CN104150941B - A kind of slag based mesoporous material and preparation method thereof - Google Patents
A kind of slag based mesoporous material and preparation method thereof Download PDFInfo
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Abstract
The invention discloses a kind of slag based mesoporous material and preparation method thereof, this slag mesoporous material made is put into whipping appts stirred by raw steel ground-slag, silicon ash, sodium hydroxide, pore forming agent Emulsion acrylic resin, form through mould molding, maintenance and roasting thereof, wherein, the add-on of silicon ash, sodium hydroxide and Emulsion acrylic resin is based on slag quality; The add-on of silicon ash is 10% of slag quality, and the add-on of sodium hydroxide is 4% of slag quality, and the add-on of Emulsion acrylic resin is the 0.1%-5% of slag quality, and the addition of water and slag mass ratio are 0.27-0.30.Compared with the sample without pore forming agent, after adding the pore forming agent of optimum quantity, the mesopore volume of sample adds 226.05%.Completely disposablely can utilize slag, obtain the mesoporous material of high added value, whole technological process is simple, without the need to carrying out any process to slag, three-waste free discharge, environmental protection; The controlled synthesis of mesoporous material can be realized.
Description
Technical field
The invention belongs to the preparation field of solid waste resource recovery recycle and novel material, be specifically related to a kind of slag based mesoporous material and preparation method thereof.
Background technology
Slag is a kind of solid waste of discharging in steelmaking process, often produces the slag that 1 ton of crude steel produces about 10-20% approximately
[1].Within 2013, crude steel output is 7.79 hundred million tons, about 1.17 hundred million tons, the slag of generation
[2].Because slag belongs to a kind of inertia slag, the utilization ratio of its high added value is very limited.So the long-term large steel slag piled up not only takies a large amount of good farmlands, and exposes to the sun and rain, and causes serious environmental pollution.It can be used as preparative chemistry to excite the starting material of slag based cementitious material, is one of effective way of slag mass-producing utilization.About utilizing prepared from steel slag for the document of Chemical-activated Materials
[3-9]and patent
[10]there are many reports.In addition, Zhang Yaojun
[11-13]deng patent of invention (ZL201110276342.2, ZL201210166582.1, ZL201210166581.7) disclose and chemi-excitation slag base composite gelled material be used for dye degrades and new forms of energy research.In recent years, some patent document discloses and utilize solid waste preparation to have mechanical large pore material.Such as true in spreading out
[14]deng Chinese patent application (CN101708399A) disclose a kind of porous slag filter material and preparation method thereof, according to slag 30-80%, clay 15-50%, pore former 5-20% (coal gangue, starch, sawdust, calcium carbonate, one wherein) raw material weight per-cent stir, spread the shaping obtained raw material ball of water, drying, 400-700 DEG C thermal pretreatment, then obtain porous slag filter material 1000-1300 DEG C of roasting, the characteristic which disclosing the grain slag filtering material adopting the method to prepare is porous, and aperture is large.Nest opens
[15]deng Chinese patent (CN102603355A) disclose a kind of basic group geopolymer porous material, this patent of invention is by slurry (water glass 20-50 part, slag 20-50 part, flyash 10-20 part, metakaolin 10-20 part, polypropylene fibre 0.1-1.5 part, and by pva powder, vinyl acetate, ethylene copolymer rubber powder composition redispersable latex powder 0.3-1.0 part) and composite foamable agent (composite foamable agent is made up of following weight parts raw material: hydrogen peroxide 24-35 part, water 64-75 part, suds-stabilizing agent 0.5-1 part, animal foaming auxiliary agent 1-1.5 part) form according to the ratio combination of weight ratio 9-38:1, foaming block intensity prepared by this patent of invention is between 0.5-8MPa, and raw material type is various, and the material of preparation has the feature of macroscopical macropore.Build up the Army in field
[16]deng Chinese patent application (CN102584318A) disclose a kind of method that Li-adding Al alloy slag prepares porous insulation material, the method is with Li-adding Al alloy slag, flyash is raw material material, cullet, clay and wilkinite are binding agent, Wingdale, SiC, carbon dust, paraffin, stearic acid, organic fibre and millet are expanding agent, by mass ratio 40%-70% Li-adding Al alloy slag, 10%-40% binding agent and 5%-30% expanding agent, by fragmentation, batch mixing, be shaped, demoulding 700-1300 DEG C of sintering, from the scanning electron microscopic picture that patent provides, what obtain after utilizing the method is the lagging material of mechanical macropore.
