CN109970069A - A kind of preparation method of high catalytic efficiency multi-stage porous silica - Google Patents
A kind of preparation method of high catalytic efficiency multi-stage porous silica Download PDFInfo
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- CN109970069A CN109970069A CN201910361207.4A CN201910361207A CN109970069A CN 109970069 A CN109970069 A CN 109970069A CN 201910361207 A CN201910361207 A CN 201910361207A CN 109970069 A CN109970069 A CN 109970069A
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- porous silica
- high catalytic
- catalytic efficiency
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- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 title claims abstract description 102
- 239000000377 silicon dioxide Substances 0.000 title claims abstract description 50
- 230000003197 catalytic effect Effects 0.000 title claims abstract description 42
- 238000002360 preparation method Methods 0.000 title claims abstract description 24
- 239000007788 liquid Substances 0.000 claims abstract description 33
- 239000000203 mixture Substances 0.000 claims abstract description 27
- BOTDANWDWHJENH-UHFFFAOYSA-N Tetraethyl orthosilicate Chemical compound CCO[Si](OCC)(OCC)OCC BOTDANWDWHJENH-UHFFFAOYSA-N 0.000 claims abstract description 25
- 239000012046 mixed solvent Substances 0.000 claims abstract description 20
- 238000001914 filtration Methods 0.000 claims abstract description 18
- 229920001495 poly(sodium acrylate) polymer Polymers 0.000 claims abstract description 18
- NNMHYFLPFNGQFZ-UHFFFAOYSA-M sodium polyacrylate Chemical compound [Na+].[O-]C(=O)C=C NNMHYFLPFNGQFZ-UHFFFAOYSA-M 0.000 claims abstract description 18
- 239000000654 additive Substances 0.000 claims abstract description 13
- 230000000996 additive effect Effects 0.000 claims abstract description 13
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 claims abstract description 8
- 239000000908 ammonium hydroxide Substances 0.000 claims abstract description 8
- 239000012263 liquid product Substances 0.000 claims abstract description 8
- 238000005406 washing Methods 0.000 claims abstract description 3
- 239000000243 solution Substances 0.000 claims description 62
- 239000011259 mixed solution Substances 0.000 claims description 39
- WQZGKKKJIJFFOK-GASJEMHNSA-N Glucose Natural products OC[C@H]1OC(O)[C@H](O)[C@@H](O)[C@@H]1O WQZGKKKJIJFFOK-GASJEMHNSA-N 0.000 claims description 32
- 239000008103 glucose Substances 0.000 claims description 31
- 229920002518 Polyallylamine hydrochloride Polymers 0.000 claims description 29
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 25
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 20
- UIIMBOGNXHQVGW-UHFFFAOYSA-M Sodium bicarbonate Chemical compound [Na+].OC([O-])=O UIIMBOGNXHQVGW-UHFFFAOYSA-M 0.000 claims description 20
- 239000003638 chemical reducing agent Substances 0.000 claims description 19
- 238000002156 mixing Methods 0.000 claims description 15
- 238000001354 calcination Methods 0.000 claims description 14
- 239000012299 nitrogen atmosphere Substances 0.000 claims description 13
- 239000000706 filtrate Substances 0.000 claims description 12
- 150000002303 glucose derivatives Chemical class 0.000 claims description 12
- 229910000030 sodium bicarbonate Inorganic materials 0.000 claims description 10
- 235000017557 sodium bicarbonate Nutrition 0.000 claims description 10
- 239000012298 atmosphere Substances 0.000 claims description 7
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims description 7
- 239000001768 carboxy methyl cellulose Substances 0.000 claims description 7
- 230000008859 change Effects 0.000 claims description 7
- 229960000935 dehydrated alcohol Drugs 0.000 claims description 7
- WBZKQQHYRPRKNJ-UHFFFAOYSA-L disulfite Chemical compound [O-]S(=O)S([O-])(=O)=O WBZKQQHYRPRKNJ-UHFFFAOYSA-L 0.000 claims description 7
- 235000019441 ethanol Nutrition 0.000 claims description 7
- 239000001301 oxygen Substances 0.000 claims description 7
- 229910052760 oxygen Inorganic materials 0.000 claims description 7
- 239000001230 potassium iodate Substances 0.000 claims description 7
- 235000006666 potassium iodate Nutrition 0.000 claims description 7
- JLKDVMWYMMLWTI-UHFFFAOYSA-M potassium iodate Chemical compound [K+].[O-]I(=O)=O JLKDVMWYMMLWTI-UHFFFAOYSA-M 0.000 claims description 7
- 229940093930 potassium iodate Drugs 0.000 claims description 7
- KDLHZDBZIXYQEI-UHFFFAOYSA-N Palladium Chemical compound [Pd] KDLHZDBZIXYQEI-UHFFFAOYSA-N 0.000 claims description 6
- ZLMJMSJWJFRBEC-UHFFFAOYSA-N Potassium Chemical compound [K] ZLMJMSJWJFRBEC-UHFFFAOYSA-N 0.000 claims description 6
- DPXJVFZANSGRMM-UHFFFAOYSA-N acetic acid;2,3,4,5,6-pentahydroxyhexanal;sodium Chemical compound [Na].CC(O)=O.OCC(O)C(O)C(O)C(O)C=O DPXJVFZANSGRMM-UHFFFAOYSA-N 0.000 claims description 6
- 229960004756 ethanol Drugs 0.000 claims description 6
- 238000000034 method Methods 0.000 claims description 6
- 229910052700 potassium Inorganic materials 0.000 claims description 6
- 239000011591 potassium Substances 0.000 claims description 6
- 239000012279 sodium borohydride Substances 0.000 claims description 6
- 229910000033 sodium borohydride Inorganic materials 0.000 claims description 6
- 235000019812 sodium carboxymethyl cellulose Nutrition 0.000 claims description 6
- 229920001027 sodium carboxymethylcellulose Polymers 0.000 claims description 6
- FDWREHZXQUYJFJ-UHFFFAOYSA-M gold monochloride Chemical compound [Cl-].[Au+] FDWREHZXQUYJFJ-UHFFFAOYSA-M 0.000 claims description 5
- WDIHJSXYQDMJHN-UHFFFAOYSA-L barium chloride Chemical compound [Cl-].[Cl-].[Ba+2] WDIHJSXYQDMJHN-UHFFFAOYSA-L 0.000 claims description 4
- 229910001626 barium chloride Inorganic materials 0.000 claims description 4
- 239000002253 acid Substances 0.000 claims description 3
- 229910052763 palladium Inorganic materials 0.000 claims description 3
- 230000008569 process Effects 0.000 claims description 3
- 238000010000 carbonizing Methods 0.000 claims description 2
- 239000000463 material Substances 0.000 abstract description 19
- 238000005516 engineering process Methods 0.000 abstract description 13
- 239000007783 nanoporous material Substances 0.000 abstract description 4
- 238000011161 development Methods 0.000 abstract description 2
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 30
- 239000000047 product Substances 0.000 description 23
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 15
- 229910052757 nitrogen Inorganic materials 0.000 description 15
- 238000006243 chemical reaction Methods 0.000 description 11
