CN106145132B - A method of ordered mesoporous material Al-MCM-41 is prepared using attapulgite - Google Patents
A method of ordered mesoporous material Al-MCM-41 is prepared using attapulgite Download PDFInfo
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- 229960000892 attapulgite Drugs 0.000 title claims abstract description 39
- 229910052625 palygorskite Inorganic materials 0.000 title claims abstract description 39
- 239000013335 mesoporous material Substances 0.000 title claims abstract description 36
- 238000000034 method Methods 0.000 title claims abstract description 23
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims abstract description 18
- 239000002994 raw material Substances 0.000 claims abstract description 16
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 15
- 239000004094 surface-active agent Substances 0.000 claims abstract description 11
- 239000008367 deionised water Substances 0.000 claims abstract description 10
- 229910021641 deionized water Inorganic materials 0.000 claims abstract description 10
- 230000004913 activation Effects 0.000 claims abstract description 8
- 230000020477 pH reduction Effects 0.000 claims abstract description 7
- 239000007787 solid Substances 0.000 claims abstract description 6
- 239000002734 clay mineral Substances 0.000 claims abstract description 3
- 239000000243 solution Substances 0.000 claims description 13
- LZZYPRNAOMGNLH-UHFFFAOYSA-M Cetrimonium bromide Chemical group [Br-].CCCCCCCCCCCCCCCC[N+](C)(C)C LZZYPRNAOMGNLH-UHFFFAOYSA-M 0.000 claims description 10
- 238000001035 drying Methods 0.000 claims description 7
- 238000005406 washing Methods 0.000 claims description 6
- 206010013786 Dry skin Diseases 0.000 claims description 5
- 239000011259 mixed solution Substances 0.000 claims description 5
- 238000007654 immersion Methods 0.000 claims description 2
- 238000010907 mechanical stirring Methods 0.000 claims description 2
- LIVNPJMFVYWSIS-UHFFFAOYSA-N silicon monoxide Chemical compound [Si-]#[O+] LIVNPJMFVYWSIS-UHFFFAOYSA-N 0.000 claims description 2
- 229910052710 silicon Inorganic materials 0.000 abstract description 21
- 239000010703 silicon Substances 0.000 abstract description 21
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 abstract description 20
- 239000011148 porous material Substances 0.000 abstract description 6
- 238000009826 distribution Methods 0.000 abstract description 4
- 238000003912 environmental pollution Methods 0.000 abstract description 4
- 150000007522 mineralic acids Chemical class 0.000 abstract description 3
- 239000003513 alkali Substances 0.000 abstract description 2
- 230000009286 beneficial effect Effects 0.000 abstract description 2
- 238000005265 energy consumption Methods 0.000 abstract description 2
- 238000004519 manufacturing process Methods 0.000 abstract description 2
- 239000000126 substance Substances 0.000 abstract description 2
- 231100001261 hazardous Toxicity 0.000 abstract 1
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 10
- 229910052782 aluminium Inorganic materials 0.000 description 10
- 239000000463 material Substances 0.000 description 9
- 238000010521 absorption reaction Methods 0.000 description 7
- 229910052500 inorganic mineral Inorganic materials 0.000 description 7
- 239000011707 mineral Substances 0.000 description 7
- 238000002360 preparation method Methods 0.000 description 7
- 238000003756 stirring Methods 0.000 description 5
- 239000003795 chemical substances by application Substances 0.000 description 4
- AXDJCCTWPBKUKL-UHFFFAOYSA-N 4-[(4-aminophenyl)-(4-imino-3-methylcyclohexa-2,5-dien-1-ylidene)methyl]aniline;hydron;chloride Chemical compound Cl.C1=CC(=N)C(C)=CC1=C(C=1C=CC(N)=CC=1)C1=CC=C(N)C=C1 AXDJCCTWPBKUKL-UHFFFAOYSA-N 0.000 description 3
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 3
- 239000002585 base Substances 0.000 description 3
- 238000006555 catalytic reaction Methods 0.000 description 3
- 238000002386 leaching Methods 0.000 description 3
- 239000005995 Aluminium silicate Substances 0.000 description 2