Mesoporous material is the material of class aperture between micropore and macropore, according to the definition of International Union of Pure and Applied Chemistry(IUPAC) (IUPAC)
[17], poromerics (aperture is less than 2nm), mesoporous material (aperture is between 2 ~ 50nm) and large pore material (aperture is greater than 50nm) can be divided into according to large young pathbreaker's porous material in aperture.Because the arranged distribution feature of hole in space is different, mesoporous material can be divided into again two kinds of order and disorder
[18].Cats product is utilized to be the classical way of synthesis M41S series ordered mesoporous material as template
[19,20]and sol-gel method prepares the typical method of unordered oxide mesoporous material.Unordered mesoporous material has hole shape complexity, irregular, and is not communicated with mutually, the feature that pore size distribution is wider.
In sum, applicant retrieved by amount of literature data and both at home and abroad patent look into new, do not find to utilize solid waste prepared from steel slag for the document of mesoporous material and patent report.
Below the leading reference that contriver provides:
[1]P.Y.Mahieux,J.E.Aubert，G.Escadeillas，Utilization ofweathered basic oxygen furnace slag in the production of hydraulicroad binders，Construction and Building Materials23(2)(2009)742–747。
[2]World Steel Association,Crude steel production2013[EB/OL],Brussels:World Steel Association,http://www.worldsteel.org/stat-istics/statistics-archive/2013-steel-production.html.2014-06-04。
[3]Q.Wang,P.Yan,Hydration properties of basic oxygen furnacesteel slag，Construction and Building Materials24(7)(2010)1134-1140。
[4] Dong Tao, Tao Zhendong, evergreen, several exciting agent on the impact of activity of steel slag, cement works 5 (2012) 27-29.
[5] He Tianhui, Huang is relied on oneself, Feng Dingwu, Liu Yuanyuan, Sun Kai, Wang little Feng, a kind of slag-kaolin based geology polymer material metal mine 9 (2012) 163-167.
[6] Li Yikai, Liu Futian, Zhou Zonghui, Cheng Xin, compound activator activated steel slag prepares composite gelled material research, Wuhan University of Technology's journal 31 (4) (2009) 11-14.
[7] Xu Bin, Deng Guozhu, Zhang Tianshi, Wang Yuping. alkali-activated carbonatite steel slag cement is studied, Chongqing Environmental Science 20 (6) (1998) 39-42.
[8]E.Belhadj,C.Diliberto,André Lecomte.Characterization andactivation of Basic Oxygen Furnace slag,Cement and ConcreteComposites34(1)(2012)34-40。
[9] Fan Chuangang, Xu Lan, Zhu Siwei, Li Jiamao, Tan Jie, the research of alkaline excitation hydration activity of steel slag, Anhui University of Technology's journal 23 (1) (2006) 30-33.
[10] Wang Binggang, clinker-free high-antiflex and-strength unburned slag cement, publication No.: CN1140152
[11] Zhang Yaojun, Liu Licai, Xu Delong, Wang Yachao, Xu Yong, Wang Jing, Ni
2+the preparation of doping geopolymer catalyzer and the application in organic matter degradation, the patent No.: ZL201110276342.2.
[12] Zhang Yaojun, Liu Licai, Wang Bingli, Ni Lulu, Wang Yachao, the slag based inorganic polymer-preparation of zinc oxide semi-conductor composite catalyst and the application in degradation of dye waste water thereof, the patent No.: ZL201210166582.1.
[13] Zhang Yaojun, slag based cementitious material-zinc oxide semi-conductor composite catalyst and the application in solar energy photocatalytic hydrogen production by water decomposition, the patent No.: ZL201210166581.7.
[14] Yu Yanzhen, Feng Yan, Wang Jiabin, Tan Juan, Zhao Chunhui, Sun Yong, Liu Zhenliang, Zhao Youheng, a kind of stephanoporate grain slag filtering material and preparation method thereof, publication number: CN101708399A.
[15] nest opens, Liu Haifeng, a kind of basic group geopolymer porous material, publication number: CN102603355A.