- 239000012065 filter cake Substances 0.000 description 10
- 230000000694 effects Effects 0.000 description 8
- 229920001971 elastomer Polymers 0.000 description 6
- 230000003712 anti-aging effect Effects 0.000 description 5
- 229920003023 plastic Polymers 0.000 description 5
- 239000004033 plastic Substances 0.000 description 5
- 238000004321 preservation Methods 0.000 description 5
- 239000003292 glue Substances 0.000 description 4
- VVJKKWFAADXIJK-UHFFFAOYSA-N Allylamine Chemical compound NCC=C VVJKKWFAADXIJK-UHFFFAOYSA-N 0.000 description 3
- ZAMOUSCENKQFHK-UHFFFAOYSA-N Chlorine atom Chemical compound [Cl] ZAMOUSCENKQFHK-UHFFFAOYSA-N 0.000 description 3
- 229910052788 barium Inorganic materials 0.000 description 3
- DSAJWYNOEDNPEQ-UHFFFAOYSA-N barium atom Chemical compound [Ba] DSAJWYNOEDNPEQ-UHFFFAOYSA-N 0.000 description 3
- 239000000460 chlorine Substances 0.000 description 3
- 229910052801 chlorine Inorganic materials 0.000 description 3
- 239000011248 coating agent Substances 0.000 description 3
- 238000000576 coating method Methods 0.000 description 3
- 230000000052 comparative effect Effects 0.000 description 3
- 229910021645 metal ion Inorganic materials 0.000 description 3
- 235000012239 silicon dioxide Nutrition 0.000 description 3
- 238000012360 testing method Methods 0.000 description 3
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 description 2
- 229920002943 EPDM rubber Polymers 0.000 description 2
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 description 2
- 230000032683 aging Effects 0.000 description 2
- 230000015572 biosynthetic process Effects 0.000 description 2
- 239000006229 carbon black Substances 0.000 description 2
- 239000000805 composite resin Substances 0.000 description 2
- 238000001514 detection method Methods 0.000 description 2
- 239000003814 drug Substances 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 229910052751 metal Inorganic materials 0.000 description 2
- 239000002184 metal Substances 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 239000002086 nanomaterial Substances 0.000 description 2
- 230000003287 optical effect Effects 0.000 description 2
- 239000011347 resin Substances 0.000 description 2
- 229920005989 resin Polymers 0.000 description 2
- 229910052708 sodium Inorganic materials 0.000 description 2
- 239000011734 sodium Substances 0.000 description 2
- 239000002904 solvent Substances 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- PQUXFUBNSYCQAL-UHFFFAOYSA-N 1-(2,3-difluorophenyl)ethanone Chemical compound CC(=O)C1=CC=CC(F)=C1F PQUXFUBNSYCQAL-UHFFFAOYSA-N 0.000 description 1
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 1
- 229920002134 Carboxymethyl cellulose Polymers 0.000 description 1
- 239000004593 Epoxy Substances 0.000 description 1
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 1
- 229920002292 Nylon 6 Polymers 0.000 description 1
- 239000004743 Polypropylene Substances 0.000 description 1
- 239000004793 Polystyrene Substances 0.000 description 1
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 1
- 241000219095 Vitis Species 0.000 description 1
- 235000009754 Vitis X bourquina Nutrition 0.000 description 1
- 235000012333 Vitis X labruscana Nutrition 0.000 description 1
- 235000014787 Vitis vinifera Nutrition 0.000 description 1
- 238000005299 abrasion Methods 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- 230000009471 action Effects 0.000 description 1
- 150000001298 alcohols Chemical class 0.000 description 1
- 238000004458 analytical method Methods 0.000 description 1
- 229920006318 anionic polymer Polymers 0.000 description 1
- 239000003242 anti bacterial agent Substances 0.000 description 1
- 229940088710 antibiotic agent Drugs 0.000 description 1
- 239000012752 auxiliary agent Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000003115 biocidal effect Effects 0.000 description 1
- 230000005540 biological transmission Effects 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- 235000010948 carboxy methyl cellulose Nutrition 0.000 description 1
- 239000008112 carboxymethyl-cellulose Substances 0.000 description 1
- 238000006555 catalytic reaction Methods 0.000 description 1
- 239000000919 ceramic Substances 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 229910052681 coesite Inorganic materials 0.000 description 1
- 239000002537 cosmetic Substances 0.000 description 1
- 229910052906 cristobalite Inorganic materials 0.000 description 1
- 230000018109 developmental process Effects 0.000 description 1
- 230000000857 drug effect Effects 0.000 description 1
- 235000013399 edible fruits Nutrition 0.000 description 1
- 238000006056 electrooxidation reaction Methods 0.000 description 1
- 229920006351 engineering plastic Polymers 0.000 description 1
- 150000002148 esters Chemical class 0.000 description 1
- 229940056319 ferrosoferric oxide Drugs 0.000 description 1
- 239000011152 fibreglass Substances 0.000 description 1
- 238000000892 gravimetry Methods 0.000 description 1
- 238000006197 hydroboration reaction Methods 0.000 description 1
- 239000001257 hydrogen Substances 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- 238000009413 insulation Methods 0.000 description 1
- WTFXARWRTYJXII-UHFFFAOYSA-N iron(2+);iron(3+);oxygen(2-) Chemical compound [O-2].[O-2].[O-2].[O-2].[Fe+2].[Fe+3].[Fe+3] WTFXARWRTYJXII-UHFFFAOYSA-N 0.000 description 1
- SZVJSHCCFOBDDC-UHFFFAOYSA-N iron(II,III) oxide Inorganic materials O=[Fe]O[Fe]O[Fe]=O SZVJSHCCFOBDDC-UHFFFAOYSA-N 0.000 description 1
- JEIPFZHSYJVQDO-UHFFFAOYSA-N iron(III) oxide Inorganic materials O=[Fe]O[Fe]=O JEIPFZHSYJVQDO-UHFFFAOYSA-N 0.000 description 1
- 230000031700 light absorption Effects 0.000 description 1
- 239000011159 matrix material Substances 0.000 description 1
- 125000000325 methylidene group Chemical group [H]C([H])=* 0.000 description 1
- 238000004377 microelectronic Methods 0.000 description 1
- 229910000510 noble metal Inorganic materials 0.000 description 1
- 231100000252 nontoxic Toxicity 0.000 description 1
- 230000003000 nontoxic effect Effects 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 238000011056 performance test Methods 0.000 description 1
- 229920000083 poly(allylamine) Polymers 0.000 description 1
- -1 polypropylene Polymers 0.000 description 1
- 229920001155 polypropylene Polymers 0.000 description 1
- 229920002223 polystyrene Polymers 0.000 description 1
- 239000011148 porous material Substances 0.000 description 1
- 239000000843 powder Substances 0.000 description 1
