CN103861556A - Mesoporous material preparation method using fly ash - Google Patents
Mesoporous material preparation method using fly ash Download PDFInfo
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- CN103861556A CN103861556A CN201210549598.0A CN201210549598A CN103861556A CN 103861556 A CN103861556 A CN 103861556A CN 201210549598 A CN201210549598 A CN 201210549598A CN 103861556 A CN103861556 A CN 103861556A
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Abstract
The invention belongs to the field of waste reutilization, and relates to a preparation method of fly-ash-based SBA-15, and the preparation method comprises the following steps: firstly, mixing fly ash and an alkali, then melting, and cooling to obtain a mixture; then adding distilled water into the mixture for dissolving, filtering to take supernatant for standby use, wherein the supernatant is an aluminosilicate solution; then, dissolving surfactant P123 in the distilled water, regulating the pH to acidic, fully stirring; then aging, filtering, washing, drying, roasting and cooling to obtain the powder-like mesoporous material fly-ash-based SBA-15. The fly-ash-based SBA-15 prepared by the method has a regular two-dimensional hexagonal structure, has a pore volume of 0.6-0.9cm<3>/g, a specific surface area as high as 800m<2>/g, and a pore diameter of 5-8nm. The method is simple, and is less in environment pollution due to use of effective components in waste as a silicon source.
Description
Technical field
The invention belongs to changing rejected material to useful resource field, relate to a kind of method of preparing fly ash base SBA-15.
Background technology
Flyash (CFA) is mainly derived from the fine grained dispersed residue after coal-burning power plant's pulverized coal friring.Utilize flyash as raw material, prepare porous material and be one of important channel that recent domestic utilizes fly ash development high value added product.Utilize the standby porous material of coal ash for manufacturing to have active carbon, zeolite etc., the Chinese patent application " producing the new technology of active carbon with flyash " that is 200810143173.3 as application number proposes from flyash, to utilize the means such as FLOTATION SEPARATION to isolate carbon particle, then obtains active carbon through multiple subsequent treatment process.But, utilize the method complex process loaded down with trivial details, the drawback such as consume energy high, with high costs, has limited its application.The Chinese patent application " a kind of method of preparing nano flyash zeolite " that and for example application number is 201010568082.1 proposes by hydro-thermal legal system for zeolite, can be used for the fields such as absorption, catalysis, but the method needs hydrothermal treatment consists, severe reaction conditions, production efficiency is low, can not be used for suitability for industrialized production.The preparation of meso pore silicon oxide material, normally take surfactant (block copolymer etc.) as structure directing agent, ethyl orthosilicate (TEOS) is silicon source, application number is that the Chinese patent application " a kind of method of novel control mesoporous material aperture and pitch of holes " of CN200910238389.2 proposes take TEOS as silicon source, preparation bulk mesoporous material.But active ingredient Si relative amount is low in TEOS, prepare mesoporous material take it as raw material and will inevitably make cost increase, be unfavorable for suitability for industrialized production.The Chinese patent application " having the synthetic method of the SBA-15 molecular sieve of Adsorption of Organic performance " that and for example application number is CN200910307921.1 also proposes to utilize TEOS for preparing the application of SBA-15 mesopore molecular sieve and adsorb organic compound aspect in silicon source.The cost of same material strengthens, and has limited the possibility of its large-scale production.
Summary of the invention
The defect the object of the invention is to for overcoming prior art provides a kind of method of coal ash for manufacturing for mesoporous material of utilizing.The method is a kind of method of the mesoporous material that is produced on a large scale of saving the energy, reduce production costs, and prepares sorbing material take coal-burning power plant's discarded object flyash under raw material room temperature.Both can solve the environmental problem that fine coal dust heap is abandoned and caused by it, can turn waste into wealth again, realize the resource of flyash.
