CN104163615A - Slag based mesoporous material and preparation method thereof - Google Patents
Slag based mesoporous material and preparation method thereof Download PDFInfo
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- CN104163615A CN104163615A CN201410344226.3A CN201410344226A CN104163615A CN 104163615 A CN104163615 A CN 104163615A CN 201410344226 A CN201410344226 A CN 201410344226A CN 104163615 A CN104163615 A CN 104163615A
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- slag
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02W—CLIMATE CHANGE MITIGATION TECHNOLOGIES RELATED TO WASTEWATER TREATMENT OR WASTE MANAGEMENT
- Y02W30/00—Technologies for solid waste management
- Y02W30/50—Reuse, recycling or recovery technologies
- Y02W30/91—Use of waste materials as fillers for mortars or concrete
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Abstract
The invention discloses a slag based mesoporous material and a preparation method thereof; the slag based mesoporous material is prepared by putting raw material slag, sodium hydroxide water and pore increasing agent glucose into a mixing device for mixing, using a die for molding, curing, and burning; and taking the adding quantity of the slag mass as a basis, the adding quantity of the sodium hydroxide is 6% of the slag mass, the adding quantity of the pore increasing agent glucose is 3%-6% of the slag mass, and the ratio of water adding quantity to slag mass is 0.24-0.28. Compared with a sample free of the pore increasing agent, after addition of the pore increasing agent in an optimum adding amount, the mesopore volume of a sample is increased by 102.63%; slag can be completely used in one time, the slag based mesoporous material with high added value can be obtained, the whole process is simple, no slag treatment is needed, no three wastes is discharged, the slag based mesoporous material is green and environmentally-friendly, and controllable preparation of the slag based 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
Blast-furnace slag is a kind of waste residue of discharging from blast furnace while smelting the pig iron, and 1 ton of pig iron of common every production approximately will discharge 0.3-0.9 ton blast furnace slag, and the output of the Chinese pig iron in 2012 reaches 6.58 hundred million tons, and the slag of discharge is hundred million tons more than of 1.97-5.9.At present, slag is mainly produced slag micropowder as operating mine slag cement or as cement, concrete Additive, produces inorganic paint, as sewage-treating agent, manufactures calcium-silicon fertilizer material, as frit
[1].In recent years, blast-furnace slag is also for the preparation of alkali-activated slag base geological polymer
[2-4].In addition, Zhang Yaojun
[5,6]deng Chinese patent application (patent No.: ZL201210166585.5, ZL201210166597.8) disclose chemi-excitation slag-based composite gelled material for dyestuff degraded and new forms of energy research.In recent years, some patent documentations disclose and have utilized solid waste preparation to have mechanical large pore material; As true in spreading out
[7]deng Chinese patent (CN101708399A) a kind of porous slag filtrate and preparation method thereof is disclosed, according to slag 30-80%, clay 15-50%, pore former 5-20% (coal gangue, starch, sawdust, calcium carbonate, wherein a kind of) raw material weight per-cent stirs, spread water moulding and make raw material ball, drying, 400-700oC thermal pretreatment, then in 1000-1300oC roasting, obtain porous slag filtrate, this patent has been reported and adopted the characteristic of grain slag filtering material prepared by the method is porous, and aperture is large.Nest opens
[8]deng Chinese patent (CN102603355A) a kind of base geopolymer porous material is disclosed, 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, redispersable latex powder 0.3-1.0 part that ethylene copolymer rubber powder forms) and composite foamable agent (composite foamable agent is comprised 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) according to the ratio of weight ratio 9-38:1, combine, foaming block intensity prepared by this application between 0.5-8MPa, the method complexity of drawing materials, the material of preparation has the feature of macroscopical macropore.Field is for army building
[9]deng Chinese patent application (CN 102584318 A) disclose and a kind ofly containing Cr slag, prepared the method for porous insulation material, this invents to contain Cr slag, flyash is raw material, cullet, clay and wilkinite are binding agent, Wingdale, SiC, carbon dust, paraffin, stearic acid, organic fibre and millet are expanding agent, mass ratio 40%-70% is contained to Cr slag, 10%-40% binding agent and 5%-30% pore-forming material, by fragmentation, batch mixing, be shaped, demoulding 700-1300 ℃ sintering, in the scanning electron microscope picture providing from Patent Application Publication, utilizing what obtain after 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)
[10], can be divided into poromerics (aperture is less than 2nm), mesoporous material (aperture is between 2～50nm) and large pore material (aperture is greater than 50nm) according to large young pathbreaker's porous material in aperture.Because hole is different in the arranged distribution feature in space, mesoporous material can be divided into again two kinds of order and disorder
[11].Utilizing cats product is the classical way of synthetic M41S series ordered mesoporous material as template
[12,13]and sol-gel method is the typical method of the unordered oxide mesoporous material of preparation.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, by a large amount of literature retrievals and domestic and international new patent searching thereof, finds the document and the patent report that utilize solid waste slag to prepare mesoporous material.
