CN103657594B - Preparation method of tiny hole type multihole clay heterogeneous material - Google Patents
Preparation method of tiny hole type multihole clay heterogeneous material Download PDFInfo
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- CN103657594B CN103657594B CN201310580048.XA CN201310580048A CN103657594B CN 103657594 B CN103657594 B CN 103657594B CN 201310580048 A CN201310580048 A CN 201310580048A CN 103657594 B CN103657594 B CN 103657594B
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- hole type
- clay
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- organobentonite
- mass ratio
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- 239000000463 material Substances 0.000 title claims abstract description 35
- 239000004927 clay Substances 0.000 title claims abstract description 8
- 238000002360 preparation method Methods 0.000 title claims abstract description 6
- 239000007787 solid Substances 0.000 claims abstract description 12
- BOTDANWDWHJENH-UHFFFAOYSA-N Tetraethyl orthosilicate Chemical compound CCO[Si](OCC)(OCC)OCC BOTDANWDWHJENH-UHFFFAOYSA-N 0.000 claims abstract description 9
- JRBPAEWTRLWTQC-UHFFFAOYSA-N dodecylamine Chemical compound CCCCCCCCCCCCN JRBPAEWTRLWTQC-UHFFFAOYSA-N 0.000 claims abstract description 9
- 238000000967 suction filtration Methods 0.000 claims abstract description 9
- 238000000034 method Methods 0.000 claims abstract description 7
- 238000001354 calcination Methods 0.000 claims abstract description 3
- 238000001035 drying Methods 0.000 claims abstract description 3
- 239000002243 precursor Substances 0.000 claims description 12
- ZZNQQQWFKKTOSD-UHFFFAOYSA-N diethoxy(diphenyl)silane Chemical compound C=1C=CC=CC=1[Si](OCC)(OCC)C1=CC=CC=C1 ZZNQQQWFKKTOSD-UHFFFAOYSA-N 0.000 claims description 9
- 238000007605 air drying Methods 0.000 claims description 6
- 229910000278 bentonite Inorganic materials 0.000 claims description 6
- 239000000440 bentonite Substances 0.000 claims description 6
- SVPXDRXYRYOSEX-UHFFFAOYSA-N bentoquatam Chemical compound O.O=[Si]=O.O=[Al]O[Al]=O SVPXDRXYRYOSEX-UHFFFAOYSA-N 0.000 claims description 6
- 238000004887 air purification Methods 0.000 claims description 3
- 230000015572 biosynthetic process Effects 0.000 claims description 3
- 238000005341 cation exchange Methods 0.000 claims description 3
- 238000002156 mixing Methods 0.000 abstract description 10
- 239000002957 persistent organic pollutant Substances 0.000 abstract description 4
- FPBVFNTVPCZBMM-UHFFFAOYSA-N 2,2-diphenylethoxy-ethoxy-dimethylsilane Chemical compound C1(=CC=CC=C1)C(CO[Si](OCC)(C)C)C1=CC=CC=C1 FPBVFNTVPCZBMM-UHFFFAOYSA-N 0.000 abstract 1
- 230000000274 adsorptive effect Effects 0.000 abstract 1
- 238000007664 blowing Methods 0.000 abstract 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 abstract 1
- 238000001179 sorption measurement Methods 0.000 description 7
- 238000004140 cleaning Methods 0.000 description 3
- 239000003344 environmental pollutant Substances 0.000 description 3
- 239000002808 molecular sieve Substances 0.000 description 3
- 231100000719 pollutant Toxicity 0.000 description 3
- 239000011148 porous material Substances 0.000 description 3
- URGAHOPLAPQHLN-UHFFFAOYSA-N sodium aluminosilicate Chemical compound [Na+].[Al+3].[O-][Si]([O-])=O.[O-][Si]([O-])=O URGAHOPLAPQHLN-UHFFFAOYSA-N 0.000 description 3
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 2
- 238000010521 absorption reaction Methods 0.000 description 2
- 229910052799 carbon Inorganic materials 0.000 description 2
- 230000007812 deficiency Effects 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 238000000746 purification Methods 0.000 description 2
- 230000010148 water-pollination Effects 0.000 description 2
- 239000002250 absorbent Substances 0.000 description 1
- 230000002745 absorbent Effects 0.000 description 1
- 238000004378 air conditioning Methods 0.000 description 1
- 239000000809 air pollutant Substances 0.000 description 1
- 231100001243 air pollutant Toxicity 0.000 description 1
- 238000003915 air pollution Methods 0.000 description 1
- 239000011248 coating agent Substances 0.000 description 1