For achieving the above object, the present invention is by the following technical solutions:
A preparation method of fly ash base SBA-15, comprises following steps:
(1) first, flyash and alkali are mixed to rear melting, cooling, obtain compound;
(2) then, add distilled water to dissolve in compound, cross leaching supernatant stand-by, wherein supernatant is aluminosilicate solution;
(3) then, surfactant P123 is dissolved in distilled water, it is acid regulating pH, fully stirs; Aging, and filter, wash, dry;
(4) last, by the dried material calcination of step (3), obtain Powdered mesoporous material fly ash base SBA-15(SBA-15-CFA after cooling).
Alkali in described step (1) is NaOH or potassium hydroxide, and wherein the mass ratio of flyash and NaOH is 1:(1 ~ 1.3), the mass ratio of flyash and potassium hydroxide is 1:(1.4 ~ 1.8).
In described step (1), be melted in Muffle furnace and carry out, temperature is 500 ℃ ~ 600 ℃, and the melting time is 1 ~ 2h, naturally cooling with stove.
In described step (3), adding 2M HCl to pH is 0.3～1.0.
In described step (3), in precursor liquid, the mol ratio of each material is n(Si): n(P123): n(HCl): n(H
2o)=1:0.016:(5.4 ~ 24.5): (200 ~ 700), wherein P123 is a kind of triblock copolymer, full name is: PEO-PPOX-PEO triblock copolymer, its molecular formula is: PEO-PPO-PEO.
In described step (3), whipping temp is 35 ~ 40 ℃, and rotating speed is 100 ~ 1000rpm.
In described step (3), aging temperature is 95 ℃, and ageing time is 24h, agingly in baking oven, carries out.
In described step (4), sintering temperature is 550 ℃, roasting time 5h, and heating rate is 1 ℃/min.
The pore volume of mesoporous material SBA-15-CFA that described step (4) makes is 0.6 ~ 0.9cm
3/ g, specific area is 370 ~ 810m
2/ g, aperture is 5 ~ 8nm.
The invention provides the method for preparing mesoporous material take flyash as raw material.This preparation method is simple to operate, with low cost, and the utilization rate of raw material is high, can be the active ingredient in sorbing material by conversions such as the silicon in flyash, reaches the object of solid waste resource.
Compared with preparing mesoporous material with traditional Ash Utilization, advantage of the present invention is apparent.Utilize flyash both to provide cost savings, thereby effectively utilized again the multicomponent element preparation in flyash to there is the mesoporous material of excellent properties, and eliminated the harm of dangerous component to environment in flyash.In addition, in the preparation of mesoporous material, without harsh conditions such as hydro-thermals, only need at 40 ℃, carry out.Utilize the present invention can realize the resource of flyash discarded object.Method energy consumption of the present invention is low, environmental protection, quick, efficient, can realize suitability for industrialized production.
Accompanying drawing explanation
Fig. 1 is the SEM photo of sorbing material in the embodiment of the present invention, and wherein figure (a) is low power (10K) SEM photo, and figure b is high power (80K) SEM photo.
Fig. 2 is the TEM photo of sorbing material in the embodiment of the present invention, and wherein scheming a is the TEM photo along [001] direction of two-dimentional hexagonal structure, and figure b is the TEM photo along [110] direction of two-dimentional hexagonal structure.
The specific embodiment
Further illustrate the present invention below in conjunction with embodiment and accompanying drawing.
Embodiment 1
(1) first, at 500 ℃ of melting 1h, cooling after flyash and NaOH (mass ratio is 1:1) are mixed, obtain compound;
(2) then, add distilled water to dissolve in compound, cross leaching supernatant stand-by, wherein supernatant is aluminosilicate solution;
(3) surfactant P123 is dissolved in distilled water, adding 2M HCl to pH is 0.9, and in mixed precursor liquid, the mol ratio of each material is 1Si:0.016P123:5.4HCl:200H
2o fully stirs at 35 ~ 40 ℃; In 95 ℃ of baking ovens, leave standstill after aging 24h, filter, wash, dry;
(4) last, by dried material 550 ℃ of roastings, roasting time 5h, heating rate is 1 ℃/min, obtains Powdered mesoporous material after cooling.
