CN1260002C - Process for preparing porous clay isomeric material - Google Patents
Process for preparing porous clay isomeric material Download PDFInfo
- Publication number
- CN1260002C CN1260002C CN 200310122775 CN200310122775A CN1260002C CN 1260002 C CN1260002 C CN 1260002C CN 200310122775 CN200310122775 CN 200310122775 CN 200310122775 A CN200310122775 A CN 200310122775A CN 1260002 C CN1260002 C CN 1260002C
- Authority
- CN
- China
- Prior art keywords
- organobentonite
- surfactant
- organic
- bentonite
- solid
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Expired - Lifetime
Links
- 239000000463 material Substances 0.000 title claims abstract description 36
- 239000004927 clay Substances 0.000 title claims abstract description 11
- 238000004519 manufacturing process Methods 0.000 title 1
- 239000000440 bentonite Substances 0.000 claims abstract description 36
- 229910000278 bentonite Inorganic materials 0.000 claims abstract description 36
- SVPXDRXYRYOSEX-UHFFFAOYSA-N bentoquatam Chemical compound O.O=[Si]=O.O=[Al]O[Al]=O SVPXDRXYRYOSEX-UHFFFAOYSA-N 0.000 claims abstract description 36
- 239000007787 solid Substances 0.000 claims abstract description 29
- 238000006243 chemical reaction Methods 0.000 claims abstract description 24
- 239000007788 liquid Substances 0.000 claims abstract description 19
- 238000003756 stirring Methods 0.000 claims abstract description 19
- 239000004094 surface-active agent Substances 0.000 claims abstract description 19
- 238000002360 preparation method Methods 0.000 claims abstract description 17
- 239000002243 precursor Substances 0.000 claims abstract description 11
- 239000003093 cationic surfactant Substances 0.000 claims abstract description 8
- 239000002994 raw material Substances 0.000 claims abstract description 8
- 150000001875 compounds Chemical class 0.000 claims abstract description 3
- 238000001179 sorption measurement Methods 0.000 claims description 53
- 238000000926 separation method Methods 0.000 claims description 19
- 238000010521 absorption reaction Methods 0.000 claims description 18
- 239000002351 wastewater Substances 0.000 claims description 14
- 230000007935 neutral effect Effects 0.000 claims description 12
- 239000004064 cosurfactant Substances 0.000 claims description 11
- 238000010792 warming Methods 0.000 claims description 9
- BOTDANWDWHJENH-UHFFFAOYSA-N Tetraethyl orthosilicate Chemical compound CCO[Si](OCC)(OCC)OCC BOTDANWDWHJENH-UHFFFAOYSA-N 0.000 claims description 8
- 238000001308 synthesis method Methods 0.000 claims description 6
- 239000011229 interlayer Substances 0.000 claims description 5
- -1 alkyl pyridine Chemical compound 0.000 claims description 3
- 150000001412 amines Chemical class 0.000 claims description 3
- 230000007062 hydrolysis Effects 0.000 claims description 3
- 238000006460 hydrolysis reaction Methods 0.000 claims description 3
- 238000012643 polycondensation polymerization Methods 0.000 claims description 3
- UQMOLLPKNHFRAC-UHFFFAOYSA-N tetrabutyl silicate Chemical compound CCCCO[Si](OCCCC)(OCCCC)OCCCC UQMOLLPKNHFRAC-UHFFFAOYSA-N 0.000 claims description 3
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 2
- 229910052799 carbon Inorganic materials 0.000 claims description 2
- 239000003795 chemical substances by application Substances 0.000 claims description 2
- 238000001035 drying Methods 0.000 claims description 2
- JUJWROOIHBZHMG-UHFFFAOYSA-N pyridine Substances C1=CC=NC=C1 JUJWROOIHBZHMG-UHFFFAOYSA-N 0.000 claims description 2
- UMJSCPRVCHMLSP-UHFFFAOYSA-N pyridine Natural products COC1=CC=CN=C1 UMJSCPRVCHMLSP-UHFFFAOYSA-N 0.000 claims description 2
- LFQCEHFDDXELDD-UHFFFAOYSA-N tetramethyl orthosilicate Chemical compound CO[Si](OC)(OC)OC LFQCEHFDDXELDD-UHFFFAOYSA-N 0.000 claims description 2