- BOTDANWDWHJENH-UHFFFAOYSA-N Tetraethyl orthosilicate Chemical compound CCO[Si](OCC)(OCC)OCC BOTDANWDWHJENH-UHFFFAOYSA-N 0.000 description 2
- 239000003463 adsorbent Substances 0.000 description 2
- 235000012211 aluminium silicate Nutrition 0.000 description 2
- 238000006243 chemical reaction Methods 0.000 description 2
- 229910052681 coesite Inorganic materials 0.000 description 2
- 230000000052 comparative effect Effects 0.000 description 2
- 229910052906 cristobalite Inorganic materials 0.000 description 2
- 239000012229 microporous material Substances 0.000 description 2
- 238000002156 mixing Methods 0.000 description 2
- 238000012545 processing Methods 0.000 description 2
- 238000011160 research Methods 0.000 description 2
- 239000000377 silicon dioxide Substances 0.000 description 2
- 238000002336 sorption--desorption measurement Methods 0.000 description 2
- 229910052682 stishovite Inorganic materials 0.000 description 2
- 239000000454 talc Substances 0.000 description 2
- 229910052623 talc Inorganic materials 0.000 description 2
- 235000012222 talc Nutrition 0.000 description 2
- LFQCEHFDDXELDD-UHFFFAOYSA-N tetramethyl orthosilicate Chemical compound CO[Si](OC)(OC)OC LFQCEHFDDXELDD-UHFFFAOYSA-N 0.000 description 2
- 229910052905 tridymite Inorganic materials 0.000 description 2
- 239000010455 vermiculite Substances 0.000 description 2
- 229910052902 vermiculite Inorganic materials 0.000 description 2
- 235000019354 vermiculite Nutrition 0.000 description 2
- 238000005303 weighing Methods 0.000 description 2
- USFZMSVCRYTOJT-UHFFFAOYSA-N Ammonium acetate Chemical compound N.CC(O)=O USFZMSVCRYTOJT-UHFFFAOYSA-N 0.000 description 1
- 239000005695 Ammonium acetate Substances 0.000 description 1
- FYYHWMGAXLPEAU-UHFFFAOYSA-N Magnesium Chemical compound [Mg] FYYHWMGAXLPEAU-UHFFFAOYSA-N 0.000 description 1
- 102220500397 Neutral and basic amino acid transport protein rBAT_M41T_mutation Human genes 0.000 description 1
- BPQQTUXANYXVAA-UHFFFAOYSA-N Orthosilicate Chemical compound [O-][Si]([O-])([O-])[O-] BPQQTUXANYXVAA-UHFFFAOYSA-N 0.000 description 1
- 229910002796 Si–Al Inorganic materials 0.000 description 1
- 239000004115 Sodium Silicate Substances 0.000 description 1
- 238000004833 X-ray photoelectron spectroscopy Methods 0.000 description 1
- 239000002250 absorbent Substances 0.000 description 1
- 230000002745 absorbent Effects 0.000 description 1
- 239000004411 aluminium Substances 0.000 description 1
- PZZYQPZGQPZBDN-UHFFFAOYSA-N aluminium silicate Chemical compound O=[Al]O[Si](=O)O[Al]=O PZZYQPZGQPZBDN-UHFFFAOYSA-N 0.000 description 1
- 229910000323 aluminium silicate Inorganic materials 0.000 description 1
- 229940043376 ammonium acetate Drugs 0.000 description 1
- 235000019257 ammonium acetate Nutrition 0.000 description 1
- 239000000440 bentonite Substances 0.000 description 1
- 229910000278 bentonite Inorganic materials 0.000 description 1
- SVPXDRXYRYOSEX-UHFFFAOYSA-N bentoquatam Chemical compound O.O=[Si]=O.O=[Al]O[Al]=O SVPXDRXYRYOSEX-UHFFFAOYSA-N 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 239000003054 catalyst Substances 0.000 description 1
- 230000003197 catalytic effect Effects 0.000 description 1
- 210000003850 cellular structure Anatomy 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 239000004927 clay Substances 0.000 description 1
- 239000002131 composite material Substances 0.000 description 1
- 238000002425 crystallisation Methods 0.000 description 1
- 238000003795 desorption Methods 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000010828 elution Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000011156 evaluation Methods 0.000 description 1
- NLYAJNPCOHFWQQ-UHFFFAOYSA-N kaolin Chemical compound O.O.O=[Al]O[Si](=O)O[Si](=O)O[Al]=O NLYAJNPCOHFWQQ-UHFFFAOYSA-N 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 239000011777 magnesium Substances 0.000 description 1
- 229910052749 magnesium Inorganic materials 0.000 description 1
- 238000004137 mechanical activation Methods 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 239000005416 organic matter Substances 0.000 description 1
