CN101920970A - Preparation method of silicate nano hollow structure material - Google Patents
Preparation method of silicate nano hollow structure material Download PDFInfo
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- CN101920970A CN101920970A CN 201010111591 CN201010111591A CN101920970A CN 101920970 A CN101920970 A CN 101920970A CN 201010111591 CN201010111591 CN 201010111591 CN 201010111591 A CN201010111591 A CN 201010111591A CN 101920970 A CN101920970 A CN 101920970A
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- 239000000463 material Substances 0.000 title claims abstract description 22
- BPQQTUXANYXVAA-UHFFFAOYSA-N Orthosilicate Chemical compound [O-][Si]([O-])([O-])[O-] BPQQTUXANYXVAA-UHFFFAOYSA-N 0.000 title claims abstract description 20
- 238000002360 preparation method Methods 0.000 title claims abstract description 19
- 239000000243 solution Substances 0.000 claims abstract description 112
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 46
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims abstract description 45
- 239000004115 Sodium Silicate Substances 0.000 claims abstract description 23
- NTHWMYGWWRZVTN-UHFFFAOYSA-N sodium silicate Chemical compound [Na+].[Na+].[O-][Si]([O-])=O NTHWMYGWWRZVTN-UHFFFAOYSA-N 0.000 claims abstract description 23
- 229910052911 sodium silicate Inorganic materials 0.000 claims abstract description 23
- 229910002651 NO3 Inorganic materials 0.000 claims abstract description 18
- NHNBFGGVMKEFGY-UHFFFAOYSA-N Nitrate Chemical compound [O-][N+]([O-])=O NHNBFGGVMKEFGY-UHFFFAOYSA-N 0.000 claims abstract description 18
- 239000011259 mixed solution Substances 0.000 claims abstract description 14
- 238000001035 drying Methods 0.000 claims abstract description 11
- 238000001914 filtration Methods 0.000 claims abstract description 11
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 claims description 42
- 238000002156 mixing Methods 0.000 claims description 30
- 229920003171 Poly (ethylene oxide) Polymers 0.000 claims description 21
- WGCNASOHLSPBMP-UHFFFAOYSA-N hydroxyacetaldehyde Natural products OCC=O WGCNASOHLSPBMP-UHFFFAOYSA-N 0.000 claims description 21
- -1 polyoxyethylene Polymers 0.000 claims description 21
- 239000003795 chemical substances by application Substances 0.000 claims description 20
- HCWCAKKEBCNQJP-UHFFFAOYSA-N magnesium orthosilicate Chemical compound [Mg+2].[Mg+2].[O-][Si]([O-])([O-])[O-] HCWCAKKEBCNQJP-UHFFFAOYSA-N 0.000 claims description 20
- 239000000391 magnesium silicate Substances 0.000 claims description 20
- 229910052919 magnesium silicate Inorganic materials 0.000 claims description 20
- 235000019792 magnesium silicate Nutrition 0.000 claims description 20
- YIXJRHPUWRPCBB-UHFFFAOYSA-N magnesium nitrate Chemical compound [Mg+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O YIXJRHPUWRPCBB-UHFFFAOYSA-N 0.000 claims description 16
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 11
- 238000013019 agitation Methods 0.000 claims description 10
- 238000010438 heat treatment Methods 0.000 claims description 10
- ONDPHDOFVYQSGI-UHFFFAOYSA-N zinc nitrate Chemical compound [Zn+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O ONDPHDOFVYQSGI-UHFFFAOYSA-N 0.000 claims description 8
- 229910000323 aluminium silicate Inorganic materials 0.000 claims description 5
- 235000019352 zinc silicate Nutrition 0.000 claims description 5
- BNGXYYYYKUGPPF-UHFFFAOYSA-M (3-methylphenyl)methyl-triphenylphosphanium;chloride Chemical compound [Cl-].CC1=CC=CC(C[P+](C=2C=CC=CC=2)(C=2C=CC=CC=2)C=2C=CC=CC=2)=C1 BNGXYYYYKUGPPF-UHFFFAOYSA-M 0.000 claims description 4
- 239000004110 Zinc silicate Substances 0.000 claims description 4
- HNPSIPDUKPIQMN-UHFFFAOYSA-N dioxosilane;oxo(oxoalumanyloxy)alumane Chemical compound O=[Si]=O.O=[Al]O[Al]=O HNPSIPDUKPIQMN-UHFFFAOYSA-N 0.000 claims description 3
- 239000002245 particle Substances 0.000 claims description 3
- 239000011258 core-shell material Substances 0.000 claims description 2
- XSMMCTCMFDWXIX-UHFFFAOYSA-N zinc silicate Chemical compound [Zn+2].[O-][Si]([O-])=O XSMMCTCMFDWXIX-UHFFFAOYSA-N 0.000 claims 1
- 150000002500 ions Chemical class 0.000 abstract description 7