- XXZNHVPIQYYRCG-UHFFFAOYSA-N trihydroxy(propoxy)silane Chemical compound CCCO[Si](O)(O)O XXZNHVPIQYYRCG-UHFFFAOYSA-N 0.000 claims description 2
- 238000005406 washing Methods 0.000 claims description 2
- 238000010189 synthetic method Methods 0.000 claims 1
- 239000011148 porous material Substances 0.000 abstract description 19
- 238000000034 method Methods 0.000 abstract description 8
- 239000000126 substance Substances 0.000 abstract description 2
- 238000006317 isomerization reaction Methods 0.000 abstract 2
- 238000007796 conventional method Methods 0.000 abstract 1
- UHOVQNZJYSORNB-UHFFFAOYSA-N Benzene Chemical compound C1=CC=CC=C1 UHOVQNZJYSORNB-UHFFFAOYSA-N 0.000 description 48
- VZGDMQKNWNREIO-UHFFFAOYSA-N tetrachloromethane Chemical compound ClC(Cl)(Cl)Cl VZGDMQKNWNREIO-UHFFFAOYSA-N 0.000 description 32
- 229920006395 saturated elastomer Polymers 0.000 description 23
- BTJIUGUIPKRLHP-UHFFFAOYSA-N 4-nitrophenol Chemical compound OC1=CC=C([N+]([O-])=O)C=C1 BTJIUGUIPKRLHP-UHFFFAOYSA-N 0.000 description 21
- LZZYPRNAOMGNLH-UHFFFAOYSA-M Cetrimonium bromide Chemical compound [Br-].CCCCCCCCCCCCCCCC[N+](C)(C)C LZZYPRNAOMGNLH-UHFFFAOYSA-M 0.000 description 18
- 239000000203 mixture Substances 0.000 description 7
- JRBPAEWTRLWTQC-UHFFFAOYSA-N dodecylamine Chemical compound CCCCCCCCCCCCN JRBPAEWTRLWTQC-UHFFFAOYSA-N 0.000 description 6
- 238000004065 wastewater treatment Methods 0.000 description 5
- 230000015572 biosynthetic process Effects 0.000 description 3
- 239000002734 clay mineral Substances 0.000 description 3
- 239000002131 composite material Substances 0.000 description 3
- 239000013335 mesoporous material Substances 0.000 description 3
- 238000003786 synthesis reaction Methods 0.000 description 3
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 2
- 230000007613 environmental effect Effects 0.000 description 2
- 239000005416 organic matter Substances 0.000 description 2
- CLWAXFZCVYJLLM-UHFFFAOYSA-N 1-chlorohexadecane Chemical compound CCCCCCCCCCCCCCCCCl CLWAXFZCVYJLLM-UHFFFAOYSA-N 0.000 description 1
- BMVXCPBXGZKUPN-UHFFFAOYSA-N 1-hexanamine Chemical compound CCCCCCN BMVXCPBXGZKUPN-UHFFFAOYSA-N 0.000 description 1
- 208000033498 Non-syndromic pontocerebellar hypoplasia Diseases 0.000 description 1
- 239000003463 adsorbent Substances 0.000 description 1
- 230000003197 catalytic effect Effects 0.000 description 1
- 238000012512 characterization method Methods 0.000 description 1
- 238000001311 chemical methods and process Methods 0.000 description 1
- 239000012141 concentrate Substances 0.000 description 1
- GUJOJGAPFQRJSV-UHFFFAOYSA-N dialuminum;dioxosilane;oxygen(2-);hydrate Chemical compound O.[O-2].[O-2].[O-2].[Al+3].[Al+3].O=[Si]=O.O=[Si]=O.O=[Si]=O.O=[Si]=O GUJOJGAPFQRJSV-UHFFFAOYSA-N 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 235000021321 essential mineral Nutrition 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 229910052901 montmorillonite Inorganic materials 0.000 description 1
- 238000005457 optimization Methods 0.000 description 1
- 150000002892 organic cations Chemical class 0.000 description 1
- 208000017262 paroxysmal cold hemoglobinuria Diseases 0.000 description 1
- 208000004351 pontocerebellar hypoplasia Diseases 0.000 description 1
- 150000003222 pyridines Chemical class 0.000 description 1
- 230000008929 regeneration Effects 0.000 description 1
- 238000011069 regeneration method Methods 0.000 description 1
- 230000001105 regulatory effect Effects 0.000 description 1
- 238000005245 sintering Methods 0.000 description 1
- 239000002689 soil Substances 0.000 description 1
- 230000002194 synthesizing effect Effects 0.000 description 1
- 239000012855 volatile organic compound Substances 0.000 description 1
Landscapes
- Solid-Sorbent Or Filter-Aiding Compositions (AREA)
- Water Treatment By Sorption (AREA)
Abstract