Below the main reference that contriver provides:
[1] Cao Deqiu, Li Canhua, China's blast-furnace slag recycling progress, Chinese iron and steel scrap 5 (2006) 26-29.
[2]J?Davidovits.Geopolymers:inorganic?polymeric?new?materials,Journal?of?Thermal?Analysis?37(1991)1633-1656。
[3] Zhang Shuzheng, Gong Kecheng, geopolymer, Materials Science and Engineering journal 21 (3) (2003) 430-436.
[4] Wang Feng, Zhang Yaojun, the research of NaOH alkali-activated slag geopolymer, nonmetalliferous ore 31 (3) (2008) 9-11.
[5] Zhang Yaojun, Liu Licai, Ni Lulu, Wang Bingli, Wang Yachao, bavin is pretty, Jing Dongsheng, Gu Xiaoze, Liu Peiyao, slag-based gelling material-ferric oxide semi-conductor composite catalyst and the application in solar energy photocatalytic hydrogen production by water decomposition, the patent No.: ZL201210166585.5.
[6] Zhang Yaojun, Liu Licai, Ni Lulu, Wang Bingli, Wang Yachao, slag-based inorganic polymer-ferric oxide semi-conductor composite catalyst and the application in dyestuff degraded, the patent No.: ZL201210166597.8.
[7] 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.
[8] nest opens, Liu Haifeng, a kind of base geopolymer porous material, publication number: CN02603355A.
[9] field is for army building, opens dark, Zhang Jing, Pan Dean, Liu Bo, a kind of method of preparing porous insulation material containing Cr slag, publication number: CN102584318A.
[10]D.H.Everett,IUPAC?manual?of?symbols?and?terminology,Pure?and?Applied?Chemistry?31(1972)578-638。
[11]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?Society?121(1999)254-255。
[12]J.S.Beck，J.E.Vartwli，et?a1.，A?new?family?of?mesoporous?molecular?sieves?prepared?with?liquid-crystal?template?mechanism，Journal?of?the?American?Chemical?Society?114(1992)10834-10843。
[13]G.T.Kresge,M.E.Leonowica，et?a1.，Ordered?mesoporous?molecular?sieves?synthesized?by?liquid-crystal?template?mechanism,Nature?359(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-based mesoporous material making is raw material slag, sodium hydroxide water and pore forming agent glucose to be put into whipping appts carry out mix, through mould molding, maintenance and roasting thereof, form, the add-on of sodium hydroxide and pore forming agent glucose be take slag quality as basis; The add-on of sodium hydroxide is 6% of slag quality; Pore forming agent glucose addition is the 3%-6% of slag quality, and the addition of water and slag mass ratio are 0.24-0.28.