- 230000005610 quantum mechanics Effects 0.000 description 1
- 230000009467 reduction Effects 0.000 description 1
- 230000004043 responsiveness Effects 0.000 description 1
- 150000003839 salts Chemical class 0.000 description 1
- 239000000565 sealant Substances 0.000 description 1
- 238000007789 sealing Methods 0.000 description 1
- RMAQACBXLXPBSY-UHFFFAOYSA-N silicic acid Chemical compound O[Si](O)(O)O RMAQACBXLXPBSY-UHFFFAOYSA-N 0.000 description 1
- 229910052710 silicon Inorganic materials 0.000 description 1
- 239000010703 silicon Substances 0.000 description 1
- 229940047670 sodium acrylate Drugs 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 238000007711 solidification Methods 0.000 description 1
- 230000008023 solidification Effects 0.000 description 1
- 238000011895 specific detection Methods 0.000 description 1
- 229910052682 stishovite Inorganic materials 0.000 description 1
- 239000000725 suspension Substances 0.000 description 1
- 230000009967 tasteless effect Effects 0.000 description 1
- 229910052905 tridymite Inorganic materials 0.000 description 1
- 230000005641 tunneling Effects 0.000 description 1
- 238000005303 weighing Methods 0.000 description 1
Classifications
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J21/00—Catalysts comprising the elements, oxides, or hydroxides of magnesium, boron, aluminium, carbon, silicon, titanium, zirconium, or hafnium
- B01J21/06—Silicon, titanium, zirconium or hafnium; Oxides or hydroxides thereof
- B01J21/08—Silica
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J35/00—Catalysts, in general, characterised by their form or physical properties
- B01J35/60—Catalysts, in general, characterised by their form or physical properties characterised by their surface properties or porosity
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B33/00—Silicon; Compounds thereof
- C01B33/113—Silicon oxides; Hydrates thereof
- C01B33/12—Silica; Hydrates thereof, e.g. lepidoic silicic acid
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Inorganic Chemistry (AREA)
- Catalysts (AREA)
Abstract
The invention discloses a kind of preparation methods of high catalytic efficiency multi-stage porous silica, belong to nano-porous materials preparation technical field.Sodium Polyacrylate is mixed with microgel 1:5~1:6 in mass ratio, and 20~30 times of Sodium Polyacrylate quality of mixed solvent and 0.2~0.6 times of Sodium Polyacrylate quality of additive is added, after being stirred, obtain template liquid, template liquid is mixed with ethyl orthosilicate volume of mixture ratio 10:1~15:1, and the ammonium hydroxide of 0.1~0.4 times of template liquid product is added, after being stirred to react, filtering, washing, it is dry, obtain blank, after blank is calcined, high catalytic efficiency multi-stage porous silica is obtained.The high catalytic efficiency multi-stage porous silica materials of technical solution of the present invention preparation have the characteristics that excellent porosity and catalytic performance, have broad prospects in the development of nano-porous materials technology industry.The high catalytic efficiency multi-stage porous silica materials of technical solution of the present invention preparation have the characteristics that excellent porosity and catalytic performance.
Description
Technical field
The invention discloses a kind of preparation methods of high catalytic efficiency multi-stage porous silica, belong to nano-porous materials system
Standby technical field.
Background technique
Nanoscale science and technology is the science and technology that substance is manufactured with single atom, molecule.Nanoscale science and technology is with many
Science and technology based on modern advanced science and technology, it is modern science (chaos physics, quantum mechanics, mesoscopic physics, molecule
Biology) and modern technologies (computer technology, microelectronics and scanning tunneling microscope technology, Nuclear analysis techniques) combine production
Object, nanoscale science and technology will cause a series of new science and technology, such as nanoelectronics, nanometer material science, nanometer machine again
Tool etc., nanoscale science and technology are considered as the high-tech occurred the turn of the century.Nano material refers in three dimensions,
At least one dimension is in the range namely 1~100 nanometer of range of nano-scale.Nano material has small-size effect, surface
Effect and macroscopic quantum are answered with drug effect, thus show many distinctive properties, are situated between in catalysis, optical filtering, light absorption, medicine, magnetic
Matter and new material etc. have wide practical use.The purposes of nano silica point is very extensive, and general weight of adding is 0.5-
2%, individual product system can be to 10% or more.The key embodied to properties of product is: fully dispersed in system.Root when use
According to different systems, nano silica is dispersed in water, acetone, alcohols or other solvents in advance, it, can for oleaginous system
It is aided with auxiliary agent to pre-process.It is used primarily in following field,
(1) nano silica after surface-active-treatment is well dispersed in silicon-modified epoxy tree by electronic package material
Rouge encapsulates in gel matrix, can significantly shorten encapsulating material curing time (for 2.0-2.5h), and solidification temperature can reduce
To room temperature, device sealing performance is made to be significantly improved, increases the service life of device.
Nanometer silicon dioxide particle is sufficiently and uniformly distributed in resin material by resin composite materials, can be improved comprehensively
Resin-based materials performance.It include: that A improves intensity and elongation percentage；B improves wearability and improves the finish of material surface；C is anti-ageing
Change performance.
Plastics are small using nano silica light transmission, granularity, plastics can be made to become finer and close, in polystyrene plastics
After adding silica in film, its transparency, intensity, toughness, waterproof performance and anti-aging property can be improved.Utilize nanometer two
Silica is modified common plastics polypropylene, make its key technical indexes (water absorption rate, insulation resistance, permanent compressive deformation,
Flexural strength etc.) meet or exceed the performance indicator of engineering plastic nylon 6.