The present invention discloses a method for preparing a porous clay material, which has the process that firstly, organic bentonite which is dehydrated and discarded is mixed and reacts with a co-surfactant; a neutrality inorganic precursor is added in for stirring reaction, and then solid and liquid are separated; a solid part is roasted so that a surfactant and an adsorbed organic dyed substance are removed, and then a required porous clay isomerization material can be obtained. A cationic surfactant in a normal compound method and a clay reaction step are unnecessary, and the additional cationic surfactant is unnecessary; the porous clay isomerization material prepared by the method conforms to the characteristics of the same type material prepared by a conventional method. Thereby, the present invention has the advantages of large specific surface area, uniform pore distribution and high gap ordered degree; the hole diameter is between a micro pore and a mesopore; because the material adopts wastes with low cost as raw materials, and the cationic surfactant is unnecessary, the compounded cost can be greatly reduced and the preparation step is simplified.
Description
Technical field
The invention belongs to the inorganic porous material technical field, be specifically related to a kind of adobe isomery preparation methods, particularly with the organobentonite after the treatment of Organic Wastewater as main body clay raw material and provide cationic surfactant to prepare the method for adobe material.
Background technology
MCM-41, MCM48, FSM-16 and HMS etc. are one of research focuses in multidisciplinary fields such as chemistry, physics, material and environmental protection in the world in recent years for the mesoporous material of representative; (Nature such as nineteen ninety-five Galameau; 1995; 374 (6): 529～531) reported first one class have (mesoporous material in 1.4～2.2nm) apertures, i.e. the adobe isomery material (PCHs) of having of good thermal stability from the super large micropore to the mesopore scope.This type of material is the same with other mesopore material, has that large aperture and aperture homogeneous can be regulated, an advantage such as space degree of order height, specific area are big, but also has better mechanical stability, hydrothermal stability.Adobe material synthetic adopted that to be different from conventional mesoporous material be template with the supramolecular structure that surfactant forms, utilize the sol-gel chemical process, route of synthesis by the interface directional guide effect assembling between organic matter-inorganic matter, in the interlayer duct of 2: 1 type layered clay minerals, carry out interlayer hydrolysis and condensation polymerization and be based on the organic cation and the neutral amine that enter the interlayer duct as the neutral inorganic precursor of cosurfactant template-directed, remove surfactant through roasting then, obtain the adobe material at last.Main preparation process is:
1) reaction of cationic surfactant and layered clay mineral generates organoclay composites;
2) organoclay composites and cosurfactant reaction;
3) with neutral inorganic precursor reaction;
4) surfactant is removed in roasting.
Research to this material at present mainly concentrates on aspects such as synthesis condition (material rate, surfactant and cosurfactant kind and ratio, reaction condition, sintering temperature etc.), structural characterization, absorption property, catalytic performance.But problems such as the more massive optimization of synthesizing and using also necessary solution synthetic technological condition, raw material source and cost.If can main body clay raw material and surfactant will promote the practical application of adobe isomery material well as raw material more widely with more cheap, source.