Above-mentioned slag-based mesoporous material and preparation method thereof, is characterized in that, comprises the following steps:
(1) by formula ratio, take slag powders and water; The mass ratio of water and slag powders is: 0.24-0.28;
(2) press formula ratio weighing sodium hydroxide, and dissolved in and in suitable quantity of water, form aqueous sodium hydroxide solution;
(3) by formula, take pore forming agent glucose, and dissolved in and in suitable quantity of water, form D/W;
(4) under room temperature, aqueous sodium hydroxide solution is poured in stirred vessel, then pore forming agent D/W is added, then slag powders is added and carry out mix, form slurry;
(5) pack slurry into die for molding, maintenance 6h under 80 ℃ of conditions of thermostat container, form removal after naturally cooling, curing room natural curing 1 day, obtains the test block of slag-based gelling material.
(6) test block of slag-based gelling material is put into muffle furnace and be warming up to 450 ℃ with the temperature rise rate of 5 ℃/min, after insulation 4h, make to take out after its naturally cooling, obtain a kind of slag-based mesoporous material.
The technique effect that slag-based mesoporous material prepared by the present invention brings is:
(1) can promote the recycling economy development of iron work, for disposable, completely innoxious, high added value, mass-producing, the recycling of slag provides a new way.
(2) raw material is cheap and easy to get, and technological process is simple, without slag is carried out to pre-treatment, three-waste free discharge, environmental protection; Can realize the controlled preparation of mesoporous material.
(3) the slag-based mesoporous material of preparing has high ultimate compression strength, can meet the demand to mesoporous material such as catalyzer and sorbent material.
Innovation of the present invention is:
Propose to using glucose and as pore forming agent, prepared the novel method of slag-based mesoporous material; Meanwhile, by control, increase dosage and the maturing temperature in aperture, to realize the controlled preparation of slag-based mesoporous material, enrich the kind of mesoporous material.Compare with the sample without pore forming agent, add after the pore forming agent of optimum quantity, the mesoporous volume of sample can net increase 102.63%.
Accompanying drawing explanation
Fig. 1 is technical process prepared by slag-based mesoporous material;
Fig. 2 is the pore size distribution curve that BET method detects slag-based mesoporous material;
Fig. 3 is the thermal analysis curve of glucose;
Below in conjunction with drawings and Examples, the present invention is described in further detail.
Embodiment
The inventor's technical thought is, take solid waste slag as raw material, take glucose as pore forming agent, by modulation preparation condition, especially by dosage and the maturing temperature of modulation pore forming agent, to realize the controlled preparation of slag-based mesoporous material, enrich the kind of mesoporous material.Meanwhile, this preparation process processing requirement is simple, without slag is carried out to pre-treatment, can the completely disposable slag that utilizes, and for the high value added utilization of slag and the recycling economy of iron and steel enterprise, have great importance.
Fig. 1 has provided technological process block-diagram prepared by slag-based mesoporous material; In following embodiment, preparing the main raw material(s) that slag-based mesoporous material adopts has industrial solid castoff slag, sodium hydroxide; Glucose, specific performance is as follows:
1, slag:
Slag, from Hancheng Long Gang company, is put into 110 ℃ of constant temperature drying 3h of baking oven by slag, and through ball milling 2 hours, density was 2.82g/cm
3, Blain specific surface is 520m
2/ kg.
The main oxides of slag forms (mass percent): SiO
2(30.01%), Al
2o
3(11.98%), CaO (37.39%), MgO (8.20%), Fe
2o
3(0.25%), TiO
2(1.17%), SO
3(1.30%), Na
2o (0.64%), K
2o (0.83%) other (8.23%).
2, sodium hydroxide
Sodium hydroxide is purchased from Tianjin Jin Dong Tian Zheng fine chemistry chemical reagent work, is analytical reagent.
3, glucose
Glucose is purchased from Tianjin Jin Dong Tian Zheng fine chemistry chemical reagent work, is analytical reagent.
