected by this experiment is higher, has occurred minute quantity Ca in sample
3al
2(SiO
4)
1.53(OH)
5.88crystalline phase, but this crystalline phase of minute quantity can not have an impact to the performance of aluminium for tobermorite sorbing material.
Embodiment 4:
1) cinder of burned coal is placed in ceramic crucible, in 680 DEG C of calcining 1.5h in electrothermal furnace, is then cooled to room temperature, after fully being ground by the product after calcining, obtains lime-ash fine powder;
2) by mass concentration be 1.4% watery hydrochloric acid join in lime-ash fine powder according to the liquid-solid ratio of 5.1mL:1g, at 78 DEG C, heated at constant temperature stirs 2.3h to carry out acidleach, filters, washing, dry after acidleach, obtains predecessor lime-ash powder;
3) by lime-ash powder, Ca (OH)
2ground and mixed, then adds NaOH wherein and ground and mixed is even, obtains mixture; Spray water glass solution on mixture, and rotary rolling forms the aluminium of spherical particle for tobermorite reactant presoma; Wherein, Ca (OH)
2in Ca and lime-ash powder in SiO
2the mol ratio of contained Si is 5:6; Ca (OH)
2be 1:1.4 with the mol ratio of NaOH;
4) in hydrothermal reaction kettle, add water, then on the water surface, set up stainless steel cloth food steamer, aluminium is inserted in stainless steel cloth food steamer for tobermorite reactant presoma, in 180 DEG C of hydro-thermal water proof steam pressure reaction 19h; React rear cooling release, then isolate product; Product is dried and namely obtains aluminium for tobermorite sorbing material.
Embodiment 5:
1) cinder of burned coal is placed in ceramic crucible, in 730 DEG C of calcining 1.3h in electrothermal furnace, is then cooled to room temperature, after fully being ground by the product after calcining, obtains lime-ash fine powder;
2) by mass concentration be 1.4% watery hydrochloric acid join in lime-ash fine powder according to the liquid-solid ratio of 5.2mL:1g, at 80 DEG C, heated at constant temperature stirs 2.0h to carry out acidleach, filters, washing, dry after acidleach, obtains predecessor lime-ash powder;
3) by lime-ash powder, Ca (OH)
2ground and mixed, then adds NaOH wherein and ground and mixed is even, obtains mixture; Spray water glass solution on mixture, and rotary rolling forms the aluminium of spherical particle for tobermorite reactant presoma; Wherein, Ca (OH)
2in Ca and lime-ash powder in SiO
2the mol ratio of contained Si is 5:6; Ca (OH)
2be 1:1.3 with the mol ratio of NaOH;
4) in hydrothermal reaction kettle, add water, then on the water surface, set up stainless steel cloth food steamer, aluminium is inserted in stainless steel cloth food steamer for tobermorite reactant presoma, in 190 DEG C of hydro-thermal water proof steam pressure reaction 17h; React rear cooling release, then isolate product; Product is dried and namely obtains aluminium for tobermorite sorbing material.
Claims (2)
1. utilize cinder of burned coal discarded object to prepare the method for aluminium for tobermorite sorbing material, it is characterized in that, comprise the following steps:
1) cinder of burned coal is calcined in electrothermal furnace, be then cooled to room temperature, by the product grinding after calcining, obtain lime-ash fine powder;
2) by the watery hydrochloric acid acidleach of lime-ash fine powder, then filter, wash, dry, obtain predecessor lime-ash powder;
3) by lime-ash powder, Ca (OH)
2ground and mixed, then adds NaOH wherein and ground and mixed is even, obtains mixture; Spray water glass solution on mixture, and rotary rolling forms the aluminium of spherical particle for tobermorite reactant presoma; Wherein, Ca (OH)
2in Ca and lime-ash powder in SiO
2the mol ratio of contained Si is 5:6; Ca (OH)
2be 1:(1.0 ~ 1.5 with the mol ratio of NaOH);
4) in hydrothermal reaction kettle, add water, then on the water surface, set up stainless steel cloth food steamer, aluminium is inserted in stainless steel cloth food steamer for tobermorite reactant presoma, in 170 ~ 190 DEG C of hydro-thermal water proof steam pressure reaction 16 ~ 20h; React rear cooling release, then isolate product; Product is dried and namely obtains aluminium for tobermorite sorbing material;
Described step 1) in calcining carry out at 650 ~ 750 DEG C, calcination time is 1 ~ 1.5h; Described step 2) in be (4.8 ~ 5.3) mL:1g by the liquid-solid ratio that adopts during the watery hydrochloric acid acidleach of lime-ash fine powder, the mass concentration of watery hydrochloric acid is 1.3 ~ 1.6%.
2. the cinder of burned coal discarded object that utilizes according to claim 1 prepares the method for aluminium for tobermorite sorbing material, it is characterized in that: described step 2) in acidleach time temperature be 70 ~ 80 DEG C, the time is 2 ~ 2.5h.
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CN1327947A (en) * | 2001-06-13 | 2001-12-26 | 中国科学院兰州化学物理研究所 | Process for preparing Ti-Si molecular sieve |
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