Bentonite is to be 2: 1 type layered clay minerals of typical case that essential mineral is formed with the montmorillonite, the organobentonite that forms after surfactant carries out organic modification improves tens to hundred times to organic adsorption efficiency than original soil, organobentonite since its to the excellent absorption property of organic matter, waste water (particularly organic wastewater) handle and the contaminated environment reparation in application become the focus of Environmental Science and Engineering area research.But lack cost-effective regeneration and method of disposal and remain one of subject matter of restriction organobentonite practical application in wastewater treatment.The organobentonite that has adsorbed organic pollution if can fully utilize, and not only reduces cost for wastewater treatment, and the secondary pollution that can avoid discarded adsorbent to bring.
Summary of the invention
The purpose of this invention is to provide a kind of adobe isomery material synthesis method.
With the organobentonite behind the adsorption treatment organic wastewater as synthetic main body clay raw material, add cosurfactant as the template direction agent, instruct neutral inorganic precursor between bentonite bed, to carry out interlayer hydrolysis and condensation polymerization in the duct, form inorganic-organic compound intermediate; The compound intermediate of organic and inorganic obtains adobe isomery material after surfactant is removed in roasting.
The concrete preparation process of adobe isomery material is as follows:
1) with the organobentonite behind the adsorption treatment organic wastewater through Separation of Solid and Liquid, in air, dry, 50～100 ℃ of drying 12～24h are to remove ADSORPTION STATE moisture then;
2) with dried organobentonite and cosurfactant by organobentonite: cosurfactant=1: 0.5～mass ratio mixed in 1: 2, in 20～80 ℃ of stirring reaction 15～60min;
3) at room temperature, by organobentonite: neutral inorganic precursor (mass ratio)=1: 100～1: 200 slowly splashes into neutral inorganic precursor, stirring reaction 2～8h;
4) Separation of Solid and Liquid need not washing, and solid portion dries under the room temperature in air, obtains inorganic-organic compound intermediate;
5) under air atmosphere, be warming up to 500～750 ℃ with 2～5 ℃/min speed, roasting 5～10h is to remove the organic pollution of surfactant and absorption.
Cosurfactant can be from chemical formula in the said method
CNH
N-1NH
2A kind of in the neutral amine of (n is a carbon number, and the n scope is 6～18), neutral inorganic precursor is a kind of in methyl silicate, ethyl orthosilicate, positive silicic acid propyl ester, the butyl silicate.Organobentonite is that a kind of and bentonite of quaternary or alkyl pyridine type cationic surfactant reacts the organic clay that obtains.
The adobe isomery material specific area of the present invention's preparation is 400～900m
2/ g, pore volume are 0.1～0.5cm
3/ g, average pore size 13～30nm, at least 750 ℃ of thermal stable temperatures, the benzene saturated adsorption capacity is (25 ℃ of 0.2～0.7g/g, benzene relative pressure 0.5 during adsorption equilibrium), carbon tetrachloride saturated adsorption capacity 0.3～0.8g/g (25 ℃, carbon tetrachloride relative pressure 0.5 during adsorption equilibrium).The adobe isomery material of the present invention's preparation is particularly suitable for the adsorbing separation of volatile organic matter (VOCs).
Advantage of the present invention is:
1) adopts wide material sources, extremely cheap discarded organobentonite as raw material, and need not additionally to add cationic surfactant, reduced the preparation cost of material;
2) preparation process is simplified, and has saved the organoclay composites synthesis technique;
3) wastewater treatment bentonite comprehensive utilization can make full use of bentonite resource, reduces cost for wastewater treatment, avoids secondary pollution, thereby promotes the application of organobentonite in wastewater treatment.
The specific embodiment
The invention will be further elaborated below by embodiment:
Embodiment 1, organobentonite (being called for short the CTMAB bentonite) in the bentonitic ratio preparation of 0.1mol softex kw/100g at first is used for the waste water that adsorption treatment contains 1000mg/L p-nitrophenol (PNP), the bentonitic saturated adsorption capacity of CTMAB is 96mgPNP/g, Separation of Solid and Liquid, the CTMAB bentonite (PNP-CTMAB bentonite) of absorption behind the p-nitrophenol dries in air, then under air atmosphere in 80 ℃ of dry 24h.Get the 14gDNP-CTMAB bentonite and mix with the 13g lauryl amine, 50 ℃ of stirring reaction 30min slowly drip the 120ml ethyl orthosilicate, dropwise back stirring at room reaction 4h.Separation of Solid and Liquid, solid portion dries, and under air atmosphere, is warming up to 560 ℃ with 3 ℃/min speed at last, and roasting 6h can obtain adobe isomery material with the organic pollution of removing surfactant and absorption.