Embodiment 2
(1) first, at 550 ℃ of melting 1.5h, cooling after flyash and NaOH (mass ratio is 1:1.2) are mixed, obtain compound;
(2) then, add distilled water to dissolve in compound, cross leaching supernatant stand-by, wherein supernatant is aluminosilicate solution;
(3) surfactant P123 is dissolved in distilled water, adding 2M HCl to pH is 0.6, and in mixed precursor liquid, the mol ratio of each material is 1Si:0.016P123:17.3HCl:200H
2o fully stirs at 35 ~ 40 ℃; In 95 ℃ of baking ovens, leave standstill after aging 24h, filter, wash, dry;
(4) last, by dried material 550 ℃ of roastings, roasting time 5h, heating rate is 1 ℃/min, obtains Powdered mesoporous material after cooling.
Embodiment 3
(1) first, at 600 ℃ of melting 2h, cooling after flyash and NaOH (mass ratio is 1:1.3) are mixed, obtain compound; (2) then, add distilled water to dissolve in compound, cross leaching supernatant stand-by, wherein supernatant is aluminosilicate solution;
(3) surfactant P123 is dissolved in distilled water, adding 2M HCl to pH is 0.3, and in mixed precursor liquid, the mol ratio of each material is 1Si:0.016P123:24.5HCl:200H
2o fully stirs at 35 ~ 40 ℃; In 95 ℃ of baking ovens, leave standstill after aging 24h, filter, wash, dry;
(4) last, by dried material 550 ℃ of roastings, roasting time 5h, heating rate is 1 ℃/min, obtains Powdered mesoporous material after cooling.
Fig. 1 is the SEM photo of SBA-15-CFA in embodiment 3, and wherein figure (a) is low power (10K) SEM photo, and figure b is high power (80K) SEM photo.Fig. 2 is the TEM photo of sorbing material in the embodiment of the present invention, and wherein figure (a) is the TEM photo along [001] direction of two-dimentional hexagonal structure, and figure (b) is the TEM photo along [110] direction of two-dimentional hexagonal structure.Can be found out by Fig. 1 (a), the mesoporous material SBA-15-CFA synthesizing is wheat head shape, can find out that from Fig. 1 (b) SBA-15-CFA has regular pore passage structure.The transmission electron microscope photo along [001] direction in Fig. 2 (a) demonstrates the pore passage structure of orderly hexagonal array, and the transmission electron microscope photo along [110] direction in Fig. 2 (b) demonstrates large-scale ordered arrangement strip structure.In conjunction with Fig. 1 and Fig. 2, can illustrate that the mesoporous material SBA-15-CFA of synthesized has orderly two-dimentional hexagonal structure.
The structural characterization data of the SBA-15-CFA that table 1 makes for embodiment 1-3.
Table 1
| ? | Specific area (m 2/g） | Aperture (nm) | Pore volume (cm 3/g） |
| Embodiment 1 | 373.68 | 5.2 | 0.61 |
| Embodiment 2 | 519.94 | 6.5 | 0.70 |
| Embodiment 3 | 806.13 | 7.2 | 0.82 |
The above-mentioned description to embodiment is can understand and apply the invention for ease of those skilled in the art.Person skilled in the art obviously can easily make various modifications to these embodiment, and General Principle described herein is applied in other embodiment and needn't passes through performing creative labour.Therefore, the invention is not restricted to the embodiment here, those skilled in the art are according to announcement of the present invention, and not departing from the improvement that category of the present invention makes and revise all should be within protection scope of the present invention.
Claims (9)
1. a preparation method of fly ash base SBA-15, is characterized in that: comprise following steps:
(1) first, flyash and alkali are mixed to rear melting, cooling, obtain compound;
(2) then, add distilled water to dissolve in compound, cross leaching supernatant stand-by, wherein supernatant is aluminosilicate solution;
(3) then, surfactant P123 is dissolved in distilled water, it is acid regulating pH, fully stirs; Then aging, and filter, wash, dry;
(4) last, by the dried material calcination of step (3), obtain Powdered mesoporous material fly ash base SBA-15 after cooling.