4, adopt BET method to detect the pore size distribution of slag-based mesoporous material.
Be the embodiment that contriver provides below, it should be noted that, these embodiment only for a better understanding of the present invention, the invention is not restricted to these embodiment.
Embodiment 1:
Accurately weigh slag powders 600g, as measurement basis (100%); Adopt outer doping, sodium hydroxide volume is 6% of slag powders quality, and water and slag powders mass ratio are 0.28.
At room temperature, sodium hydroxide is dissolved in water, form aqueous sodium hydroxide solution.This aqueous solution is poured into and two turned double speed and only starch in stirrer, add again slag powders to carry out mix, form even slurry, pack slurry into 31.5mm * 31.5mm * 50mm steel three die for molding, three gang mould tools are put into plastics film sealing bag, under 80 ℃ of conditions of thermostat container, maintenance is 6 hours, form removal after cooling, room temperature maintenance 1 day, obtains the test block of slag-based gelling material, and detecting its ultimate compression strength is 41MPa.
This slag-based gelling material test block is put into muffle furnace, with the temperature rise rate of 5 ℃/min, be warming up to 450 ℃, insulation 4h, makes to take out after its naturally cooling, obtains slag-based gelatinous material, and detecting its ultimate compression strength is 65.8MPa; BET method detects the pore size distribution of sample, and result is as shown in table 1 and Fig. 2, and as can be seen from Table 1, the mesoporous volume of slag-based gelling material is 0.048956 (mL/g).
Table 1:BET method detects the pore size distribution result of sample
Embodiment 2:
Accurately weigh slag powders 600g, as measurement basis (100%); Adopt outer doping, sodium hydroxide volume is 6% of slag powders quality, and pore forming agent glucose volume is 3% of slag quality, and water and slag powders mass ratio are 0.24.At room temperature, sodium hydroxide is water-soluble, form aqueous sodium hydroxide solution; Solid glucose is dissolved in water, form D/W.Aqueous sodium hydroxide solution and D/W are poured into successively and twoly turned double speed and only starch in stirrer, add again slag powders to carry out mix, the slurry that formation mixes, pack slurry into 31.5mm * 31.5mm * 50mm steel three die for molding, three gang mould tools are put into plastics film sealing bag, under 80 ℃ of conditions of thermostat container, maintenance is 6 hours, cooling form removal, after room temperature maintenance 1 day, obtain the test block of slag-based gelling material, detecting its ultimate compression strength is 60.7MPa.
This slag-based gelling material test block obtaining is put into muffle furnace, with the temperature rise rate of 5 ℃/min, be warming up to 450 ℃, after insulation 4h, make to take out after its naturally cooling, obtain slag-based mesoporous material, detecting its ultimate compression strength is 80.3MPa; BET method detects the pore size distribution of sample, and result is as shown in table 1 and Fig. 2, and as can be seen from Table 1, the mesoporous volume of slag-based mesoporous material is 0.080229 (mL/g).Than the mesoporous volume that does not add the slag-based gelling material of pore forming agent, increased by 0.031273 (mL/g), the mesoporous percent by volume of increase is 63.87%; Meanwhile, as can be seen from Figure 2, the area under the curve that is less than 50nm aperture significantly increases.
The maturing temperature of preparing slag-based mesoporous material is chosen for the selection reason of 450 ℃, take weight loss (%) in the thermal analysis curve of Fig. 3 glucose and the weightless maximum temperature 312oC in differential thermogravimetric curve is foundation, in order to ensure glucose, decomposing completely, is the complete decomposition temperature of glucose therefore select 450 ℃.