- 238000000576 coating method Methods 0.000 description 1
- 230000000052 comparative effect Effects 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 230000002708 enhancing effect Effects 0.000 description 1
- 230000002209 hydrophobic effect Effects 0.000 description 1
- 230000000391 smoking effect Effects 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
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- Solid-Sorbent Or Filter-Aiding Compositions (AREA)
Abstract
The invention discloses a preparation method of a micro-hole type multihole clay heterogeneous material. The method comprises the following steps: uniformly mixing tetraethoxysilane and diphenyl dimethyldiethoxylsilane at a mass ratio of 1:(0.1-100) to form a mixing solution; fully uniformly mixing lauryl amine, organobentonite and the mixing solution at a mass ratio of (1-40);1:120 to obtain a front body solution; carrying out water bath reaction on the front body solution at 30-70 DEG C for 6-18 hours, carrying out suction filtration, naturally blowing or drying the obtained solid, placing the solid in a muffle furnace at 450-650 DEG C, and calcining for 2-6 hours to obtain the micro-hole type multihole clay heterogeneous material. The prepared material provided by the invention has the advantages that the adsorptive property of an indoor organic pollutant is better than that of the PCH material synthetized by the traditional method, and the material has wide application prospect.
Description
Technical field
The invention belongs to technical field of absorbent, be specifically related to a kind of preparation method of micro-hole type multihole clay isomery material.
Background technology
Room air pollution serious harm human health, its purification techniques is subject to people and more and more pays close attention to.Absorption method has that efficiency is high, cost is low, nonhazardous, be easy to advantages such as commercially producing, is widely used in indoor air purification.Wherein common sorbing material has active carbon and molecular sieve etc., and active carbon is usually used in removing hydrophobic organic pollutant, but is difficult to effectively remove polarity organic pollution.Molecular sieve can be used for adsorption cleaning hydrophily organic pollution, but cost is high.Adobe isomery material (being called for short PCH) is a kind of porous material of surface hydrophilic, can be used for adsorption cleaning hydrophily organic pollution, and cost is significantly lower than molecular sieve.But traditional PCH material is as a kind of mesopore adsorption material (aperture >2nm), it is difficult to reach real requirement to the adsorption effect of light concentration organic pollutant in room air, thus needs to develop the abundant novel PC H material of micropore (aperture <2nm).
Summary of the invention
For solving the few deficiency of conventional P CH micro content, the present invention adopts diphenyl diethoxy silane as pore former, and low temperature has synthesized the novel PC H material containing enriching micropore.
The inventive method comprises the following steps:
Step (1). in bentonite, add softex kw mix, obtain organobentonite; The addition of softex kw is one times of bentonite cation exchange capacity (CEC) CEC;
Step (2). by ethyl orthosilicate with diphenyl diethoxy silane by 1:(0.1 ~ 100) mass ratio mix formation mixed liquor;
Step (3). the mixed liquor that the organobentonite synthesize lauryl amine, step (1) and step (2) obtain fully mixes by the mass ratio of (1 ~ 40): 1:120, obtains precursor solution;
Step (4). the precursor solution that step (3) is obtained after 30 ~ 70 DEG C of water-bath 6 ~ 18h hours and suction filtration, the solid natural air drying obtained or oven dry;
Step (5). the drying solid that step (4) obtains is put into Muffle furnace 450 ~ 650 DEG C calcining 2 ~ 6h and obtain micropore PCH material.
The present invention adopts diphenyl diethoxy silane as pore former, makes the material micropore size <2nm finally prepared, can reach the adsorption effect of light concentration organic pollutant in room air better.