The main character index of sample: specific area is 660m
2/ g, pore volume are 0.25cm
3/ g, average pore size 24nm, at least 750 ℃ of thermal stable temperatures, benzene saturated adsorption capacity are 0.35g/g (25 ℃, benzene relative pressure 0.5 during adsorption equilibrium), carbon tetrachloride saturated adsorption capacity 0.50g/g (25 ℃, carbon tetrachloride relative pressure 0.5 during adsorption equilibrium).
Embodiment 2, organobentonite (being called for short the CPC bentonite) in the bentonitic ratio preparation of 0.1mol chloro-hexadecane yl pyridines/100g at first is used for the waste water that adsorption treatment contains 1000mg/L p-nitrophenol (PNP), the bentonitic saturated adsorption capacity of CPC is 94mgPNP/g, Separation of Solid and Liquid, the CPC bentonite (PNP-CPC bentonite) of absorption behind the p-nitrophenol dries in air, then under air atmosphere in 80 ℃ of dry 24h.Get the 14gDNP-CPC bentonite and mix with the 13g lauryl amine, 50 ℃ of stirring reaction 30min slowly drip the 120ml ethyl orthosilicate, dropwise back stirring at room reaction 4h.Separation of Solid and Liquid, solid portion dries, and under air atmosphere, is warming up to 560 ℃ with 3 ℃/min speed at last, and roasting 6h can obtain adobe isomery material with the organic pollution of removing surfactant and absorption.
The main character index of sample: specific area is 550m
2/ g, pore volume are 0.23cm
3/ g, average pore size 22nm, at least 750 ℃ of thermal stable temperatures, benzene saturated adsorption capacity are 0.25g/g (25 ℃, benzene relative pressure 0.5 during adsorption equilibrium), carbon tetrachloride saturated adsorption capacity 0.45g/g (25 ℃, carbon tetrachloride relative pressure 0.5 during adsorption equilibrium).
Embodiment 3, organobentonite (being called for short the CTMAB bentonite) in the bentonitic ratio preparation of 0.1mol softex kw/100g at first is used for the waste water that adsorption treatment contains 1000mg/L p-nitrophenol (PNP), the bentonitic saturated adsorption capacity of CTMAB is 96mgPNP/g, Separation of Solid and Liquid, the CTMAB bentonite (PNP-CTMAB bentonite) of absorption behind the p-nitrophenol dries in air, then under air atmosphere in 80 ℃ of dry 24h.Get the 14gDNP-CTMAB bentonite and mix with the 28g lauryl amine, 50 ℃ of stirring reaction 30min slowly drip the 120ml ethyl orthosilicate, dropwise back stirring at room reaction 4h.Separation of Solid and Liquid, solid portion dries, and under air atmosphere, is warming up to 560 ℃ with 3 ℃/min speed at last, and roasting 6h can obtain adobe isomery material with the organic pollution of removing surfactant and absorption.
The main character index of sample: specific area is 680m
2/ g, pore volume are 0.26cm
3/ g, average pore size 24nm, at least 750 ℃ of thermal stable temperatures, benzene saturated adsorption capacity are 0.42g/g (25 ℃, benzene relative pressure 0.5 during adsorption equilibrium), carbon tetrachloride saturated adsorption capacity 0.55g/g (25 ℃, carbon tetrachloride relative pressure 0.5 during adsorption equilibrium).