- 239000011796 hollow space material Substances 0.000 abstract description 6
- 238000010521 absorption reaction Methods 0.000 abstract description 5
- 229910001385 heavy metal Inorganic materials 0.000 abstract description 3
- 238000006555 catalytic reaction Methods 0.000 abstract description 2
- 239000003814 drug Substances 0.000 abstract description 2
- 238000003912 environmental pollution Methods 0.000 abstract description 2
- 239000002202 Polyethylene glycol Substances 0.000 abstract 2
- 229920001223 polyethylene glycol Polymers 0.000 abstract 2
- 229940079593 drug Drugs 0.000 abstract 1
- 238000003760 magnetic stirring Methods 0.000 abstract 1
- 238000000034 method Methods 0.000 description 8
- 239000011777 magnesium Substances 0.000 description 5
- 238000005342 ion exchange Methods 0.000 description 4
- ZOIVSVWBENBHNT-UHFFFAOYSA-N dizinc;silicate Chemical compound [Zn+2].[Zn+2].[O-][Si]([O-])([O-])[O-] ZOIVSVWBENBHNT-UHFFFAOYSA-N 0.000 description 3
- 239000005995 Aluminium silicate Substances 0.000 description 2
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 2
- YKTSYUJCYHOUJP-UHFFFAOYSA-N [O--].[Al+3].[Al+3].[O-][Si]([O-])([O-])[O-] Chemical compound [O--].[Al+3].[Al+3].[O-][Si]([O-])([O-])[O-] YKTSYUJCYHOUJP-UHFFFAOYSA-N 0.000 description 2
- 235000012211 aluminium silicate Nutrition 0.000 description 2
- 229910052898 antigorite Inorganic materials 0.000 description 2
- 238000006243 chemical reaction Methods 0.000 description 2
- 229910052620 chrysotile Inorganic materials 0.000 description 2
- 238000010586 diagram Methods 0.000 description 2
- 229910052899 lizardite Inorganic materials 0.000 description 2
- 229910021645 metal ion Inorganic materials 0.000 description 2
- 238000003756 stirring Methods 0.000 description 2
- VTLYFUHAOXGGBS-UHFFFAOYSA-N Fe3+ Chemical compound [Fe+3] VTLYFUHAOXGGBS-UHFFFAOYSA-N 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 230000000274 adsorptive effect Effects 0.000 description 1
- 238000004458 analytical method Methods 0.000 description 1
- 239000011324 bead Substances 0.000 description 1
- 239000002775 capsule Substances 0.000 description 1
- 239000003575 carbonaceous material Substances 0.000 description 1
- 230000002950 deficient Effects 0.000 description 1
- 239000008367 deionised water Substances 0.000 description 1
- 229910021641 deionized water Inorganic materials 0.000 description 1
- 230000009977 dual effect Effects 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000007429 general method Methods 0.000 description 1
- 229910052745 lead Inorganic materials 0.000 description 1
- 239000004973 liquid crystal related substance Substances 0.000 description 1
- 239000007791 liquid phase Substances 0.000 description 1
- 229910052749 magnesium Inorganic materials 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 description 1
- 239000004530 micro-emulsion Substances 0.000 description 1
- 239000012046 mixed solvent Substances 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 238000006386 neutralization reaction Methods 0.000 description 1
- 229920000642 polymer Polymers 0.000 description 1
- FGIUAXJPYTZDNR-UHFFFAOYSA-N potassium nitrate Chemical compound [K+].[O-][N+]([O-])=O FGIUAXJPYTZDNR-UHFFFAOYSA-N 0.000 description 1
- 229910052604 silicate mineral Inorganic materials 0.000 description 1
- 239000000377 silicon dioxide Substances 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 238000001179 sorption measurement Methods 0.000 description 1
- BFKJFAAPBSQJPD-UHFFFAOYSA-N tetrafluoroethene Chemical group FC(F)=C(F)F BFKJFAAPBSQJPD-UHFFFAOYSA-N 0.000 description 1
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Abstract