[16] build up the Army in field, and Zhang Shengen, Zhang Jing, Pan Dean, Liu Bo, a kind of Li-adding Al alloy slag prepares the method for porous insulation material, publication number: CN102584318A.
[17]D.H.Everett,IUPAC manual of symbols and terminology,Pureand Applied Chemistry31(1972)578-638。
[18]P.Schmidt-Winkel,W.W.Lukens，D.Jr Zhao，et a1.，Mesocellular siliceous foams with unifomrly sized cells and windows,Journal of the American Chemical Society121(1999)254-255。
[19]J.S.Beck，J.E.Vartwli，et a1.,A new family of mesoporousmolecular sieves prepared with liquid-crystal template mechanism,Journal of the American Chemical Society114(1992)10834-10843。
[20]G.T.Kresge,M.E.Leonowica,et a1.,Ordered mesoporousmolecular sieves synthesized by liquid-crystal template mechanism,Nature359(1992)710-712。
Summary of the invention
The object of the invention is to, a kind of slag based mesoporous material and preparation method thereof is provided.
In order to realize above-mentioned task, the present invention takes following technical solution:
A kind of slag based mesoporous material, it is characterized in that, this slag mesoporous material made is that raw steel ground-slag, silicon ash, sodium hydroxide, pore forming agent Emulsion acrylic resin are put into whipping appts and carried out mix, form through mould molding, maintenance and roasting thereof, wherein, the add-on of silicon ash, sodium hydroxide and Emulsion acrylic resin is based on slag quality; The add-on of silicon ash is 10% of slag quality, and the add-on of sodium hydroxide is 4% of slag quality, and the add-on of Emulsion acrylic resin is the 0.1%-5% of slag quality, and the addition of water and slag mass ratio are 0.27-0.30.
Above-mentioned slag based mesoporous material and preparation method thereof, is characterized in that, comprise the following steps:
(1) take slag, silicon ash and water by formula ratio, wherein water and slag mass ratio are: 0.27-0.30, and steel-making slag powder are mixed with silicon ash;
(2) sodium hydroxide of formula ratio is dissolved in suitable quantity of water, form aqueous sodium hydroxide solution;
(3) pore forming agent acrylate resin emulsion is taken by formula rate;
(4) under room temperature, aqueous sodium hydroxide solution is poured in stirred vessel, then pore forming agent Emulsion acrylic resin is added, then the steel-making slag powder mixed and silicon ash are added and carry out mix, form slurry;
(5) slurry is loaded die for molding, 60 DEG C of maintenance 6h in thermostat container, after taking-up, room temperature maintenance form removal after 1 day, curing room natural curing 2 days, obtains slag based cementitious material block, detects its ultimate compression strength and folding strength.
(6) slag based cementitious material block is put into muffle furnace and be warming up to 450 DEG C with the temperature rise rate of 2 DEG C/min, after insulation 4h, naturally cooling, obtains slag based mesoporous material, detects its ultimate compression strength.Mercury penetration method detection aperture distributes.
The technique effect that slag based mesoporous material prepared by the present invention brings is:
(1) recycling economy development of steelworks can be promoted, for disposable completely innoxious, the high added value of slag, mass-producing, recycling provide a new way.
(2) cheaper starting materials is easy to get, simple for process, without the need to carrying out any process to slag, three-waste free discharge, environmental protection; The controlled synthesis of mesoporous material can be realized.
(3) the slag based mesoporous material prepared has higher ultimate compression strength, can meet the demand to mesoporous material such as catalyzer and sorbent material.
Innovation of the present invention is:
Propose the novel method preparing slag based mesoporous material using acrylate resin emulsion as pore forming agent; Meanwhile, by controlling the dosage increasing aperture, maturing temperature, to realize the controlled synthesis of slag based mesoporous material, has enriched the new variety of mesoporous material.
Accompanying drawing explanation
Fig. 1 is operational path prepared by slag based mesoporous material;
Fig. 2 is the pore size distribution curve that mercury penetration method detects slag based mesoporous material sample;
Fig. 3 is Emulsion acrylic resin thermal analysis curve;
Below in conjunction with drawings and Examples, the present invention is described in further detail.