Embodiment 4, organobentonite (being called for short the CTMAB bentonite) in the bentonitic ratio preparation of 0.1mol softex kw/100g at first is used for the waste water that adsorption treatment contains 1000mg/L p-nitrophenol (PNP), the bentonitic saturated adsorption capacity of CTMAB is 96mgPNP/g, Separation of Solid and Liquid, the CTMAB bentonite (PNP-CTMAB bentonite) of absorption behind the p-nitrophenol dries in air, then under air atmosphere in 80 ℃ of dry 24h.Get the 14gDNP-CTMAB bentonite and mix with the 13g lauryl amine, 50 ℃ of stirring reaction 30min slowly drip the 200ml ethyl orthosilicate, dropwise back stirring at room reaction 4h.Separation of Solid and Liquid, solid portion dries, and under air atmosphere, is warming up to 560 ℃ with 3 ℃/min speed at last, and roasting 6h can obtain adobe isomery material with the organic pollution of removing surfactant and absorption.
The main character index of sample: specific area is 680m
2/ g, pore volume are 0.28cm
3/ g, average pore size 24nm, at least 750 ℃ of thermal stable temperatures, benzene saturated adsorption capacity are 0.46g/g (25 ℃, benzene relative pressure 0.5 during adsorption equilibrium), carbon tetrachloride saturated adsorption capacity 0.62g/g (25 ℃, carbon tetrachloride relative pressure 0.5 during adsorption equilibrium).
Embodiment 5, organobentonite (being called for short the CTMAB bentonite) in the bentonitic ratio preparation of 0.1mol softex kw/100g at first is used for the waste water that adsorption treatment contains 1000mg/L p-nitrophenol (PNP), the bentonitic saturated adsorption capacity of CTMAB is 96mgPNP/g, Separation of Solid and Liquid, the CTMAB bentonite (PNP-CTMAB bentonite) of absorption behind the p-nitrophenol dries in air, then under air atmosphere in 80 ℃ of dry 24h.Get the 14gDNP-CTMAB bentonite and mix with the 13g n-hexylamine, 50 ℃ of stirring reaction 30min slowly drip the 120ml ethyl orthosilicate, dropwise back stirring at room reaction 4h.Separation of Solid and Liquid, solid portion dries, and under air atmosphere, is warming up to 560 ℃ with 3 ℃/min speed at last, and roasting 6h can obtain adobe isomery material with the organic pollution of removing surfactant and absorption.
The main character index of sample: specific area is 510m
2/ g, pore volume are 0.19cm
3/ g, average pore size 21nm, at least 750 ℃ of thermal stable temperatures, benzene saturated adsorption capacity are 0.31g/g (25 ℃, benzene relative pressure 0.5 during adsorption equilibrium), carbon tetrachloride saturated adsorption capacity 0.39g/g (25 ℃, carbon tetrachloride relative pressure 0.5 during adsorption equilibrium).
Embodiment 6, organobentonite (being called for short the CTMAB bentonite) in the bentonitic ratio preparation of 0.1mol softex kw/100g at first is used for the waste water that adsorption treatment contains 1000mg/L p-nitrophenol (PNP), the bentonitic saturated adsorption capacity of CTMAB is 96mgPNP/g, Separation of Solid and Liquid, the CTMAB bentonite (PNP-CTMAB bentonite) of absorption behind the p-nitrophenol dries in air, then under air atmosphere in 80 ℃ of dry 24h.Get the 14gDNP-CTMAB bentonite and mix with the 13g lauryl amine, 50 ℃ of stirring reaction 30min slowly drip the 120ml ethyl orthosilicate, dropwise back stirring at room reaction 4h.Separation of Solid and Liquid, solid portion dries, and under air atmosphere, is warming up to 700 ℃ with 3 ℃/min speed at last, and roasting 6h can obtain adobe isomery material with the organic pollution of removing surfactant and absorption.
The main character index of sample: specific area is 600m
2/ g, pore volume are 0.24cm
3/ g, average pore size 23nm, at least 750 ℃ of thermal stable temperatures, benzene saturated adsorption capacity are 0.33g/g (25 ℃, benzene relative pressure 0.5 during adsorption equilibrium), carbon tetrachloride saturated adsorption capacity 0.47g/g (25 ℃, carbon tetrachloride relative pressure 0.5 during adsorption equilibrium).