- 230000010355 oscillation Effects 0.000 description 1
- 239000003208 petroleum Substances 0.000 description 1
- 231100000614 poison Toxicity 0.000 description 1
- 230000007096 poisonous effect Effects 0.000 description 1
- 238000004064 recycling Methods 0.000 description 1
- 229910052604 silicate mineral Inorganic materials 0.000 description 1
- -1 silicon aluminate Chemical class 0.000 description 1
- 238000001988 small-angle X-ray diffraction Methods 0.000 description 1
- 235000019795 sodium metasilicate Nutrition 0.000 description 1
- NTHWMYGWWRZVTN-UHFFFAOYSA-N sodium silicate Chemical compound [Na+].[Na+].[O-][Si]([O-])=O NTHWMYGWWRZVTN-UHFFFAOYSA-N 0.000 description 1
- 229910052911 sodium silicate Inorganic materials 0.000 description 1
- 238000001179 sorption measurement Methods 0.000 description 1
- 239000007858 starting material Substances 0.000 description 1
- 239000004575 stone Substances 0.000 description 1
- 239000000758 substrate Substances 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
- 230000002194 synthesizing effect Effects 0.000 description 1
- 238000012360 testing method Methods 0.000 description 1
- 239000002351 wastewater Substances 0.000 description 1
- 239000002023 wood Substances 0.000 description 1
Classifications
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B37/00—Compounds having molecular sieve properties but not having base-exchange properties
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B39/00—Compounds having molecular sieve and base-exchange properties, e.g. crystalline zeolites; Their preparation; After-treatment, e.g. ion-exchange or dealumination
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2002/00—Crystal-structural characteristics
- C01P2002/70—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data
- C01P2002/72—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data by d-values or two theta-values, e.g. as X-ray diagram
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2002/00—Crystal-structural characteristics
- C01P2002/80—Crystal-structural characteristics defined by measured data other than those specified in group C01P2002/70
- C01P2002/82—Crystal-structural characteristics defined by measured data other than those specified in group C01P2002/70 by IR- or Raman-data
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/12—Surface area
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/16—Pore diameter
- C01P2006/17—Pore diameter distribution
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Life Sciences & Earth Sciences (AREA)
- Engineering & Computer Science (AREA)
- Chemical Kinetics & Catalysis (AREA)
- General Life Sciences & Earth Sciences (AREA)
- Geology (AREA)
- Materials Engineering (AREA)
- Silicates, Zeolites, And Molecular Sieves (AREA)
Abstract
The present invention relates to a kind of methods for preparing ordered mesoporous material Al-MCM-41 using attapulgite, comprising steps of, with the inorganic acid soak of moderate strength, obtaining acidification attapulgite using natural clay mineral attapulgite as raw material；It to be acidified attapulgite as raw material, is uniformly mixed with NaOH solid, high-temperature roasting activation；Deionized water is added in attapulgite after activation, takes upper layer leachate spare；Upper layer leachate is added in surfactant solution, autoclave is transferred to, hydrothermal crystallizing obtains presoma；Presoma filters, and washs, dry, roasting.The beneficial effects of the present invention are: being prepared using the attapulgite of acidification as raw material by chemical method, directly obtained with alkali process, silicon, silicon source is added without additional, the utilization rate of raw material is high, and production cost is low, and free from environmental pollution, low energy consumption；The pore-size distribution of ordered mesoporous material is concentrated, and pore performance is good, can quickly go hazardous contaminant-magenta in water removal.