The suspension stability that coating can improve coating is poor, thixotropy is poor, weatherability is poor, abrasion resistance difference etc., make film with
Wall bond strength greatly improves, and hardness of film increases, and clean surfaces ability is also improved.
Rubber silica is known as white carbon black, the intensity of product, wear-resisting after a small amount of nano Si 02 is added in General Purpose Rubber
The performances such as property and ageing resistance meet or exceed high-grade rubber product, and can keep color permanency.Nano modification
Colored EPDM waterproof rolled sheet, wearability, tensile strength, fold resistance, anti-aging property are obviously improved, and color is fresh
It is gorgeous, protect color excellent effect.
Nano silica is a kind of inorganic chemical industry material, is commonly called as white carbon black.Due to being ultrafine nanometer, size range exists
1~100nm, therefore there are many unique properties, such as have to anti-ultraviolet optical property, it is anti-ageing other materials to be improved
Change, intensity and chemical-resistance.Purposes is very extensive.Nanometer grade silica is amorphous white powder, nontoxic, tasteless, nothing
Pollution, micro-structure is spherical shape, and in cotton-shaped and netted quasi- grain structure, molecular formula and structural formula are SiO2, not soluble in water.Nanometer
The purposes of silica point is very extensive, and for general weight of adding in 0.5-2%, individual systems can be to 10% or more.Be used primarily in
Lower field: electronic package material, resin composite materials, plastics, coating, face (dye) material, ceramics, sealant, glass fiber reinforced plastics product, medicine
Object carrier, cosmetics, anti-biotic material, rubber etc..It is the intensity of product, wear-resisting after adding a small amount of nano Si 02 in General Purpose Rubber
The performances such as property and ageing resistance meet or exceed high-grade rubber product, and can keep color permanency.Nano modification
Colored EPDM waterproof rolled sheet, wearability, tensile strength, fold resistance, anti-aging property are obviously improved, and color is fresh
It is gorgeous, protect color excellent effect.
What high catalytic efficiency multi-stage porous silica hole rate and catalytic performance traditional at present can not further increase asks
Topic, developing the high catalytic efficiency multi-stage porous silica with good comprehensive performance in the hope of exploration is problem to be solved.
Summary of the invention
The present invention solves the technical problem of: for traditional high catalytic efficiency multi-stage porous silica hole rate and
The problem of catalytic performance can not be promoted further provides a kind of preparation method of high catalytic efficiency multi-stage porous silica.
In order to solve the above-mentioned technical problem, the technical scheme adopted by the invention is that:
A kind of preparation method of high catalytic efficiency multi-stage porous silica, it is specific the preparation method comprises the following steps:
(1) pretreatment glucose mixed liquor is mixed with barium chloride solution 1:3~1:5 in mass ratio, filters, obtains filtrate, will filter
Liquid is mixed with metabisulfite solution 1:3~1:4 in mass ratio, and filtering obtains modified glucose solution；
(2) polyallylamine hydrochlorides are mixed with water 1:100~1:110 in mass ratio, obtains polyallylamine hydrochlorides solution, adjusted
The pH to 9.8~10.0 of polyallylamine hydrochlorides solution, and be added 0.5~1.3 times of polyallylamine hydrochlorides solution quality and change
Property glucose solution after being stirred, obtains mixed solution under nitrogen atmosphere；
(3) mixed solution is mixed with reducing agent 400:1~500:1 in mass ratio, under nitrogen atmosphere, after being stirred to react, mistake
Filter, washing, obtains microgel；
(4) Sodium Polyacrylate is mixed with microgel 1:5~1:6 in mass ratio, and is added 20~30 times of Sodium Polyacrylate quality
Mixed solvent and 0.2~0.6 times of Sodium Polyacrylate quality of additive, after being stirred, obtain template liquid, by template liquid with just
Silester volume of mixture ratio 10:1~15:1 mixing, and the ammonium hydroxide of 0.1~0.4 times of template liquid product is added, it is stirred to react
Afterwards, it filters, washs, it is dry, blank is obtained, after blank is calcined, obtains high catalytic efficiency multi-stage porous silica.
Step (1) the pretreatment glucose mixed liquor be glucose is mixed with water 1:20~1:25 in mass ratio, and
0.1~0.2 times of glucose quality of Potassiumiodate is added, under nitrogen atmosphere, after being stirred to react, glucose mixing must be pre-processed
Liquid.
Step (3) reducing agent is any one in sodium borohydride or potassium borohydride.
Step (4) mixed solvent is to mix ethyl alcohol with water 6:1~8:1 in mass ratio, obtains mixed solvent.
Step (4) additive is any one in gold chloride or palladium acid potassium.
Step (4) the ethyl orthosilicate mixture is by ethyl orthosilicate and dehydrated alcohol 10:1~10:3 in mass ratio
Mixing, obtains ethyl orthosilicate mixture.
Step (4) calcining manners be prior under nitrogen atmosphere, under conditions of 250~400 DEG C, heat preservation charing 2~
After 3h, under oxygen atmosphere, under conditions of 450~550 DEG C, 1~3h of calcining at constant temperature.
0.1~0.2 times of quality in mixed solution of sodium bicarbonate and mixed solution are added in step (3) described mixed solution
The fe that 0.02~0.04 times of quality.
The sodium carboxymethylcellulose of template liquid quality 0.1~0.2 can be added in step (4) the template liquid.
The beneficial effects of the present invention are:
(1) microgel and Sodium Polyacrylate are added when preparing high catalytic efficiency multi-stage porous silica by the present invention, firstly, micro- solidifying
The addition of glue can be used as template, so that silica is had porous structure, also, since microgel has pH responsiveness, not
With different degrees of expansion can occur under alkaline pH, so as to form different mesoporous of pore size in silica interior
Structure, and then make the hole of product formation that hierarchical porous structure abundant be presented, and specific surface area increases, improve the use effect of product
Fruit；Secondly, the Sodium Polyacrylate being added in the product be anionic polymer template, after being mixed with microgel, can with it is micro-
Gel forms certain network structure under the action of electrostatic force in preparation system, thus in high catalytic efficiency multi-stage porous two
When prepared by silica, make to improve the multistage of product containing more abundant and connection microcellular structure around product meso-hole structure
Property, and further increase the porosity of product and specific surface area, and then further increase the using effect of product；
(2) additive is added when preparing high catalytic efficiency multi-stage porous silica by the present invention, and additive is being added in addition production
After in the preparation system of product, the metal ion complex with negative electrical charge can be ionized out in system, and can be in electrostatic force
It is adsorbed in inside microgel under effect, during carburising step in product preparation process, metal ion complex can be by Portugal
The carbon that grape sugar charcoalization is formed is restored, to form precipitated metal in interiors of products, the precipitated metal of formation is on the one hand fillable
The biggish hole of silica interior, controls the size in product aperture, and product on the other hand can be achieved to the effective negative of noble metal
It carries, and then improves the using effect of product；
(3) present invention is added sodium bicarbonate and fe when prepare high catalytic efficiency multi-stage porous silica, sodium bicarbonate with
The addition of fe can react during product is carbonized and prepares, and the water that fe can be formed with sodium bicarbonate reacts,
Hydrogen is generated, to promote the reduction of metal ion complex, also, the ferroso-ferric oxide that fe reaction generates has magnetic
Property, it can further improve the service efficiency of product.
