CN102908993A - Preparation method of porous adsorbent - Google Patents
Preparation method of porous adsorbent Download PDFInfo
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- CN102908993A CN102908993A CN2012104108853A CN201210410885A CN102908993A CN 102908993 A CN102908993 A CN 102908993A CN 2012104108853 A CN2012104108853 A CN 2012104108853A CN 201210410885 A CN201210410885 A CN 201210410885A CN 102908993 A CN102908993 A CN 102908993A
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- preparation
- hydrotalcite
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- lauryl amine
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Abstract
The invention discloses a preparation method of a porous adsorbent. The preparation method comprises the following steps of: adding waste organic hydrotalcite produced in wastewater treatment to water to obtain turbid liquid, wherein the solid-to-liquid ratio is 1: 10 to 1: 30; adding ethyl silicate as the inorganic neutral precursor, and adding lauryl amine as the cosurfactant, wherein the mass ratio of the organic hydrotalcite to the lauryl amine to the ethyl silicate is 1: (1 to 2): (80 to 120); agitating to react for 4 to 8 hours at the temperature within 50 to 60 DEG C; filtering through a Buchner funnel after the reaction; standing the solid part for 12 to 24 hours at room temperature; and then roasting for 6 to 8 hours at the temperature within 450 to 550 DEG C, so as to obtain the product. According to the preparation method, the surface active agent and the pollutant in the waste organic hydrotalcite are adopted as the templates, the ethyl silicate serving as the inorganic precursor is introduced to the layers, so that the neutral amine and the surface active agent ions form a mixed stick-shaped micelle, and monox hydrate surrounds the micelle; the mixed stick-shaped micelle is roasted to remove the organic part, so as to obtain a porous solid material; and the preparation process is simple.
Description
Technical field
The present invention relates to a kind of preparation method of porous adsorbent, belong to technical field of waste gas treatment in the environmental protection.
Background technology
Desirable waste-gas adsorbant should possess following point usually: 1) adsorbance enough greatly and adsorb reversiblely, namely the enterable space of adsorbate is larger; 2) adsorbate is not wished the catalytic activity that produces, generate to avoid accessory substance, affect the organic matter recovery; 3) since organic exhaust gas in often contain certain steam, the competitive Adsorption effect of hydrone so that adsorbent organic absorption property is affected, so require adsorbent surface certain hydrophobicity to be arranged with the impact of reduce moisture on adsorption effect; 4) regenerated with hot air, high-temperature vapor regeneration are the most frequently used adsorbent reactivation means, and adsorbent has high thermal stability and high hydrothermal stability is to carry out the basis that multiple adsorb/regeneration cycle is used; 5) easily regeneration namely can adapt to multiple regeneration as far as possible.At present, waste gas absorption, the most frequently used adsorbent of lock out operation the most commonly used are active carbons, although it has the advantage that specific surface is large, adsorbance is high, still there are some more formidable deficiencies in using, such as problem inflammable, that the hole is blocked, hydrophobicity is relatively poor and other is relevant with regeneration.
Hydrotalcite layers is introduced in organic anion be prepared into organic hydrotalcite, not only can be used as adsorbent to improve the adsorbance to organic pollution, also can make material have INFRARED ABSORPTION, ultraviolet deadening and excellent catalytic performance, be applied to the preparation of special composite material and new catalytic material.The organic anion pillared hydrotalcite has many special natures, thereby obtains further investigation and widely application.Common application is aspect wastewater treatment, such as: utilize the anion interchangeability of magnalium laminar compound hydrotalcite and host-guest to interact, the dodecyl sodium sulfonate intercalated houghite (DSO-LDHs) for preparing take magnalium nitrate anion hydrotalcite (MgAl-NO3-LDHs) as presoma, dodecyl sulphate intercalated houghite (DS-LDHs) and DBSA intercalated houghite (DBS-LDHs) are to the absorption of the dyestuffs such as disperse blue S-3BG effect (Xu Li preferably again, intercalation assembling and the application study in treatment of dyeing wastewater of magnalium hydrotalcite, Xi'an Technology University, Master's thesis, 2008).After organic hydrotalcite is saturated through absorption, generally need landfill or burning disposal, the organic hydrotalcite after the processing is a kind of waste again without purposes.
From avoiding polluting the angle that control technique produces secondary pollution and improves economy, research is economical, discarded organic hydrotalcite recoverying and utilizing method is very important efficiently.