Description
Technical field
The invention belongs to field of inorganic nonmetallic material, it is related to a kind of preparing ordered mesoporous material Al- using attapulgite
The method of MCM-41.
Background technique
Beck of Mobil company in 1992 et al. has synthesized M41S silicon base ordered mesopore material with organic silicon source, due to this
Material has the characteristics that the skeleton of big specific surface area, orderly cellular structure, adjustable aperture and nano-scale, makes it
Rapidly become one of the hot spot of catalysis material research.In petrochemical industry, mesoporous material is often used as the catalysis of PETROLEUM PROCESSING
The carrier of agent and catalyst.At the same time, due to high porosity and good hydrothermal stability, so that mesoporous
Material is more wide in Journal of Molecular Catalysis, the application prospect for the fields such as being selectively adsorbing and separating.
Currently, preparing silicon source used by silicon base ordered mesopore material is mostly existing chemical reagent, such as ethyl orthosilicate
(TEOS), methyl orthosilicate (TMOS) and sodium metasilicate etc., expensive starting materials and easily cause environmental pollution.And natural silicate mine
Object, it is resourceful, it is cheap, and it is rich in silicon, aluminium element, it is the desirable feedstock for preparing silicon-based mesoporous material on a large scale.Example
Such as, the Chinese patent application (CN 1765741A) of Yang Huaming etc. discloses a kind of side using preparing micro/mesoporous material using talc
Method carries out mechanical activation acidleach processing as raw material using natural talcum mineral and forms micro/meso porous material, and resulting materials granularity is equal
Even, average grain diameter is at 7 μm or so, and leaching effect is good, and leaching rate is up to 90% or more.In addition, the China of Yang Huaming etc.
Patent application (CN101643217A) also discloses a kind of method for preparing ordered mesoporous material using bentonite, preparation process
Simply, raw material is cheap and easy to get, and organic matter raw material concentration is low, free from environmental pollution, the specific surface area of prepared ordered mesoporous material
Reach as high as 1000m2/ g, Kong Rong can reach 1.00cm3/ g or more, pore-size distribution are concentrated.The Chinese patent application of Wu Ping night etc.
(CN101007635A) a kind of organic-pillared vermiculite mesoporous material and preparation method and application is then disclosed, vermiculite is through mesoporous column
After support, specific surface area is by 40m2/ g is increased to 280~360m2/ g, interlamination region are increased to 2.0~6.5nm by 1.50nm, absorption
Performance increases substantially.Recently, the Chinese patent application (CN 104016369A) of Du Chunfang etc. discloses a kind of using kaolin
Synthesizing high-stability ordered mesoporous material Al-SBA-15, the preparation process is simple, and raw material is easy to get, and the mesoporous material of synthesis has
Good hydrothermal stability and catalytic activity.
But in all kinds of natural silicate minerals, is there is no at present about exploitation Features of Attapulgite Minerals, prepare high-performance
The research of mesoporous Si-Al material is reported.Attapulgite is a kind of aqueous rich magnesium aluminium silicate mineral of crystalloid, due to being crystallized
The influence of many factors such as characteristic, form, depositional mode and internal gutter, mineral specific surface area with higher, in addition its
Charge unbalance phenomenon existing for surface, so that it is with good absorption property.Features of Attapulgite Minerals is resourceful, but comprehensive
It closes and utilizes level lower, therefore, using natural attapulgite as raw material, silicon substrate Al-MCM-41 ordered mesoporous material is prepared, to excellent
Change the comprehensive utilization of Features of Attapulgite Minerals resource and promote economic development and has important practical significance.
Summary of the invention
The technical problem to be solved by the present invention is based on the above issues, the present invention provides a kind of utilization attapulgite preparation
The method of ordered mesoporous material Al-MCM-41.