Specific embodiment
Glucose and water 1:20~1:25 in mass ratio are mixed in flask, and glucose quality is added into flask
0.1~0.2 times of Potassiumiodate, then nitrogen is passed through with the rate of 20~30mL/min into beaker, it is 20~35 DEG C in temperature, turns
Under conditions of speed is 300~350r/min, after being stirred to react 12~14h, glucose mixed liquor must be pre-processed；Grape will be pre-processed
Barium chloride solution 1:3~1:5 in mass ratio that sugared mixed liquor and mass fraction are 12~20% mix, in temperature be 20~30 DEG C,
Under conditions of revolving speed is 250~400r/min, after being stirred 30~50min, filtering obtains filtrate, by filtrate and mass fraction
It is mixed for 15~20% metabisulfite solution 1:3~1:4 in mass ratio, is 20~35 DEG C in temperature, revolving speed is 280~380r/
It under conditions of min, is filtered after being stirred 30~60min, obtains modified glucose solution；Polyallylamine hydrochlorides and water are pressed into matter
Amount is mixed than 1:100~1:110, is 40~50 DEG C in temperature, under conditions of revolving speed is 260~380r/min, is stirred 30
After~50min, polyallylamine hydrochlorides solution is obtained, polyallylamine hydrochlorides solution is added in three-necked flask, mass fraction is used
The pH to 9.8~10.0 of polyallylamine hydrochlorides solution is adjusted for 10~12% sodium hydroxide solution, and is added into three-necked flask
The modified glucose solution for entering 0.5~1.3 times of polyallylamine hydrochlorides solution quality, into three-necked flask with 15~25mL/min
Rate be passed through nitrogen, in temperature be 30~35 DEG C, revolving speed be 250~380r/min under conditions of, after being stirred 2~3h,
Obtain mixed solution；Mixed solution is mixed with reducing agent 400:1~500:1 in mass ratio, and to mixed solution and reducing agent
Nitrogen is passed through with the rate of 20~28mL/min in mixture, is 20~40 DEG C in temperature, revolving speed is the item of 250~380r/min
Under part, after being stirred to react 12~15h, filtering obtains filter cake, after filter cake is washed with deionized 2~5 times, obtains microgel；It will gather
Sodium acrylate and microgel 1:5~1:6 in mass ratio are mixed in beaker, and be added into beaker Sodium Polyacrylate quality 20~
30 times of mixed solvent and 0.2~0.6 times of Sodium Polyacrylate quality of additive, in temperature be 30~45 DEG C, revolving speed be 200~
Under conditions of 380r/min, after being stirred 30~60min, template liquid is obtained, by template liquid and ethyl orthosilicate volume of mixture
Be mixed in reaction kettle than 10:1~15:1, and into reaction kettle be added template liquid product 0.1~0.4 times mass fraction be 15~
25% ammonium hydroxide, in temperature be 45~55 DEG C, revolving speed be 250~400r/min under conditions of, after being stirred to react 2~4h, filtering,
Blank must be pre-processed, it is dry under conditions of being 80~90 DEG C in temperature after pretreatment blank is washed with deionized 5~8 times
After 40~60min, blank is obtained, after blank is calcined, obtains high catalytic efficiency multi-stage porous silica.The reducing agent is hydroboration
Any one in sodium or potassium borohydride.The mixed solvent is to mix ethyl alcohol with water 6:1~8:1 in mass ratio, must be mixed molten
Agent.The additive is any one in gold chloride or palladium acid potassium.The ethyl orthosilicate mixture be by ethyl orthosilicate with
Dehydrated alcohol 10:1~10:3 in mass ratio mixing, obtains ethyl orthosilicate mixture.The calcining manners are prior to nitrogen atmosphere
Under, under conditions of 250~400 DEG C, after 2~3h of heat preservation charing, under oxygen atmosphere, under conditions of 450~550 DEG C,
1~3h of calcining at constant temperature.0.1~0.2 times of quality in mixed solution of sodium bicarbonate and mixed solution are added in the mixed solution
The fe that 0.02~0.04 times of quality.The carboxymethyl cellulose of template liquid quality 0.1~0.2 can be added in the template liquid
Sodium.
Glucose and water 1:25 in mass ratio are mixed in flask, and 0.2 times of glucose quality is added into flask
Potassiumiodate, then nitrogen is passed through with the rate of 30mL/min into beaker, it is 35 DEG C in temperature, revolving speed is the condition of 350r/min
Under, after being stirred to react 14h, glucose mixed liquor must be pre-processed；The chlorine that glucose mixed liquor and mass fraction are 20% will be pre-processed
Change barium solution 1:5 in mass ratio mixing, in temperature be 30 DEG C, revolving speed be 400r/min under conditions of, after being stirred 50min,
Filtering, obtains filtrate, and filtrate is mixed with the metabisulfite solution 1:4 in mass ratio that mass fraction is 20%, is 35 DEG C in temperature, turns
Under conditions of speed is 380r/min, is filtered after being stirred 60min, obtain modified glucose solution；By polyallylamine hydrochlorides with
Water 1:110 in mass ratio mixing is 50 DEG C in temperature, under conditions of revolving speed is 380r/min, after being stirred 50min, obtains poly-
Polyallylamine hydrochlorides solution is added in three-necked flask allylamine hydrochloride solution, the sodium hydroxide for being 12% with mass fraction
Solution adjusts the pH to 10.0 of polyallylamine hydrochlorides solution, and polyallylamine hydrochlorides solution quality is added into three-necked flask
1.3 times of modified glucose solution, is passed through nitrogen into three-necked flask with the rate of 25mL/min, in temperature be 35 DEG C, revolving speed
Under conditions of 380r/min, after being stirred 3h, mixed solution is obtained；Mixed solution and reducing agent 500:1 in mass ratio are mixed
It closes, and nitrogen is passed through with the rate of 28mL/min into the mixture of mixed solution and reducing agent, be 40 DEG C in temperature, revolving speed is
Under conditions of 380r/min, after being stirred to react 15h, filtering obtains filter cake, after filter cake is washed with deionized 5 times, obtains micro- solidifying
Glue；Sodium Polyacrylate and microgel 1:6 in mass ratio are mixed in beaker, and Sodium Polyacrylate quality 30 is added into beaker
Mixed solvent and 0.6 times of Sodium Polyacrylate quality of additive again is 45 DEG C in temperature, and revolving speed is the condition of 380r/min
Under, after being stirred 60min, template liquid is obtained, template liquid and ethyl orthosilicate volume of mixture ratio 15:1 are mixed in reaction kettle,
And into reaction kettle be added template liquid product 0.4 times mass fraction be 25% ammonium hydroxide, in temperature be 55 DEG C, revolving speed 400r/
Under conditions of min, after being stirred to react 4h, filtering obtains pretreatment blank, after pretreatment blank is washed with deionized 8 times, in
Under the conditions of at a temperature of 90 °C after dry 60min, blank is obtained, after blank is calcined, obtains high catalytic efficiency multi-stage porous silica.