2. method according to claim 1, it is characterized in that: the alkali in described step (1) is NaOH or potassium hydroxide, wherein the mass ratio of flyash and NaOH is 1:(1 ~ 1.3), the mass ratio of flyash and potassium hydroxide is 1:(1.4 ~ 1.8).
3. method according to claim 1, is characterized in that: in described step (1), be melted in Muffle furnace and carry out, temperature is 500 ℃ ~ 600 ℃, and the melting time is 1 ~ 2h, naturally cooling with stove.
4. method according to claim 1, is characterized in that: in described step (3), adding 2M HCl to pH is 0.3 ~ 1.0.
5. method according to claim 1, is characterized in that: in described step (3), in precursor liquid, the mol ratio of each material is n(Si): n(P123): n(HCl): n(H
2o)=1:0.016:(5.4 ~ 24.5): (200 ~ 700).
6. method according to claim 1, is characterized in that: in described step (3), whipping temp is 35 ~ 40 ℃, and rotating speed is 100 ~ 1000rpm.
7. method according to claim 1, is characterized in that: in described step (3), aging temperature is 95 ℃, and ageing time is 24h, agingly in baking oven, carries out.
8. method according to claim 1, is characterized in that: in described step (4), sintering temperature is 550 ℃, roasting time 5h, and heating rate is 1 ℃/min.
9. method according to claim 1, is characterized in that: the pore volume of mesoporous material SBA-15-CFA that described step (4) makes is 0.6 ~ 0.9cm
3/ g, specific area is 370 ~ 810m
2/ g, aperture is 5 ~ 8nm.
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Cited By (13)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105214636A (en) * | 2015-09-30 | 2016-01-06 | 王立鹏 | Modification drift sand biodiesel catalyst and its preparation method and application |
| CN106622115A (en) * | 2016-12-30 | 2017-05-10 | 华南农业大学 | Potassium type heavy metal mesoporous adsorption material with molybdenum ore tailings as raw material, and preparation method and application thereof |
| CN106669591A (en) * | 2017-01-20 | 2017-05-17 | 贵州省材料产业技术研究院 | Treatment method for adsorbing xanthate in wastewater |
| CN107930576A (en) * | 2017-11-27 | 2018-04-20 | 吉林大学 | A kind of preparation method of fly ash micro-sphere porous material and obtained porous material |
| CN108745272A (en) * | 2018-06-15 | 2018-11-06 | 福建工程学院 | A kind of method that flyash directly prepares Jie's microporous adsorbent material |
| CN108816180A (en) * | 2018-06-15 | 2018-11-16 | 福建工程学院 | Trap the preparation method of Jie's microporous adsorbent material of carbon dioxide |
| CN108928829A (en) * | 2017-05-24 | 2018-12-04 | 神华集团有限责任公司 | SBA-15 mesopore molecular sieve and its preparation method and application |
| CN108946754A (en) * | 2017-05-24 | 2018-12-07 | 神华集团有限责任公司 | SBA-15 mesopore molecular sieve and preparation method and application and flyash produce the method for aluminium oxide and SBA-15 mesopore molecular sieve |
| CN110124727A (en) * | 2018-02-02 | 2019-08-16 | 神华集团有限责任公司 | The method of fly ash base denitrating catalyst and preparation method thereof and denitration |
| CN110668458A (en) * | 2018-07-02 | 2020-01-10 | 国家能源投资集团有限责任公司 | Al-SBA-15 mesoporous molecular sieve, denitration catalyst, preparation methods of Al-SBA-15 mesoporous molecular sieve and denitration catalyst, and application of Al-SBA-15 mesoporous molecular sieve and denitration catalyst |
| CN112023872A (en) * | 2020-08-26 | 2020-12-04 | 昆明理工大学 | Method for synthesizing mesoporous silicon-aluminum composite material by using high-alumina fly ash |