Embodiment
Technical thought of the present invention is for raw material with solid waste slag, take Emulsion acrylic resin as pore forming agent, by modulation preparation condition, especially by dosage and the maturing temperature of modulation pore forming agent, to realize the controlled synthesis of slag based mesoporous material, enrich the kind of mesoporous material.Meanwhile, preparation process technique wants simple, disposablely can utilize slag, non-secondary pollution, have great importance for the high value added utilization of slag and the recycling economy of iron and steel enterprise.
As shown in Figure 1, Fig. 1 gives technical process prepared by slag based mesoporous material; Below in an example, preparing the main raw material(s) that slag based mesoporous material adopts is industrial solid castoff slag, silicon ash, sodium hydroxide; Emulsion acrylic resin, specific performance is as follows:
1, slag:
Slag, from Hancheng Region, Shaanxi Long Gang company, is put into baking oven 110 DEG C of constant temperature drying 3h by slag, and through ball milling 2 hours, density was 3.40g/cm
3, Blain specific surface is 539m
2/ kg.
Main oxides composition (mass percent): the SiO of slag
2(16.40%), Al
2o
3(3.45%), CaO (44.00%), Fe
2o
3(19.68%), MgO (5.67%), TiO
2(0.90%), Na
2o (0.12%), other (9.78%).
2, silicon ash
Silicon ash raw material is purchased from Xi'an Lin Yuan limited liability company, and silicon ash raw material is put into air dry oven, and dry 3h, naturally cooling under 110 DEG C of conditions, its density is 2.2 × 10
3kg/m
3.
Main oxides composition (mass percent): the SiO of silicon ash
2(86.75%), Al
2o
3(0.49%), CaO (0.60%), Fe
2o
3(1.18%), MgO (2.94%), Na
2o (1.17%), ZnO (1.33%), other (5.54%).
3, sodium hydroxide
Sodium hydroxide is purchased from Tianjin Jin Dong Tian Zheng fine chemistry chemical reagent work, is analytical reagent.
4, acrylate resin emulsion
Acrylate resin emulsion is purchased from sends Buddhist nun's chemical reagent factory, outward appearance blue streak ivory-white stringy liquid, solid content 48%, pH=9.5; Experiment shows that acrylate resin emulsion has satisfactory stability in dense sodium hydroxide solution.
5, mercury penetration method is adopted to detect the pore size distribution of sample.
Here is the embodiment that contriver provides, and it should be noted that, these embodiments only for a better understanding of the present invention, the invention is not restricted to these embodiments.
Embodiment 1:
Precise slag 1400g, as measurement basis (100%); Adopt outer doping, Silica fume content is 10% of slag quality, and solid sodium hydroxide volume is 4% of slag quality, and water and slag mass ratio are 0.27.
At room temperature, solid sodium hydroxide is dissolved in water, form aqueous sodium hydroxide solution.This aqueous solution is poured into and two turn double speed and only starch in stirrer, add again and be pre-mixed uniform steel-making slag powder and wollastonite powder carries out mix, form the slurry mixed, slurry is contained into 40mm × 40mm × 160mm steel three die for molding, three gang mould tools are put into plastics film sealing bag, maintenance 6 hours under thermostat container 60 DEG C of conditions, after taking-up, room temperature maintenance form removal after 1 day, maintenance 2 days again in curing room, obtain slag based cementitious material block, detect its ultimate compression strength 26.1MPa, folding strength 3.1MPa.
This slag based cementitious material block is put into muffle furnace, is warming up to 450 DEG C with the temperature rise rate of 2 DEG C/min, after insulation 4h, take out after making its naturally cooling, obtain slag based cementitious material, detecting its ultimate compression strength is 24.8MPa; Mercury penetration method detects the pore size distribution result of sample as shown in table 1 and Fig. 2, and as can be seen from Table 1, the mesopore volume of slag based cementitious material is 0.030768 (mL/g).