The invention relates to a preparation method of a silicate nano hollow structure material, which comprises the following steps: (1) orderly adding 0.2 mol/L nitrate solution and 0.2 mol/L sodium silicate solution into mixed liquor of ethanol and polyethylene glycol to form a mixed solution, wherein the mixed solution respectively comprises 20-30 parts of ethanol, 2-3 parts of polyethylene glycol, 1 part of nitrate solution and 1-2 parts of sodium silicate solution in parts by volume; (2) adding NaOH solution into the mixed solution obtained in step (1), wherein the volume ratio of NaOH solution to nitrate solution is 1:0.03-0.2; and after conducting magnetic stirring, transferring the mixed solution to a hydrothermal kettle, reacting under the hydrothermal condition of 100-200 DEG C, filtering and drying to obtain the silicate nano hollow structure material. The obtained silicate hollow material can be used for heavy metal ion absorption, and can also be used in the fields of catalysis, medicines, environmental pollution treatment and the like.
Description
Technical field
The present invention relates to a kind of preparation method of hollow material, particularly a kind of preparation method of silicate nano hollow structure material.
Background technology
At present developed a lot of methods that prepare hollow material both at home and abroad, the most general method has with inorganics, metal, polymer billet etc. as the hard template method of template with the soft template method as template such as microemulsion, vesica.For example, Yoon S.B. etc. reported on the AdvancedMaterials magazine and use the solid-surface mesoporous silico-aluminate bead of submicron-scale as template in 2002, made surface mesoporous carbon material Capsules (Adv.Mater., 2002,14:19-21).Djojoputro H. etc. reported use vesica and liquid crystal dual mould plate method in 2006 on Journal of The AmericanChemical Society magazine, made the mesoporous organosilicon hollow material (J.Am.Chem.Soc. of the rule of adjustable wall thickness, 2006,128:6320-6321).Therefore hard template method and soft template method all can obtain uniformly meso-porous hollow material, yet hard template method is to the removal of template particles very expensive and consuming time always, and for the effective preparation of soft template more complicated usually in the soft template method.
Summary of the invention
In order to overcome the defective of above-mentioned prior art, the object of the present invention is to provide a kind of preparation method of silicate nano hollow structure material, nitrate and sodium silicate solution are joined in ethanol and the polyoxyethylene glycol mixed solvent, regulate the pH value with NaOH, be transferred to liquid phase reaction in the closed reaction vessel tetrafluoroethylene autoclave, the silicate hollow material that obtains can be used aspect heavy metal ion adsorbed to some extent, can be used for fields such as catalysis, medicine, environmental pollution improvement.
In order to achieve the above object, technical scheme of the present invention is achieved in that
A kind of preparation method of silicate nano hollow structure material may further comprise the steps:
One, in the mixed solution of ethanol and polyoxyethylene glycol, add the nitrate solution of 0.2mol/L and the sodium silicate solution of 0.2mol/L successively, form mixing solutions, the volume parts of ethanol, polyoxyethylene glycol, nitrate solution and sodium silicate solution is respectively 20-30 part, 2-3 part, 1 part and 1-2 part in this mixing solutions;
Two, in the mixing solutions that step 1 makes, add 4mol/L NaOH solution, NaOH solution is 1 with nitrate solution volume parts ratio in the step 1: 0.03-0.2, behind the magnetic agitation 15-30min, be transferred in the water heating kettle, react 12-48h under 100 ℃~200 ℃ hydrothermal conditions, filtration drying obtains silicate nano hollow structure material.
The resulting silicate hollow structure material of the present invention is to heavy metal ion, as Pb
2+, Cr
3+, Cd
2+And Fe
3+Deng good exchange absorption property is arranged, this is because the nano-scale of material and hollow structure have increased the specific surface that silicate can be used for ion-exchange and absorption, no matter and be silicate stratiform or chain-like structure, be free between the silica casing ply or metal ion that interchain can move freely can more touch external environment, and replaced by other metal ion.So the silicate hollow structure material that the present invention obtains is bigger than the ion-exchange performance of silicate minerals material in the past.