Summary of the invention
The object of the invention is to for the deficiencies in the prior art, a kind of preparation method of porous adsorbent is proposed, utilize discarded organic hydrotalcite to be controlled to be the purpose adsorbent as raw material are synthetic with exhaust emission, the difficulty of discarded organic hydrotalcite after both can having overcome disposal or having recycled wastewater treatment also provides possibility for preparation low-cost high-efficiency waste gas sorbing material simultaneously.
The technical solution used in the present invention is to adopt following steps: the organic hydrotalcite that will be used for discarding after the wastewater treatment first be added to the water and be prepared into suspension, solid-to-liquid ratio is 1:10 ~ 1:30, add silester as neutral inorganic precursor and lauryl amine as cosurfactant, organic hydrotalcite, lauryl amine, silester mass ratio are 1:(1 ~ 2): (80 ~ 120), in 50 ~ 60 ℃ of stirring reaction 4 ~ 8 h; After reaction is finished, filter with Buchner funnel, solid portion is at room temperature placed 12 ~ 24 h, then get final product at 450 ℃ ~ 550 ℃ lower roasting 6 ~ 8 h.
The present invention utilizes surfactant and the pollutant in the discarded organic hydrotalcite to be template, the inorganic precursor silester is introduced interlayer, surfactant and silicate hydrolyzate product---silicon oxide hydrate interacts, so that forming, neutral amine and surface active agent ion mix rod-shaped micelle, silicon oxide hydrate is centered around around the micella, organic moiety is removed in roasting, forms cellular solid.The invention has the beneficial effects as follows:
1. raw material sources are simple, are the equal of with the refuse reuse.
2. preparation process is simple, through modification presoma is introduced interlayer, and roasting can obtain porous material again.
The specific embodiment
To be added to the water for organic hydrotalcite discarded after the wastewater treatment and be prepared into suspension, solid-to-liquid ratio is 1:10 ~ 1:30, add simultaneously silester as neutral inorganic precursor and lauryl amine as cosurfactant, discarded organic hydrotalcite, lauryl amine, silester are 1:(1 ~ 2 in mass ratio): mix (80 ~ 120), in 50 ~ 60 ℃ of stirring reaction 4 ~ 8 h; In this process, under the effect of cosurfactant, silester is because its lipophile, enters the interlayer of organic hydrotalcite by distributional effects, introduces element silicon for interlayer and provides the foundation.
After stirring reaction is finished, filter with Buchner funnel, solid portion is at room temperature placed 12 ~ 24 h, again solid portion is namely obtained porous adsorbent at 450 ℃ ~ 550 ℃ lower roasting 6 ~ 8 h after the placement.
3 embodiment of the present invention below are provided:
Embodiment 1
To be added to the water for organic hydrotalcite discarded after the wastewater treatment and be prepared into suspension, solid-to-liquid ratio is 1:10, add silester and do and lauryl amine, discarded organic hydrotalcite and lauryl amine, silester in mass ratio 1:1:80 mix, in 60 ℃ of stirring reaction 8 h; After reaction was finished, Buchner funnel filtered, and placed 24 h under the solid portion room temperature, at last at 550 ℃ of lower roasting 6h.
The product that obtains by analysis, specific area is 482 m
2/ g, pore volume are 0.36 cm
3/ g, average pore size is 24 nm, is 0.34g/g(25 ℃ to the saturated adsorption capacity of benzene, benzene relative pressure 0.5 during adsorption equilibrium).
Embodiment 2
To be added to the water for organic hydrotalcite discarded after the wastewater treatment and be prepared into suspension, solid-to-liquid ratio is 1:30, add silester and do and lauryl amine, discarded organic hydrotalcite and lauryl amine, silester in mass ratio 1:2:120 mix, in 50 ℃ of stirring reaction 4 h; After reaction was finished, Buchner funnel filtered, and placed 12 h under the solid portion room temperature, at last at 450 ℃ of lower roasting 8h.
The product that obtains by analysis, specific area is 502 m
2/ g, pore volume are 0.34 cm
3/ g, average pore size is 27 nm, to CO
2Saturated adsorption capacity be 0.28g/g(25 ℃, CO during adsorption equilibrium
2Relative pressure 0.5).