The reducing agent is sodium borohydride.The mixed solvent is to mix ethyl alcohol with water 8:1 in mass ratio, obtains mixed solvent.It is described
Additive is gold chloride.The ethyl orthosilicate mixture is to mix ethyl orthosilicate with dehydrated alcohol 10:3 in mass ratio,
Obtain ethyl orthosilicate mixture.The calcining manners be prior under nitrogen atmosphere, under conditions of 400 DEG C, after heat preservation charing 3h,
Under oxygen atmosphere, under conditions of 550 DEG C, calcining at constant temperature 3h.Quality 0.2 in mixed solution is added in the mixed solution
Sodium bicarbonate and 0.04 times of mixed solution quality of fe again.The carboxylic of template liquid quality 0.2 can be added in the template liquid
Sodium carboxymethylcellulose pyce.
Glucose and water 1:25 in mass ratio are mixed in flask, and 0.2 times of glucose quality is added into flask
Potassiumiodate, then nitrogen is passed through with the rate of 30mL/min into beaker, it is 35 DEG C in temperature, revolving speed is the condition of 350r/min
Under, after being stirred to react 14h, glucose mixed liquor must be pre-processed；The chlorine that glucose mixed liquor and mass fraction are 20% will be pre-processed
Change barium solution 1:5 in mass ratio mixing, in temperature be 30 DEG C, revolving speed be 400r/min under conditions of, after being stirred 50min,
Filtering, obtains filtrate, and filtrate is mixed with the metabisulfite solution 1:4 in mass ratio that mass fraction is 20%, is 35 DEG C in temperature, turns
Under conditions of speed is 380r/min, is filtered after being stirred 60min, obtain modified glucose solution；By polyallylamine hydrochlorides with
Water 1:110 in mass ratio mixing is 50 DEG C in temperature, under conditions of revolving speed is 380r/min, after being stirred 50min, obtains poly-
Polyallylamine hydrochlorides solution is added in three-necked flask allylamine hydrochloride solution, the sodium hydroxide for being 12% with mass fraction
Solution adjusts the pH to 10.0 of polyallylamine hydrochlorides solution, and polyallylamine hydrochlorides solution quality is added into three-necked flask
1.3 times of modified glucose solution, is passed through nitrogen into three-necked flask with the rate of 25mL/min, in temperature be 35 DEG C, revolving speed
Under conditions of 380r/min, after being stirred 3h, mixed solution is obtained；Mixed solution and reducing agent 500:1 in mass ratio are mixed
It closes, and nitrogen is passed through with the rate of 28mL/min into the mixture of mixed solution and reducing agent, be 40 DEG C in temperature, revolving speed is
Under conditions of 380r/min, after being stirred to react 15h, filtering obtains filter cake, after filter cake is washed with deionized 5 times, obtains micro- solidifying
Glue；By microgel in beaker, and be added into beaker 30 times of microgel quality mixed solvent and 0.6 times of microgel quality
Additive is 45 DEG C in temperature, under conditions of revolving speed is 380r/min, after being stirred 60min, template liquid is obtained, by template liquid
It is mixed in reaction kettle with ethyl orthosilicate volume of mixture ratio 15:1, and the matter of 0.4 times of template liquid product is added into reaction kettle
The ammonium hydroxide that score is 25% is measured, is 55 DEG C in temperature, under conditions of revolving speed is 400r/min, after being stirred to react 4h, filtering is obtained pre-
Blank is handled, after pretreatment blank is washed with deionized 8 times, under the conditions of at a temperature of 90 °C after dry 60min, obtains base
Material, after blank is calcined, obtains high catalytic efficiency multi-stage porous silica.The reducing agent is sodium borohydride.The mixed solvent
To mix ethyl alcohol with water 8:1 in mass ratio, mixed solvent is obtained.The additive is gold chloride.The ethyl orthosilicate mixing
Object is to mix ethyl orthosilicate with dehydrated alcohol 10:3 in mass ratio, obtains ethyl orthosilicate mixture.The calcining manners are
It is permanent under conditions of 550 DEG C under oxygen atmosphere prior under conditions of 400 DEG C, keeping the temperature after carbonizing 3h under nitrogen atmosphere
Temperature calcining 3h.In the mixed solution be added mixed solution in 0.2 times of quality sodium bicarbonate and 0.04 times of mixed solution quality
Fe.The sodium carboxymethylcellulose of template liquid quality 0.2 can be added in the template liquid.