Embodiment 7, organobentonite (being called for short the CTMAB bentonite) in the bentonitic ratio preparation of 0.1mol softex kw/100g at first is used for the waste water that adsorption treatment contains 1000mg/L p-nitrophenol (PNP), the bentonitic saturated adsorption capacity of CTMAB is 96mgPNP/g, Separation of Solid and Liquid, the CTMAB bentonite (PNP-CTMAB bentonite) of absorption behind the p-nitrophenol dries in air, then under air atmosphere in 80 ℃ of dry 24h.Get the 14gDNP-CTMAB bentonite and mix with the 13g lauryl amine, 50 ℃ of stirring reaction 30min slowly drip the 120ml butyl silicate, dropwise back stirring at room reaction 4h.Separation of Solid and Liquid, solid portion dries, and under air atmosphere, is warming up to 560 ℃ with 3 ℃/min speed at last, and roasting 6h can obtain adobe isomery material with the organic pollution of removing surfactant and absorption.
The main character index of sample: specific area is 560m
2/ g, pore volume are 0.22cm
3/ g, average pore size 25nm, at least 750 ℃ of thermal stable temperatures, benzene saturated adsorption capacity are 0.30g/g (25 ℃, benzene relative pressure 0.5 during adsorption equilibrium), carbon tetrachloride saturated adsorption capacity 0.42g/g (25 ℃, carbon tetrachloride relative pressure 0.5 during adsorption equilibrium).
Claims (5)
1. adobe isomery material synthesis method, it is characterized in that with the organobentonite behind the adsorption treatment organic wastewater as synthetic main body clay raw material, add cosurfactant as the template direction agent, instruct neutral inorganic precursor between bentonite bed, to carry out interlayer hydrolysis and condensation polymerization in the duct, form inorganic-organic compound intermediate; The compound intermediate of organic and inorganic obtains adobe isomery material after surfactant is removed in roasting.
2. a kind of adobe isomery material synthesis method according to claim 1 is characterized in that the concrete preparation process of said synthetic method is as follows:
1) with the organobentonite behind the adsorption treatment organic wastewater through Separation of Solid and Liquid, in air, dry, 50～100 ℃ of drying 12～24h are to remove ADSORPTION STATE moisture then;
2) with dried organobentonite and cosurfactant by organobentonite: cosurfactant=1: 0.5～mass ratio mixed in 1: 2, in 20～80 ℃ of stirring reaction 15～60min;
3) at room temperature, by organobentonite: the mass ratio of neutral inorganic precursor=1: 100～1: 200 slowly splashes into neutral inorganic precursor, stirring reaction 2～8h;
4) Separation of Solid and Liquid need not washing, and solid portion dries under the room temperature in air, obtains inorganic-organic compound intermediate;
5) under air atmosphere, be warming up to 500～750 ℃ with 2～5 ℃/min speed, roasting 5～10h is to remove the organic pollution of surfactant and absorption.
3. a kind of adobe isomery material synthesis method according to claim 1 is characterized in that said organobentonite is that a kind of and bentonite of quaternary or alkyl pyridine type cationic surfactant reacts the organic clay that obtains.
4. a kind of adobe isomery material synthesis method according to claim 1 is characterized in that said cosurfactant is formula C
nH
N-1NH
2Neutral amine, n is a carbon number, the n scope is 6～18.