The present invention solves a technical solution used by its technical problem: a kind of prepared using attapulgite is orderly situated between
The method of Porous materials Al-MCM-41, comprising the following steps:
(1) it using natural clay mineral attapulgite as raw material, with 60 DEG C of immersion 12h of inorganic acid of moderate strength, filters,
It is washed repeatedly with deionized water to neutrality, 80 DEG C of dryings, obtains acidification attapulgite；
(2) it to be acidified attapulgite as raw material, is uniformly mixed with NaOH solid, 550~600 DEG C of high-temperature roasting activation 3~
5h；
(3) under room temperature, deionized water is added in the attapulgite after activation, mechanical stirring for 24 hours, takes upper layer leachate conduct
Silicon and aluminum source is spare；
(4) upper layer leachate obtained by step (3) is added in surfactant solution, adjusting mixed solution pH value is 3
~9,1h is stirred, is transferred to autoclave, 60~210 DEG C of 6~48h of hydrothermal crystallizing obtain presoma；
(5) the resulting presoma of step (4) is filtered, washing, 80 DEG C of dryings, 550 DEG C of 4~5h of roasting, removal surface is living
Property agent, be made Al-MCM-41 ordered mesoporous material.
Further, in step (1) inorganic acid of moderate strength be 6mol/L HCl.
Further, the additional amount of NaOH solid is 1~2 times for being acidified attapulgite quality in step (2).
Further, in step (3) deionized water additional amount be every 1g activate attapulgite be added 5~10ml go from
Sub- water.
Further, surfactant is CTAB, CTAB and SiO in system in step (4)2Mass ratio be 0.05~
0.5:1.
The beneficial effects of the present invention are: (1) present invention is to prepare using the attapulgite of acidification as raw material by chemical method
High stability ordered mesoporous material Al-MCM-41, is directly obtained with alkali process, and silicon, silicon source, the utilization of raw material is added without additional
Rate is high, and production cost is low, while having widened the application range of attapulgite, can be used for producing the mineral base composite wood of high added value
Material；
(2) present invention process is simple, and raw material is cheap and easy to get, and preparation condition is loose, free from environmental pollution, and low energy consumption；
(3) specific surface area of Al-MCM-41 ordered mesoporous material prepared by the invention is up to 998m2/ g, pore volume can
Reach 0.80cm3/ g or more, pore-size distribution are concentrated, and pore performance is good；
(4) with magenta (60~120mg/L) dye wastewater containing higher concentration, evaluation prepares resulting Al-
MCM-41 ordered mesoporous material, the experimental results showed that, the absorption property of the material is higher, can quickly go poisonous and harmful in water removal
Pollutant-magenta.
Detailed description of the invention
The following further describes the present invention with reference to the drawings.
Fig. 1 is the small angle X-ray diffraction figure of the Al-MCM-41 prepared, wherein (a): different CTAB/SiO2Mass ratio
Value: (1) 0.05, (2) 0.1, (3) 0.3, (4) 0.5；(b): different mixed solution pH value: (5) pH=3, (6) pH=5, (7)
PH=7, (8) pH=9；(c): different hydrothermal crystallizing temperature: (9) 60 DEG C, (10) 110 DEG C, (11) 160 DEG C, (12) 210 DEG C；
(d): the different hydrothermal crystallizing time: (13) 6h, (14) 12h, (15) for 24 hours, (16) 48h；
Fig. 2 is to work as CTAB/SiO2Mass values be 0.1 when, (a): N of the Al-MCM-41 of preparation2Adsorption-desorption isothermal
Line；(b): BJH pore size distribution curve；
Fig. 3 is scanning electron microscope diagram, wherein (a): natural attapulgite；(b): acidification attapulgite；(c) and
(d): Al-MCM-41 mesoporous material；
Fig. 4 is the x-ray photoelectron spectroscopy figure for being acidified attapulgite and Al-MCM-41 mesoporous material, wherein (a): Quan Pu
Scanning；(b): Al 2p；(c): Si 2p；(d): O 1s；
Fig. 5 is the fourier infrared spectrogram of Al-MCM-41 mesoporous material, wherein (a): before absorption is pinkish red；(b): absorbent articles
After red；
Fig. 6 is Al-MCM-41 after absorption is pinkish red after the ammonium acetate solution recycling elution of various concentration, fuchsin solution
Adsorption-desorption concentration map, wherein the initial concentration of fuchsin solution is 60mg/L, and adsorbent inventory is 1g/L, temperature 25
DEG C, (a): absorption is pinkish red；(b): desorption is pinkish red.