Glucose and water 1:25 in mass ratio are mixed in flask, and 0.2 times of glucose quality is added into flask
Potassiumiodate, then nitrogen is passed through with the rate of 30mL/min into beaker, it is 35 DEG C in temperature, revolving speed is the condition of 350r/min
Under, after being stirred to react 14h, glucose mixed liquor must be pre-processed；The chlorine that glucose mixed liquor and mass fraction are 20% will be pre-processed
Change barium solution 1:5 in mass ratio mixing, in temperature be 30 DEG C, revolving speed be 400r/min under conditions of, after being stirred 50min,
Filtering, obtains filtrate, and filtrate is mixed with the metabisulfite solution 1:4 in mass ratio that mass fraction is 20%, is 35 DEG C in temperature, turns
Under conditions of speed is 380r/min, is filtered after being stirred 60min, obtain modified glucose solution；By polyallylamine hydrochlorides with
Water 1:110 in mass ratio mixing is 50 DEG C in temperature, under conditions of revolving speed is 380r/min, after being stirred 50min, obtains poly-
Polyallylamine hydrochlorides solution is added in three-necked flask allylamine hydrochloride solution, the sodium hydroxide for being 12% with mass fraction
Solution adjusts the pH to 10.0 of polyallylamine hydrochlorides solution, and polyallylamine hydrochlorides solution quality is added into three-necked flask
1.3 times of modified glucose solution, is passed through nitrogen into three-necked flask with the rate of 25mL/min, in temperature be 35 DEG C, revolving speed
Under conditions of 380r/min, after being stirred 3h, mixed solution is obtained；Mixed solution and reducing agent 500:1 in mass ratio are mixed
It closes, and nitrogen is passed through with the rate of 28mL/min into the mixture of mixed solution and reducing agent, be 40 DEG C in temperature, revolving speed is
Under conditions of 380r/min, after being stirred to react 15h, filtering obtains filter cake, after filter cake is washed with deionized 5 times, obtains micro- solidifying
Glue；Sodium Polyacrylate and microgel 1:6 in mass ratio are mixed in beaker, and Sodium Polyacrylate quality 30 is added into beaker
Mixed solvent again is 45 DEG C in temperature, under conditions of revolving speed is 380r/min, after being stirred 60min, obtains template liquid, will
Template liquid and ethyl orthosilicate volume of mixture ratio 15:1 are mixed in reaction kettle, and template liquid product 0.4 is added into reaction kettle
Times mass fraction be 25% ammonium hydroxide, in temperature be 55 DEG C, revolving speed be 400r/min under conditions of, after being stirred to react 4h, mistake
Filter, obtains pretreatment blank, after pretreatment blank is washed with deionized 8 times, the dry 60min under the conditions of at a temperature of 90 °C
Afterwards, blank is obtained, after blank is calcined, obtains high catalytic efficiency multi-stage porous silica.The reducing agent is sodium borohydride.It is described mixed
Bonding solvent is to mix ethyl alcohol with water 8:1 in mass ratio, obtains mixed solvent.The ethyl orthosilicate mixture is by positive silicic acid second
Ester is mixed with dehydrated alcohol 10:3 in mass ratio, obtains ethyl orthosilicate mixture.The calcining manners be prior under nitrogen atmosphere,
Under conditions of 400 DEG C, after heat preservation charing 3h, under oxygen atmosphere, under conditions of 550 DEG C, calcining at constant temperature 3h.It is described mixed
It closes and 0.2 times of quality of sodium bicarbonate and 0.04 times of mixed solution quality of fe in mixed solution is added in solution.The mould
The sodium carboxymethylcellulose of template liquid quality 0.2 can be added in plate liquid.
Comparative example: glucose and water 1:25 in mass ratio are mixed in flask, and glucose quality is added into flask
0.2 times of Potassiumiodate, then nitrogen is passed through with the rate of 30mL/min into beaker, in temperature be 35 DEG C, revolving speed 350r/min
Under conditions of, after being stirred to react 14h, glucose mixed liquor must be pre-processed；It is with mass fraction by pretreatment glucose mixed liquor
20% barium chloride solution 1:5 in mass ratio mixing is 30 DEG C in temperature, under conditions of revolving speed is 400r/min, is stirred
After 50min, filtering obtains filtrate, and filtrate is mixed with the metabisulfite solution 1:4 in mass ratio that mass fraction is 20%, is in temperature
It 35 DEG C, under conditions of revolving speed is 380r/min, is filtered after being stirred 60min, obtains modified glucose solution；By polyallylamine salt
Hydrochlorate is mixed with water 1:110 in mass ratio, is 50 DEG C in temperature, under conditions of revolving speed is 380r/min, is stirred 50min
Afterwards, polyallylamine hydrochlorides solution is obtained, polyallylamine hydrochlorides solution is added in three-necked flask, is 12% with mass fraction
Sodium hydroxide solution adjusts the pH to 10.0 of polyallylamine hydrochlorides solution, and polyallylamine hydrochlorides are added into three-necked flask
1.3 times of solution quality of modified glucose solution, is passed through nitrogen into three-necked flask with the rate of 25mL/min, in temperature be 35
DEG C, under conditions of revolving speed is 380r/min, after being stirred 3h, obtain mixed solution；In mass ratio by mixed solution and reducing agent
500:1 mixing, and is passed through nitrogen into the mixture of mixed solution and reducing agent with the rate of 28mL/min, in temperature be 40
DEG C, under conditions of revolving speed is 380r/min, after being stirred to react 15h, filtering obtains filter cake, filter cake is washed with deionized 5 times
Afterwards, microgel is obtained；30 times of microgel quality of mixed solvent is added into beaker in beaker for microgel, in temperature be 45
DEG C, under conditions of revolving speed is 380r/min, after being stirred 60min, template liquid is obtained, by template liquid and ethyl orthosilicate mixture
Volume ratio 15:1 is mixed in reaction kettle, and the ammonium hydroxide that the mass fraction of 0.4 times of template liquid product is 25% is added into reaction kettle,
It is 55 DEG C in temperature, under conditions of revolving speed is 400r/min, after being stirred to react 4h, filtering obtains pretreatment blank, will pre-process base
After material is washed with deionized 8 times, under the conditions of at a temperature of 90 °C after dry 60min, blank is obtained, after blank is calcined, is obtained
High catalytic efficiency multi-stage porous silica.The reducing agent is sodium borohydride.The mixed solvent is that ethyl alcohol and water are pressed quality
It is mixed than 8:1, obtains mixed solvent.The ethyl orthosilicate mixture is by ethyl orthosilicate and dehydrated alcohol 10:3 in mass ratio
Mixing, obtains ethyl orthosilicate mixture.The calcining manners are prior under nitrogen atmosphere, under conditions of 400 DEG C, heat preservation is carbonized
After 3h, under oxygen atmosphere, under conditions of 550 DEG C, calcining at constant temperature 3h.Matter in mixed solution is added in the mixed solution
Measure 0.2 times of sodium bicarbonate and 0.04 times of mixed solution quality of fe.Template liquid quality 0.2 can be added in the template liquid
Sodium carboxymethylcellulose.