| CN113620659A (en) * | 2020-05-08 | 2021-11-09 | 中联环股份有限公司 | Method for preparing non-autoclaved hydrophobic fiber reinforced calcium silicate board by utilizing fly ash |
| CN113976095A (en) * | 2021-11-29 | 2022-01-28 | 刘磊 | Preparation method of waste polymethyl methacrylate catalytic cracking catalyst |
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Cited By (18)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN105214636A (en) * | 2015-09-30 | 2016-01-06 | 王立鹏 | Modification drift sand biodiesel catalyst and its preparation method and application |
| CN105214636B (en) * | 2015-09-30 | 2019-02-26 | 榆林学院 | Modified drift sand biodiesel catalyst and its preparation method and application |
| CN106622115A (en) * | 2016-12-30 | 2017-05-10 | 华南农业大学 | Potassium type heavy metal mesoporous adsorption material with molybdenum ore tailings as raw material, and preparation method and application thereof |
| CN106622115B (en) * | 2016-12-30 | 2019-05-07 | 华南农业大学 | It is a kind of based on the potassium type heavy metal mesoporous adsorption material and its preparation method and application that molybdenum ore tailings is raw material |
| CN106669591A (en) * | 2017-01-20 | 2017-05-17 | 贵州省材料产业技术研究院 | Treatment method for adsorbing xanthate in wastewater |
| CN106669591B (en) * | 2017-01-20 | 2019-06-11 | 贵州省材料产业技术研究院 | It is a kind of for adsorbing the processing method of xanthate in waste water |
| CN108946754B (en) * | 2017-05-24 | 2021-02-26 | 神华集团有限责任公司 | SBA-15 mesoporous molecular sieve, preparation method and application thereof, and method for producing alumina and SBA-15 mesoporous molecular sieve from fly ash |
| CN108928829A (en) * | 2017-05-24 | 2018-12-04 | 神华集团有限责任公司 | SBA-15 mesopore molecular sieve and its preparation method and application |
| CN108946754A (en) * | 2017-05-24 | 2018-12-07 | 神华集团有限责任公司 | SBA-15 mesopore molecular sieve and preparation method and application and flyash produce the method for aluminium oxide and SBA-15 mesopore molecular sieve |
| CN107930576A (en) * | 2017-11-27 | 2018-04-20 | 吉林大学 | A kind of preparation method of fly ash micro-sphere porous material and obtained porous material |
| CN107930576B (en) * | 2017-11-27 | 2021-06-04 | 吉林大学 | Preparation method of fly ash microbead porous material and prepared porous material |
| CN110124727A (en) * | 2018-02-02 | 2019-08-16 | 神华集团有限责任公司 | The method of fly ash base denitrating catalyst and preparation method thereof and denitration |
| CN108745272A (en) * | 2018-06-15 | 2018-11-06 | 福建工程学院 | A kind of method that flyash directly prepares Jie's microporous adsorbent material |
| CN108816180A (en) * | 2018-06-15 | 2018-11-16 | 福建工程学院 | Trap the preparation method of Jie's microporous adsorbent material of carbon dioxide |
| CN110668458A (en) * | 2018-07-02 | 2020-01-10 | 国家能源投资集团有限责任公司 | Al-SBA-15 mesoporous molecular sieve, denitration catalyst, preparation methods of Al-SBA-15 mesoporous molecular sieve and denitration catalyst, and application of Al-SBA-15 mesoporous molecular sieve and denitration catalyst |
| CN113620659A (en) * | 2020-05-08 | 2021-11-09 | 中联环股份有限公司 | Method for preparing non-autoclaved hydrophobic fiber reinforced calcium silicate board by utilizing fly ash |
| CN112023872A (en) * | 2020-08-26 | 2020-12-04 | 昆明理工大学 | Method for synthesizing mesoporous silicon-aluminum composite material by using high-alumina fly ash |
| CN113976095A (en) * | 2021-11-29 | 2022-01-28 | 刘磊 | Preparation method of waste polymethyl methacrylate catalytic cracking catalyst |
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Application publication date: 20140618 |