Specific embodiment
Presently in connection with specific embodiment, the invention will be further described, following embodiment be intended to illustrate invention rather than
Limitation of the invention further.
Embodiment 1
The Concave-convex clay rod for weighing 4 parts of 20g respectively impregnates 12h with the HCl of 80ml 6mol/L at 60 DEG C, filter,
Deionized water is washed repeatedly to neutrality, must be acidified attapulgite 18.2g after 80 DEG C of dryings.The acidification for weighing 4 parts of 10g respectively is concave-convex
Stick stone is uniformly mixed, with 15g NaOH solid abrasive in 600 DEG C of roasting 5h.Mixture after roasting has been transferred to respectively and has been stirred
In the container mixed, deionized water 65ml is added, stirring for 24 hours, dissolves soluble silicon aluminate therein sufficiently, takes the leaching on upper layer
Liquid is spare as silicon and aluminum source out.
It is 0.5g, 1.0g, 3.0g that above-mentioned 4 parts of silicon and aluminum sources, which are separately added into containing Surfactant CTAB, in the solution of 5.0g.
The pH=5 of above-mentioned mixed solution is adjusted with the HCl of 0.1mol/L, after stirring 1h, is transferred in 4 autoclaves respectively.110
Hydrothermal crystallizing 12h at a temperature of DEG C, obtains presoma, which is filtered, washing, dry, 550 DEG C of roastings removal surface-actives
Agent, obtains Al-MCM-41 1~4# of ordered mesoporous material, surface nature (including specific surface area, pore volume and aperture number
According to) it is shown in Table 1.
Embodiment 2
According to identical method in embodiment 1, then the useful silicon and aluminum source in 4 parts of activation attapulgites is extracted respectively.It will be upper
It states 4 parts of silicon and aluminum sources to be separately added into the solution for being 1.0g containing Surfactant CTAB.Above-mentioned mixing is adjusted with the HCl of 0.1mol/L
The pH=3 of solution, pH=5, pH=7, pH=9.After stirring 1h, it is transferred in 4 autoclaves respectively.In 110 DEG C of temperature
Lower hydrothermal crystallizing 12h, obtains presoma, which is filtered, washing, drying, and 550 DEG C of roastings remove surfactants, that is, make
5~8# of Al-MCM-41 ordered mesoporous material is obtained, surface nature is shown in Table 1.
Embodiment 3
According to identical method in embodiment 1, then the useful silicon and aluminum source in 4 parts of activation attapulgites is extracted respectively.It will be upper
It states 4 parts of silicon and aluminum sources to be separately added into the solution for being 1.0g containing Surfactant CTAB.Above-mentioned mixing is adjusted with the HCl of 0.1mol/L
The pH=5 of solution.After stirring 1h, it is transferred in 4 autoclaves respectively.The temperature at 60,110,160,210 DEG C is lauched respectively
Thermal crystallisation 12h, obtains presoma, which is filtered, washing, drying, and 550 DEG C of roastings remove surfactants, obtain Al-
MCM-41 9~12# of ordered mesoporous material, surface nature are shown in Table 1.
Embodiment 4
According to identical method in embodiment 1, then the useful silicon and aluminum source in 4 parts of activation attapulgites is extracted respectively.
Above-mentioned 4 parts of silicon and aluminum sources are separately added into the solution for being 1.0g containing Surfactant CTAB.With the HCl of 0.1mol/L
Adjust the pH=5 of above-mentioned mixed solution.After stirring 1h, it is transferred in 4 autoclaves respectively.Respectively 110 DEG C at a temperature of
Hydrothermal crystallizing 6,12,24,48h, obtain presoma, which are filtered, washing, dry, 550 DEG C of roastings removal surface-actives
Agent, obtains Al-MCM-41 13~16# of ordered mesoporous material, and surface nature is shown in Table 1.