Material prepared by the present invention all has obvious lifting than conventional P CH material in the parameters such as aperture, specific area, micropore specific area, significantly strengthens the adsorption capacity of low concentration pollutant.
The material of the present invention's synthesis can be applicable to indoor air purification, such as: be that core prepares clean air package with material, be installed on air purifier, effectively can remove the pollutant as finishing, smoking etc. produce; Be installed on air-conditioning equipment, then can realize removing indoor pollutant in the process of Air conditioner air exchange, effectively reduce the indoor healthy risk because new wind deficiency causes; Material preparation being become coating, the adsorption cleaning to being indoor air pollutants can being realized.This materials'use place is extensive, as resident indoor, hospital, school and factory etc., is with a wide range of applications in light concentration gas field of purification.
Accompanying drawing explanation
The micropore PCH material of Fig. 1 prepared by embodiment 1 and the pore-size distribution comparison diagram of conventional P CH material.
Detailed description of the invention
Below in conjunction with the drawings and specific embodiments, the present invention is further analyzed.
Comparative example.
By 2g organobentonite and the mixing of 40g lauryl amine, 50 DEG C are stirred 30min; Added by 240g ethyl orthosilicate, 35 DEG C are stirred 12h; Gained solid natural air drying after suction filtration; Namely Muffle furnace with 2 DEG C/min temperature programming to 600 DEG C, and obtains conventional P CH material after keeping 4h, is designated as PCH0.
Embodiment 1.
180g ethyl orthosilicate and 60g diphenyl diethoxy silane are mixed and form 240g mixed liquor, by 2g organobentonite and the mixing of 40g lauryl amine, 50 DEG C are stirred 30min, then add 240g mixed liquor, and 35 DEG C are stirred 12h; Gained solid natural air drying after suction filtration; Namely Muffle furnace with 2 DEG C/min temperature programming to 600 DEG C, and obtains micropore PCH material after keeping 4h, be designated as PCH25.
As shown in table 1, Fig. 1, specific area and the micropore specific area of PCH25 are all greater than PCH0; PCH25 and PCH0 compares, and its micro content significantly increases, and mesopore content obviously reduces, and the enhancing more obvious than PCH0 of the absorption potential of PCH25 is described.
The specific area of the different PCH sorbing material of table 1 and micropore specific area
| Sorbing material | Specific area m 2g -1 | Micropore specific surface m 2g -1 |
| PCH0 | 855 | 732 |
| PCH25 | 963 | 875 |
Embodiment 2.
120g ethyl orthosilicate and 120g diphenyl diethoxy silane are mixed and form 240g mixed liquor, by 2g organobentonite and the mixing of 40g lauryl amine, 50 DEG C are stirred 30min, then add 240g mixed liquor, and 35 DEG C are stirred 12h, obtain precursor solution; By gained solid natural air drying after precursor solution suction filtration; Muffle furnace with 2 DEG C/min temperature programming to 600 DEG C, and obtains micropore PCH material after keeping 600 DEG C to calcine 4h.
Embodiment 3.
60g ethyl orthosilicate and 180g diphenyl diethoxy silane are mixed and form 240g mixed liquor, by 2g organobentonite and the mixing of 40g lauryl amine, 70 DEG C are stirred 30min, then add 240g mixed liquor, and 35 DEG C are stirred 12h, obtain precursor solution; By gained solid after precursor solution suction filtration 70 DEG C oven dry; Muffle furnace with 2 DEG C/min temperature programming to 600 DEG C, and obtains micropore PCH material after keeping 600 DEG C to calcine 4h.
Embodiment 4.
218.2g ethyl orthosilicate and 21.8g diphenyl diethoxy silane are mixed and form 240g mixed liquor, by 2g organobentonite and the mixing of 2g lauryl amine, 50 DEG C are stirred 30min, then add 240g mixed liquor, and 35 DEG C are stirred 12h, obtain precursor solution; By gained solid natural air drying after precursor solution suction filtration; Muffle furnace with 2 DEG C/min temperature programming to 450 DEG C, and obtains micropore PCH material after keeping 450 DEG C to calcine 6h.
Embodiment 5.