Table 1: mercury penetration method detects the pore size distribution result of sample
Embodiment 2:
Precise slag 1400g, as measurement basis (100%); Adopt outer doping, Silica fume content is 10% of slag quality, and solid sodium hydroxide volume is 4% of slag quality, and the quality of Emulsion acrylic resin is 0.1% of slag quality, and water and slag mass ratio are 0.27.At room temperature, solid sodium hydroxide is dissolved in water, form aqueous sodium hydroxide solution.Aqueous sodium hydroxide solution and Emulsion acrylic resin are poured into and two turn double speed and only starch in stirrer, add again and be pre-mixed uniform steel-making slag powder and wollastonite powder carries out mix, form the slurry mixed, slurry is loaded 40mm × 40mm × 160mm steel three die for molding, three gang mould tools are put into plastics film sealing bag, maintenance 6 hours under thermostat container 60 DEG C of conditions, after taking-up, room temperature maintenance form removal after 1 day, the maintenance 2 days again of curing room room temperature, obtain slag based cementitious material block, detect its ultimate compression strength 25.3MPa, folding strength 5.6MPa.
This slag based cementitious material block is put into muffle furnace, is warming up to 450 DEG C with the temperature rise rate of 2 DEG C/min, after insulation 4h, take out after naturally cooling, obtain slag based mesoporous material, detecting its ultimate compression strength is 23.5MPa;
Mercury penetration method detects the pore size distribution of sample, result is as shown in table 1 and Fig. 2, as can be seen from Table 1, the mesopore volume of slag based mesoporous material is 0.065648 (mL/g), add 0.03488 (mL/g) than the mesopore volume of slag based cementitious material when not mixing Emulsion acrylic resin, the mesopore volume percentage ratio of increase is 113.36%; Meanwhile, as can be seen from Figure 2, the area under the curve under 10-30nm aperture obviously increases.
The reason that the maturing temperature preparing slag based mesoporous material is chosen for 450 DEG C is, with the maximum temperature 380 DEG C of the weight loss (%) in Fig. 3 Emulsion acrylic resin thermal analysis curve and the weightlessness in differential thermogravimetric curve for foundation, be decomposed to form mesoporous completely in order to ensure pore forming agent acrylic resin, therefore selection 450 DEG C is the complete decomposition temperature of acrylic resin.
Embodiment 3:
Precise slag 1400g, as measurement basis (100%); Adopt outer doping, Silica fume content is 10% of slag quality, and solid sodium hydroxide volume is 4% of slag quality, and the quality of Emulsion acrylic resin is 5% of slag quality, and water and slag mass ratio are 0.30.At room temperature, solid sodium hydroxide is dissolved in water, form aqueous sodium hydroxide solution.Aqueous sodium hydroxide solution and Emulsion acrylic resin are poured into and two turn double speed and only starch in stirrer, add again and be pre-mixed uniform steel-making slag powder and wollastonite powder carries out mix, form the slurry mixed, slurry is loaded 40mm × 40mm × 160mm steel three die for molding, three gang mould tools are put into plastics film sealing bag, under thermostat container 60 DEG C of conditions, maintenance is taken out for 6 hours, room temperature maintenance form removal after 1 day, maintenance 2 days again under curing room natural condition, obtain the test block of slag based cementitious material, detect its ultimate compression strength 18.9MPa, folding strength 3.1MPa.
Muffle furnace is put in this slag based cementitious material test block, is warming up to 450 DEG C with the temperature rise rate of 2 DEG C/min, after insulation 4h, take out after making its naturally cooling, obtain slag based mesoporous material, detecting its ultimate compression strength is 15.1MPa.
Mercury penetration method detects the pore size distribution of sample, result is as shown in table 1 and Fig. 2, as can be seen from Table 1, the mesopore volume of slag based mesoporous material is 0.100320 (mL/g), add 0.069552 (mL/g) than the mesopore volume of slag based cementitious material during not admixture Emulsion acrylic resin, the percent by volume of increase is 226.05%; Meanwhile, as can be seen from Figure 2, the area under the curve of 2-50nm mesoporous pore size significantly increases, and it can amass aperture significantly to the displacement of mesoporous direction.As long as show to control the dosage of pore forming agent Emulsion acrylic resin and maturing temperature and temperature rise rate, the controlled synthesis of slag based mesoporous material just can be realized.
Embodiment 4:
Using the obtained slag based mesoporous material of embodiment 3 as support of the catalyst, the cerium dioxide of load 8% (mass percent) is as catalyzer.
Accurately take 0.05 gram of above-mentioned catalyzer, put it in the beaker of the 8mg/L malachite green aqueous solution filling 100mL under magnetic stirring, with simulated visible light source (500W xenon lamp) from the aqueous solution the plan vertical irradiation beaker of beaker, carry out the photocatalytic degradation of dyestuff, irradiation 220 minutes, the degradation rate detecting malachite green is 100%; And at identical conditions, the degradation rate of pure cerium dioxide to malachite green is only 5%; Show that slag based mesoporous material has high visible light catalysis activity as support of the catalyst.