Comparative example 1
Table 1 lists the surface nature and adsorbing and removing water of the 1-16# ordered mesoporous material of above-mentioned different process preparation
The performance of middle higher concentration magenta compares.Comparative test condition: adsorption reaction carries out on water bath with thermostatic control shaking table, frequency of oscillation
150rpm, 25 DEG C of reaction temperature, pH value 6.5, the inventory of adsorbent is 0.05g, and the initial concentration of fuchsin solution is 80mg/
L。
Pinkish red removal efficiency is calculated using following formula:
Pinkish red removal efficiency=(the pinkish red concentration after pinkish red initial concentration-absorption)/magenta initial concentration × 100%.
The surface nature of 1 ordered mesoporous material Al-MCM-41 of table and pinkish red removal efficiency is compared
Taking the above-mentioned ideal embodiment according to the present invention as inspiration, through the above description, relevant staff is complete
Various changes and amendments can be carried out without departing from the scope of the technological thought of the present invention' entirely.The technology of this invention
Property range is not limited to the contents of the specification, it is necessary to which the technical scope thereof is determined according to the scope of the claim.
Claims (5)
1. a kind of method for preparing ordered mesoporous material Al-MCM-41 using attapulgite, it is characterized in that: the following steps are included:
(1) it using natural clay mineral attapulgite as raw material, with 60 DEG C of immersion 12h of HCl, filters, is washed repeatedly with deionized water
It washs to neutrality, 80 DEG C of dryings, obtains acidification attapulgite；
(2) it to be acidified attapulgite as raw material, is uniformly mixed with NaOH solid, 550~600 DEG C of high-temperature roastings activate 3~5h；
(3) under room temperature, deionized water is added in the attapulgite after activation, mechanical stirring for 24 hours, takes upper layer leachate as sial
Source is spare；
(4) upper layer leachate obtained by step (3) is added in surfactant solution, adjusting mixed solution pH value is 3~9,
1h is stirred, is transferred to autoclave, 60~210 DEG C of 6~48h of hydrothermal crystallizing obtain presoma；
(5) the resulting presoma of step (4) is filtered, washing, 80 DEG C of dryings, 550 DEG C of roasting 4~5h, obtained Al-MCM-41 have
Sequence mesoporous material.
2. a kind of method for preparing ordered mesoporous material Al-MCM-41 using attapulgite according to claim 1, special
Sign is: HCl concentration is 6mol/L in the step (1).
3. a kind of method for preparing ordered mesoporous material Al-MCM-41 using attapulgite according to claim 1, special
Sign is: the additional amount of NaOH solid is 1~2 times for being acidified attapulgite quality in the step (2).
4. a kind of method for preparing ordered mesoporous material Al-MCM-41 using attapulgite according to claim 1, special
Sign is: the additional amount of deionized water is the deionized water that every 1g activates that 5~10ml is added in attapulgite in the step (3).
5. a kind of method for preparing ordered mesoporous material Al-MCM-41 using attapulgite according to claim 1,
Be characterized in: surfactant is CTAB, CTAB and SiO in system in the step (4)2Mass ratio be 0.05~0.5:
1。
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| CN107128948B (en) * | 2017-05-09 | 2020-05-26 | 西安工程大学 | Preparation method of mesoporous molecular sieve MCM-41 |
| CN108190906A (en) * | 2018-01-23 | 2018-06-22 | 浙江睿升环保科技有限公司 | A kind of method that ordered mesoporous material SBA-16 is prepared using attapulgite |
| CN108745274B (en) * | 2018-05-29 | 2021-08-03 | 武汉大学 | Rectorite mesoporous material and preparation method and application thereof |
| CN112264085B (en) * | 2020-11-23 | 2022-06-14 | 淮阴工学院 | Solid base catalyst KF/Mg-Al-LDO/MCM-41 and preparation method and application thereof |
| CN117019088B (en) * | 2023-08-11 | 2024-06-25 | 生态环境部南京环境科学研究所 | Ordered mesoporous material loaded nano zero-valent iron material, and preparation method and application thereof |
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