2.4g ethyl orthosilicate and 237.6g diphenyl diethoxy silane are mixed and form 240g mixed liquor, by 2g organobentonite and the mixing of 80g lauryl amine, 70 DEG C are stirred 30min, then add 240g mixed liquor, and 35 DEG C are stirred 12h, obtain precursor solution; By gained solid after precursor solution suction filtration 70 DEG C oven dry; Muffle furnace with 2 DEG C/min temperature programming to 650 DEG C, and obtains micropore PCH material after keeping 650 DEG C to calcine 2h.
Above-described embodiment organobentonite used in bentonite, adds softex kw mix and form; The addition of softex kw is one times of bentonite cation exchange capacity (CEC) CEC.
Above embodiment is only described further invention, and scope of the present invention is not limited to by illustrated embodiment.
Claims (1)
1. a preparation method for micro-hole type multihole clay isomery material, is characterized in that the method comprises the following steps:
Step (1). in bentonite, add softex kw mix, obtain organobentonite; The addition of softex kw is one times of bentonite cation exchange capacity (CEC) CEC;
Step (2). by ethyl orthosilicate with diphenyl diethoxy silane by 1:(0.1 ~ 100) mass ratio mix formation mixed liquor;
Step (3). the mixed liquor that the organobentonite synthesize lauryl amine, step (1) and step (2) obtain fully mixes by the mass ratio of (1 ~ 40): 1:120, obtains precursor solution;
Step (4). the precursor solution that step (3) is obtained after 30 ~ 70 DEG C of water-bath 6 ~ 18h hours and suction filtration, the solid natural air drying obtained or oven dry;
Step (5). the drying solid that step (4) obtains is put into Muffle furnace 450 ~ 650 DEG C calcining 2 ~ 6h and obtain micro-hole type multihole clay isomery material;
The micro-hole type multihole clay isomery materials application that said method prepares is in indoor air purification.
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| CN201310580048.XA CN103657594B (en) | 2013-11-19 | 2013-11-19 | Preparation method of tiny hole type multihole clay heterogeneous material |
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| CN201310580048.XA CN103657594B (en) | 2013-11-19 | 2013-11-19 | Preparation method of tiny hole type multihole clay heterogeneous material |
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| CN103657594A CN103657594A (en) | 2014-03-26 |
| CN103657594B true CN103657594B (en) | 2015-07-15 |
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Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5726113A (en) * | 1996-03-19 | 1998-03-10 | Board Of Trustees Operating Michigan State University | Porous clay heterostructures prepared by gallery templated synthesis |
| CN1462726A (en) * | 2003-04-07 | 2003-12-24 | 浙江大学 | Integral method of synthesizing organobentonite-treating wastewater |
| CN1554475A (en) * | 2003-12-19 | 2004-12-15 | 浙江大学 | Process for preparing porous clay isomeric material |
| CN102272239A (en) * | 2008-11-26 | 2011-12-07 | 爱尔兰国家大学科克学院 | A process for preparing silica microparticles |
-
2013
- 2013-11-19 CN CN201310580048.XA patent/CN103657594B/en active Active
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5726113A (en) * | 1996-03-19 | 1998-03-10 | Board Of Trustees Operating Michigan State University | Porous clay heterostructures prepared by gallery templated synthesis |
| CN1462726A (en) * | 2003-04-07 | 2003-12-24 | 浙江大学 | Integral method of synthesizing organobentonite-treating wastewater |
| CN1554475A (en) * | 2003-12-19 | 2004-12-15 | 浙江大学 | Process for preparing porous clay isomeric material |
| CN102272239A (en) * | 2008-11-26 | 2011-12-07 | 爱尔兰国家大学科克学院 | A process for preparing silica microparticles |
Non-Patent Citations (2)
| Title |
|---|
| Adsorption behaviors of volatile organic compounds(VOCs) on porous clay heterostructures(PCH);Fang Qu et al.;《Journal of Hazardous Materials》;20090515;第170卷;第7-12页 * |
| 热处理蒙脱石的γ-氨丙基三乙氧基硅烷改性研究;覃宗华等;《矿物学报》;20120331;第32卷(第1期);第14-21页 * |
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