Embodiment 3:
Accurately weigh slag powders 600g, as measurement basis (100%); Adopt outer doping, sodium hydroxide volume is 6% of slag powders quality, and pore forming agent glucose volume is 6% of slag quality, and water and slag powders mass ratio are 0.24.At room temperature, solid sodium hydroxide is dissolved in water, form aqueous sodium hydroxide solution.Solid glucose is dissolved in water, form D/W.Aqueous sodium hydroxide solution and D/W are added successively and twoly turn double speed and only starch in stirrer, add again slag powders to carry out mix, the slurry that formation mixes, pack slurry into 31.5mm * 31.5mm * 50mm steel three die for molding, three gang mould tools are put into plastics film sealing bag, under 80 ℃ of conditions of thermostat container, maintenance is 6 hours, cooling form removal, after room temperature maintenance 1 day, obtain slag-based gelling test block, detecting its ultimate compression strength is 54.6MPa.
This slag-based gelling test block is put into muffle furnace, with the temperature rise rate of 5 ℃/min, be warming up to 450 ℃, after insulation 4h, make to take out after its naturally cooling, obtain slag-based mesoporous material, detecting its ultimate compression strength is 90.4MPa; BET 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 mesoporous volume of slag-based mesoporous material is 0.099200 (mL/g), than the mesoporous volume of not mixing the slag-based gelling material of pore forming agent, increased by 0.050244 (mL/g), the mesoporous percent by volume of increase is 102.63%; Meanwhile, as can be seen from Figure 2, the area under the curve in 2nm-50nm aperture significantly increases, and it can amass aperture significantly to mesoporous direction displacement.Show, as long as control pore forming agent glucose dosage and maturing temperature and temperature rise rate, just can realize the controlled preparation of slag-based mesoporous material.
Embodiment 4:
The slag-based mesoporous material that the embodiment 3 of usining makes is as support of the catalyst, and the tungstic oxide of load 5% mass percent is as catalyzer.
Accurately take 0.4 gram of above-mentioned catalyzer, under magnetic agitation, put it in the beaker of the purple aqueous solution of 4mg/L alkalescence that fills 100mL, the aqueous solution with simulation visible light source (500W xenon lamp) from the vertical irradiation beaker in top of beaker, carry out the photocatalytic degradation of dyestuff, irradiation 70 minutes, detecting the purple degradation rate of alkalescence is 97%; And under identical condition, pure tungstic oxide is 60% to the purple degradation rate of alkalescence; Show that slag-based mesoporous material has high visible light catalysis activity as support of the catalyst.
Claims (4)
1. a slag-based mesoporous material, it is characterized in that, this slag-based mesoporous material making is raw material slag, sodium hydroxide water and pore forming agent glucose to be put into whipping appts carry out mix, through mould molding, maintenance and roasting thereof, form, the add-on of sodium hydroxide and pore forming agent glucose be take slag quality as basis; The add-on of sodium hydroxide is 6% of slag quality; Pore forming agent glucose addition is the 3%-6% of slag quality, and the addition of water and slag mass ratio are 0.24-0.28.
2. slag-based mesoporous material as claimed in claim 1, is characterized in that, the main oxides mass percent of described slag consists of: SiO
2: 30.01%, Al
2o
3: 11.98%, CaO:37.39%, MgO:8.20%, Fe
2o
3: 0.25%, TiO
2: 1.17%, SO
3: 1.30%, Na
2o:0.64%, K
2o:0.83%, other: 8.23%.
3. the preparation method of the slag-based mesoporous material described in claim 1 or 2, is characterized in that, comprises the following steps:
(1) by formula ratio, take slag powders and water; The mass ratio of water and slag powders is: 0.24-0.28;
(2) press formula ratio weighing sodium hydroxide, and dissolved in and in suitable quantity of water, form aqueous sodium hydroxide solution;
(3) by formula, take pore forming agent glucose, and dissolved in and in suitable quantity of water, form D/W;
(4) under room temperature, aqueous sodium hydroxide solution is poured in stirred vessel, then D/W is added, then slag powders is added and carry out mix, form slurry;
(5) pack slurry into die for molding, maintenance 6h under 80 ℃ of conditions of thermostat container, form removal after naturally cooling, curing room natural curing 1 day, obtains the test block of slag-based gelling material;
(6) test block of slag-based gelling material is put into muffle furnace and be warming up to 450 ℃ with the temperature rise rate of 5 ℃/min, after insulation 4h, make to take out after its naturally cooling, obtain slag-based mesoporous material.