5. a kind of adobe isomery material synthesis method according to claim 1 is characterized in that said neutral inorganic precursor is a kind of in methyl silicate, ethyl orthosilicate, positive silicic acid propyl ester, the butyl silicate.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 200310122775 CN1260002C (en) | 2003-12-19 | 2003-12-19 | Process for preparing porous clay isomeric material |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 200310122775 CN1260002C (en) | 2003-12-19 | 2003-12-19 | Process for preparing porous clay isomeric material |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN1554475A CN1554475A (en) | 2004-12-15 |
| CN1260002C true CN1260002C (en) | 2006-06-21 |
Family
ID=34338755
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN 200310122775 Expired - Lifetime CN1260002C (en) | 2003-12-19 | 2003-12-19 | Process for preparing porous clay isomeric material |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN1260002C (en) |
Families Citing this family (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101104525B (en) * | 2007-08-06 | 2010-05-26 | 浙江大学 | Method for preparing anatase type bentonite-base porous titanium dioxide nano material |
| CN102908993A (en) * | 2012-10-25 | 2013-02-06 | 常州大学 | Preparation method of porous adsorbent |
| CN103657594B (en) * | 2013-11-19 | 2015-07-15 | 浙江大学 | Preparation method of tiny hole type multihole clay heterogeneous material |
| KR102431511B1 (en) * | 2016-07-01 | 2022-08-12 | 인제비티 사우스 캐롤라이나, 엘엘씨 | Method for enhancing volumetric capacity in gas storage and release systems |
| CN112337427B (en) * | 2020-10-15 | 2022-07-19 | 四川轻化工大学 | La @ Zr @ SiO2Preparation method of @ bentonite composite phosphorus removal adsorbent |
| CN112657460A (en) * | 2020-11-04 | 2021-04-16 | 浙江工商大学 | Porous clay-based adsorption material for adsorbing polycyclic aromatic hydrocarbons in atmosphere, and preparation and application thereof |
-
2003
- 2003-12-19 CN CN 200310122775 patent/CN1260002C/en not_active Expired - Lifetime
Also Published As
| Publication number | Publication date |
|---|---|
| CN1554475A (en) | 2004-12-15 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN104826582B (en) | A kind of preparation method of graphene meso-porous titanium dioxide silica aerogel | |
| CN104709906B (en) | Preparation method of three dimensional graded porous activated carbon material | |
| CN1113692C (en) | Modified carbon adsorbents and process for adsorption | |
| CN102179230B (en) | Preparation method of magnetized silicon dioxide aerogel | |
| CN105254916A (en) | Preparation method for oxidized graphene-poly-dopamine composite aerogel | |
| CN104587918A (en) | Silver nano-particle modified carbon ball/graphene composite aero-gel material as well as preparation method and application of material | |
| CN105413639A (en) | Bio-friendly type lecithin/vermiculite composite material as wall as preparation method and application thereof | |
| JP2011241097A (en) | Method for producing hydrophobic zeolite and hydrophobic zeolite obtained by the method | |
| CN1260002C (en) | Process for preparing porous clay isomeric material | |
| CN109621903A (en) | A method of preparing sludge base charcoal zeolite functional material | |
| CN109160507A (en) | The magnanimity preparation method of fluorinated graphene | |
| KR20140056650A (en) | Adsorbents using alum sludges and adsorbents having modified surfaces | |
| CN107512712B (en) | A kind of multi-stage porous Carbon Materials and preparation method thereof | |
| CN109926031B (en) | MOFs (metal-organic frameworks)/sponge composite material as well as preparation method and application thereof | |
| KR20120132873A (en) | Recycle method of spent carbons by chemical impregnation and heating treatments in vacuum | |
| CN1944443A (en) | Process for preparing silicon material containing sulfonic group | |
| CN1724344A (en) | Preparing multipurpous carbon with regular constructure and high ratio surface area by mould board carbonizing process | |
| CN101380569B (en) | Preparation method of three-dimensional ordered macropore carbon loaded with titanium dioxide particles and application method thereof | |
| CN113000019A (en) | Na-P-rich zeolite adsorbent and preparation method and application thereof | |
| CN103333367B (en) | Preparation method of thermostability enhanced melamine covalent functionalized graphene based nanohybrid material | |
| Liang et al. | Regeneration of spent bleaching clay by ultrasonic irradiation and its application in methylene blue adsorption | |
| CN105921113A (en) | Adsorbent used for removing phthalic acid in water and preparation method thereof | |
| CN101439282B (en) | Method for preparing modified expanded graphite and use in benzene gas processing | |
| CN109281063B (en) | Preparation method and application of organic silicon fiber membrane containing secondary amino group | |
| Sulaiman et al. | Microstructure of CuO assisted activated carbon adsorbent from rubber wood sawdust produced by mechanochemical processing |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| C14 | Grant of patent or utility model | ||
| GR01 | Patent grant | ||
| CX01 | Expiry of patent term |
Granted publication date: 20060621 |
|
| CX01 | Expiry of patent term |