Claims (5)
1. a slag based mesoporous material, it is characterized in that, this slag mesoporous material made is that raw steel ground-slag, silicon ash, sodium hydroxide, pore forming agent Emulsion acrylic resin are put into whipping appts and carried out mix, slag based cementitious material is obtained through mould molding, maintenance, then form through roasting, wherein, the add-on of silicon ash, sodium hydroxide and Emulsion acrylic resin is based on slag quality; The add-on of silicon ash is 10% of slag quality, and the add-on of sodium hydroxide is 4% of slag quality, and the add-on of Emulsion acrylic resin is the 0.1%-5% of slag quality, and the addition of water and slag mass ratio are 0.27-0.30;
Described roasting slag based cementitious material block is put into muffle furnace be warming up to 450 DEG C with the temperature rise rate of 2 DEG C/min, after insulation 4h, and naturally cooling.
2. slag based mesoporous material as claimed in claim 1, is characterized in that, consisting of of the main oxides mass percent of described slag: SiO
2: 16.40%, Al
2o
3: 3.45%, CaO:44.00%, Fe
2o
3: 19.68%, MgO:5.67%, TiO
2: 0.90%, Na
2o:0.12%, other: 9.78%.
3. slag based mesoporous material as claimed in claim 1, it is characterized in that, the main oxides mass percent of described silicon ash consists of: SiO
2: 86.75%, Al
2o
3: 0.49%, CaO:0.60%, Fe
2o
3: 1.18%, MgO:2.94%, Na
2o:1.17%, ZnO:1.33%, other: 5.54%.
4. the preparation method of the slag based mesoporous material of claims 1 to 3 described in one of them, is characterized in that, comprise the following steps:
1) take slag, silicon ash and water by formula ratio, wherein water and slag mass ratio are: 0.27-0.30, and steel-making slag powder are mixed with silicon ash;
2) sodium hydroxide of formula ratio is dissolved in suitable quantity of water, form aqueous sodium hydroxide solution;
3) pore forming agent acrylate resin emulsion is taken by formula rate;
4) under room temperature, aqueous sodium hydroxide solution is poured in stirred vessel, then pore forming agent Emulsion acrylic resin is added, then the steel-making slag powder mixed and silicon ash are added and carry out mix, form slurry;
5) slurry is loaded die for molding, 60 DEG C of maintenance 6h in thermostat container, after taking-up, room temperature maintenance form removal after 1 day, curing room natural curing 2 days, obtains slag based cementitious material block;
6) slag based cementitious material block is put into muffle furnace and be warming up to 450 DEG C with the temperature rise rate of 2 DEG C/min, after insulation 4h, naturally cooling, obtains slag based mesoporous material.
5. the slag based mesoporous material described in claim 1 or 2 is used for the application of support of the catalyst.
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| CN106215615A (en) * | 2016-08-03 | 2016-12-14 | 福瑞莱环保科技（深圳）有限公司 | A kind of sub-preparation method and applications of absorption with absorption and degradation function |
| WO2020141379A1 (en) | 2019-01-04 | 2020-07-09 | Sabic Global Technologies B.V. | Steel ladle furnace slag binder materials and uses thereof |
| CN114377662A (en) * | 2022-03-03 | 2022-04-22 | 华北理工大学 | Steel slag-based porous geopolymer adsorption material and preparation method thereof |
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| CN101445254A (en) * | 2008-12-31 | 2009-06-03 | 平朔煤炭工业公司 | Method for producing 4A molecular sieve |
| CN102633280A (en) * | 2012-03-21 | 2012-08-15 | 淮南联合大学 | Method for synthesising mesoporous molecular sieve by utilizing pulverized fuel ash |
| CN103172080A (en) * | 2013-03-27 | 2013-06-26 | 南京理工大学 | Method for preparing mesoporous molecular sieve |
| CN103435064A (en) * | 2013-08-20 | 2013-12-11 | 东北石油大学 | Method for preparing nano-scale ZSM-5 molecular sieve by using coal ash |
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