Example 1 to the resulting high catalytic efficiency multi-stage porous silica of example 3 and comparative example product are subjected to performance detection,
The specific detection method is as follows:
Porosity: porosity uses gravimetry.By samples weighing, it is denoted as m1, by electrochemical corrosion after weigh, remember
For m2, the KOH solid of 3g is dissolved in 100mL water, and the sample corroded is placed wherein, is dissolved generates bubble rapidly,
Silicon chip extracting is weighed to bubble is no longer generated, is denoted as m3.Porosity (P) is calculated from formula, by test specimen as methylene
In blue solution and surveys it and use the catalytic performance after 5h.
Specific testing result is as shown in table 1:
The high catalytic efficiency multi-stage porous silica performance test results of table 1
| Detection project | Example 1 | Example 2 | Example 3 | Comparative example |
| Porosity/% | 96.8 | 91.2 | 92.7 | 83.1 |
| Catalytic efficiency/% | 85.6 | 78.1 | 73.8 | 65.7 |
By 1 testing result of table it is found that the high catalytic efficiency multi-stage porous silica materials of technical solution of the present invention preparation are with excellent
The characteristics of different porosity and catalytic performance, has broad prospects in the development of nano-porous materials technology industry.
Claims (9)
1. a kind of preparation method of high catalytic efficiency multi-stage porous silica, which is characterized in that it is specific the preparation method comprises the following steps:
(1) pretreatment glucose mixed liquor is mixed with barium chloride solution 1:3~1:5 in mass ratio, filters, obtains filtrate, will filter
Liquid is mixed with metabisulfite solution 1:3~1:4 in mass ratio, and filtering obtains modified glucose solution；
(2) polyallylamine hydrochlorides are mixed with water 1:100~1:110 in mass ratio, obtains polyallylamine hydrochlorides solution, adjusted
The pH to 9.8~10.0 of polyallylamine hydrochlorides solution, and be added 0.5~1.3 times of polyallylamine hydrochlorides solution quality and change
Property glucose solution after being stirred, obtains mixed solution under nitrogen atmosphere；
(3) mixed solution is mixed with reducing agent 400:1~500:1 in mass ratio, under nitrogen atmosphere, after being stirred to react, mistake
Filter, washing, obtains microgel；
(4) Sodium Polyacrylate is mixed with microgel 1:5~1:6 in mass ratio, and is added 20~30 times of Sodium Polyacrylate quality
Mixed solvent and 0.2~0.6 times of Sodium Polyacrylate quality of additive, after being stirred, obtain template liquid, by template liquid with just
Silester volume of mixture ratio 10:1~15:1 mixing, and the ammonium hydroxide of 0.1~0.4 times of template liquid product is added, it is stirred to react
Afterwards, it filters, washs, it is dry, blank is obtained, after blank is calcined, obtains high catalytic efficiency multi-stage porous silica.
2. a kind of preparation method of high catalytic efficiency multi-stage porous silica according to claim 1, it is characterised in that: step
Suddenly (1) described pretreatment glucose mixed liquor is to mix glucose with water 1:20~1:25 in mass ratio, and glucose is added
The Potassiumiodate that 0.1~0.2 times of quality after being stirred to react, must pre-process glucose mixed liquor under nitrogen atmosphere.
3. a kind of preparation method of high catalytic efficiency multi-stage porous silica according to claim 1, it is characterised in that: step
Suddenly (3) described reducing agent is any one in sodium borohydride or potassium borohydride.
4. a kind of preparation method of high catalytic efficiency multi-stage porous silica according to claim 1, it is characterised in that: step
Suddenly (4) described mixed solvent is to mix ethyl alcohol with water 6:1~8:1 in mass ratio, obtains mixed solvent.
5. a kind of preparation method of high catalytic efficiency multi-stage porous silica according to claim 1, it is characterised in that: step
Suddenly (4) described additive is any one in gold chloride or palladium acid potassium.
6. a kind of preparation method of high catalytic efficiency multi-stage porous silica according to claim 1, it is characterised in that: step
Suddenly (4) described ethyl orthosilicate mixture is to mix ethyl orthosilicate with dehydrated alcohol 10:1~10:3 in mass ratio, is obtained just
Silester mixture.
7. a kind of preparation method of high catalytic efficiency multi-stage porous silica according to claim 1, it is characterised in that: step
Suddenly (4) described calcining manners are prior under conditions of 250~400 DEG C, keeping the temperature after carbonizing 2~3h, then at oxygen under nitrogen atmosphere
Under atmosphere is enclosed, under conditions of 450~550 DEG C, 1~3h of calcining at constant temperature.
8. a kind of preparation method of high catalytic efficiency multi-stage porous silica according to claim 1, it is characterised in that: step
Suddenly in (3) described mixed solution be added mixed solution in 0.1~0.2 times of quality sodium bicarbonate and mixed solution quality 0.02~
0.04 times of fe.
9. a kind of preparation method of high catalytic efficiency multi-stage porous silica according to claim 1, it is characterised in that: step
Suddenly the sodium carboxymethylcellulose of template liquid quality 0.1~0.2 can be added in (4) described template liquid.
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| CN110527517A (en) * | 2019-09-19 | 2019-12-03 | 凃雨菲 | A kind of renovation agent and preparation method thereof for heavy metal pollution of soil |
| CN111962176A (en) * | 2019-09-25 | 2020-11-20 | 舒伟伟 | Manufacturing method of composite conductive fabric |
| CN112500016A (en) * | 2021-01-08 | 2021-03-16 | 成都楠裘榕科技有限公司 | Preparation method of concrete water reducing agent |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110527517A (en) * | 2019-09-19 | 2019-12-03 | 凃雨菲 | A kind of renovation agent and preparation method thereof for heavy metal pollution of soil |
| CN111962176A (en) * | 2019-09-25 | 2020-11-20 | 舒伟伟 | Manufacturing method of composite conductive fabric |
| CN111979587A (en) * | 2019-09-25 | 2020-11-24 | 舒伟伟 | Manufacturing method of composite conductive fabric |
| CN111962176B (en) * | 2019-09-25 | 2022-09-30 | 广东莱竣电子科技有限公司 | Manufacturing method of composite conductive fabric |
| CN111979587B (en) * | 2019-09-25 | 2022-10-25 | 昱天(上海)新材料有限公司 | Manufacturing method of composite conductive fabric |
| CN112500016A (en) * | 2021-01-08 | 2021-03-16 | 成都楠裘榕科技有限公司 | Preparation method of concrete water reducing agent |
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