4. the slag-based mesoporous material described in claim 1 or 2 is for the application of support of the catalyst.
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105693265A (en) * | 2016-01-11 | 2016-06-22 | 中国计量学院 | Method for preparing aluminum oxide based porous ceramic membrane |
| CN106345219A (en) * | 2016-09-08 | 2017-01-25 | 北京神雾环境能源科技集团股份有限公司 | Method for preparing air purification components from calcium carbide furnace gas dust and product of method |
| CN106994327A (en) * | 2017-04-18 | 2017-08-01 | 内蒙古师范大学 | A kind of method of modifying of blast furnace slag |
| CN110734277A (en) * | 2019-08-23 | 2020-01-31 | 福建贝迪陶瓷科技有限公司 | artificial corallite formula and its making process |
| CN111892422A (en) * | 2020-07-22 | 2020-11-06 | 西安理工大学 | Preparation method of porous sound absorption and noise reduction ceramic |
| JP2021127280A (en) * | 2020-02-14 | 2021-09-02 | 国立大学法人大阪大学 | Metal oxide composite and its production method, and method of separating carbon dioxide |
| CN118459151A (en) * | 2024-07-10 | 2024-08-09 | 常熟理工学院 | Method for preparing porous filter material by using blast furnace slag and application |
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| WO2011068830A2 (en) * | 2009-12-01 | 2011-06-09 | Arizona Board Of Regents For And On Behalf Of Arizona State University | Porous geopolymer materials |
| CN102671664A (en) * | 2012-05-25 | 2012-09-19 | 西安建筑科技大学 | Slag-based cementitious material-iron oxide semi-conductor composite catalyst and application in solar photocatalytic hydrogen production through water decomposition |
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Cited By (10)
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|---|---|---|---|---|
| CN105693265A (en) * | 2016-01-11 | 2016-06-22 | 中国计量学院 | Method for preparing aluminum oxide based porous ceramic membrane |
| CN105693265B (en) * | 2016-01-11 | 2018-04-20 | 中国计量学院 | A kind of method for preparing alumina oxide matrix porous ceramic membrane |
| CN106345219A (en) * | 2016-09-08 | 2017-01-25 | 北京神雾环境能源科技集团股份有限公司 | Method for preparing air purification components from calcium carbide furnace gas dust and product of method |
| CN106994327A (en) * | 2017-04-18 | 2017-08-01 | 内蒙古师范大学 | A kind of method of modifying of blast furnace slag |
| CN110734277A (en) * | 2019-08-23 | 2020-01-31 | 福建贝迪陶瓷科技有限公司 | artificial corallite formula and its making process |
| JP2021127280A (en) * | 2020-02-14 | 2021-09-02 | 国立大学法人大阪大学 | Metal oxide composite and its production method, and method of separating carbon dioxide |
| CN111892422A (en) * | 2020-07-22 | 2020-11-06 | 西安理工大学 | Preparation method of porous sound absorption and noise reduction ceramic |
| CN111892422B (en) * | 2020-07-22 | 2022-07-15 | 西安理工大学 | Preparation method of porous sound-absorbing noise-reducing ceramic |
| CN118459151A (en) * | 2024-07-10 | 2024-08-09 | 常熟理工学院 | Method for preparing porous filter material by using blast furnace slag and application |
| CN118459151B (en) * | 2024-07-10 | 2024-10-18 | 常熟理工学院 | Method for preparing porous filter material by using blast furnace slag and application |
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|---|---|
| CN104163615B (en) | 2016-02-03 |
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