Embodiment 3
To be added to the water for organic hydrotalcite discarded after the wastewater treatment and be prepared into suspension, solid-to-liquid ratio is 1:20, add silester and do and lauryl amine, discarded organic hydrotalcite and lauryl amine, silester in mass ratio 1:2:100 mix, in 55 ℃ of stirring reaction 6 h; After reaction was finished, Buchner funnel filtered, and placed 18 h under the solid portion room temperature, at last at 500 ℃ of lower roasting 7h.
The product that obtains by analysis, specific area is 495 m
2/ g, pore volume are 0.35 cm
3/ g, average pore size is 25 nm, is 0.49g/g(25 ℃ to the saturated adsorption capacity of toluene, toluene relative pressure 0.5 during adsorption equilibrium).
Claims (1)
1. the preparation method of a porous adsorbent is characterized in that adopting following steps:
1) will be added to the water for organic hydrotalcite discarded after the wastewater treatment and be prepared into suspension, solid-to-liquid ratio is 1:10 ~ 1:30, add silester as neutral inorganic precursor and lauryl amine as cosurfactant, organic hydrotalcite, lauryl amine, silester mass ratio are 1:(1 ~ 2): (80 ~ 120), in 50 ~ 60 ℃ of stirring reaction 4 ~ 8 h;
2) after reaction is finished, filter with Buchner funnel, solid portion is at room temperature placed 12 ~ 24 h, then get final product at 450 ℃ ~ 550 ℃ lower roasting 6 ~ 8 h.
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| CN2012104108853A CN102908993A (en) | 2012-10-25 | 2012-10-25 | Preparation method of porous adsorbent |
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| Application Number | Priority Date | Filing Date | Title |
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| CN2012104108853A CN102908993A (en) | 2012-10-25 | 2012-10-25 | Preparation method of porous adsorbent |
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| CN102908993A true CN102908993A (en) | 2013-02-06 |
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| CN2012104108853A Pending CN102908993A (en) | 2012-10-25 | 2012-10-25 | Preparation method of porous adsorbent |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109867306B (en) * | 2017-12-05 | 2022-02-15 | 中国科学院大连化学物理研究所 | Low-temperature preparation method of mesoporous manganese dioxide nanosheets |
Citations (5)
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|---|---|---|---|---|
| CN1554475A (en) * | 2003-12-19 | 2004-12-15 | 浙江大学 | Process for preparing porous clay isomeric material |
| CN1579938A (en) * | 2004-05-21 | 2005-02-16 | 浙江工业大学 | Method for preparing mesoporous silicon metal layer-column clay material |
| JP2009160495A (en) * | 2007-12-28 | 2009-07-23 | Tokyo Institute Of Technology | Separating agent and its manufacturing method |
| CN102294209A (en) * | 2011-06-13 | 2011-12-28 | 北京化工大学 | Preparation method of hydrotalcite hollow microballoon |
| CN102513056A (en) * | 2011-12-20 | 2012-06-27 | 江苏四方锅炉有限公司 | Preparation method of absorbent used for removing mercury vapor pollutant |
-
2012
- 2012-10-25 CN CN2012104108853A patent/CN102908993A/en active Pending
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1554475A (en) * | 2003-12-19 | 2004-12-15 | 浙江大学 | Process for preparing porous clay isomeric material |
| CN1579938A (en) * | 2004-05-21 | 2005-02-16 | 浙江工业大学 | Method for preparing mesoporous silicon metal layer-column clay material |
| JP2009160495A (en) * | 2007-12-28 | 2009-07-23 | Tokyo Institute Of Technology | Separating agent and its manufacturing method |
| CN102294209A (en) * | 2011-06-13 | 2011-12-28 | 北京化工大学 | Preparation method of hydrotalcite hollow microballoon |
| CN102513056A (en) * | 2011-12-20 | 2012-06-27 | 江苏四方锅炉有限公司 | Preparation method of absorbent used for removing mercury vapor pollutant |
Non-Patent Citations (2)
| Title |
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| 周春晖等: "介孔硅层柱蒙脱石材料合成的新方法与表征", 《高等学校化学学报》 * |
| 周春晖等: "层间模板剂导向合成新型多孔蒙脱石材料的研究", 《无机材料学报》 * |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109867306B (en) * | 2017-12-05 | 2022-02-15 | 中国科学院大连化学物理研究所 | Low-temperature preparation method of mesoporous manganese dioxide nanosheets |
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Application publication date: 20130206 |