Description of drawings
Fig. 1 is that the XRD of embodiment 1,2 prepared Magnesium Silicate q-agent hollow balls and nucleocapsid ball product characterizes, and wherein: a is that the XRD of hollow ball characterizes the XRD phenogram of b nucleocapsid ball product.
Fig. 2 is the TEM phenogram of embodiment 1 prepared Magnesium Silicate q-agent nucleocapsid ball product.
Fig. 3 is the SEM phenogram of embodiment 2 prepared Magnesium Silicate q-agent hollow ball products.
Fig. 4 is the EDS composition analysis figure of embodiment 1 and 2 prepared Magnesium Silicate q-agent hollow balls and nucleocapsid ball product
Fig. 5 is the TEM phenogram and the SEM phenogram of embodiment 3 and 4 prepared zinc silicates, hollow aluminosilicate ball product, and wherein: a, b are zinc silicate, and c, d are pure aluminium silicate.
Embodiment
Embodiment one
The preparation method of present embodiment may further comprise the steps:
One, in the mixed solution of ethanol and polyoxyethylene glycol, add the magnesium nitrate solution of 0.2mol/L and the sodium silicate solution of 0.2mol/L successively, form mixing solutions, the volume parts of ethanol, polyoxyethylene glycol, magnesium nitrate solution and sodium silicate solution is respectively 30 parts, 3 parts, 1 part and 1 part in this mixing solutions;
Two, in the mixing solutions that step 1 makes, add 4mol/LNaOH solution, NaOH solution is 1: 0.03 with nitrate solution volume parts ratio in the step 1, behind the magnetic agitation 15min, be transferred in the water heating kettle, react 12h under 190 ℃ of hydrothermal conditions, filtration drying obtains Magnesium Silicate q-agent core-shell particles product.
Among Fig. 1: the b curve is that the XRD of embodiment 1 prepared nucleocapsid ball product characterizes, main diffraction peak 2 θ=19.493,24.366,35.307 and 60.414 ° and Mg
3Si
2O
5(OH)
4(JCPDS no.52-1562) is consistent for standard diagram, has illustrated that product is a Magnesium Silicate q-agent.
Fig. 2 is that the TEM of embodiment 1 prepared nucleocapsid ball product characterizes, and picture shows that almost 90% sample is made up of hollow ball shell and kernel, and the diameter of nucleocapsid ball is between 100~200nm.
Embodiment two
The preparation method of present embodiment may further comprise the steps:
One, in the mixed solution of ethanol and polyoxyethylene glycol, add the magnesium nitrate solution of 0.2mol/L and the sodium silicate solution of 0.2mol/L successively, form mixing solutions, the volume parts of ethanol, polyoxyethylene glycol, magnesium nitrate solution and sodium silicate solution is respectively 30 parts, 3 parts, 1 part and 1 part in this mixing solutions;
Two, in the mixing solutions that step 1 makes, add 4mol/LNaOH solution, NaOH solution is 1: 0.1 with nitrate solution volume parts ratio in the step 1, behind the magnetic agitation 15min, be transferred in the water heating kettle, react 12h under 190 ℃ of hydrothermal conditions, filtration drying obtains Magnesium Silicate q-agent tiny balloon product.
Among Fig. 1: a curve is that the XRD of embodiment 2 prepared Magnesium Silicate q-agent hollow balls characterizes, main diffraction peak 2 θ=19.493,24.366,35.307 and 60.414 ° and Mg
3Si
2O
5(OH)
4(JCPDS no.52-1562) is consistent for standard diagram, has illustrated that product is a Magnesium Silicate q-agent.
Fig. 3 is that the TEM of example 2 prepared Magnesium Silicate q-agent hollow balls characterizes, and as can be seen from the figure, institute's synthetic product is homogeneous (almost 90% is hollow ball) comparatively, and the diameter dimension of hollow ball is between 100~200nm, and the Magnesium Silicate q-agent hollow ball is made up of small pieces.
As can be seen from Figure 1, the difference of two embodiment degree of crystallinity that is Magnesium Silicate q-agent hollow ball product good than nucleocapsid ball product.And Fig. 4 EDS collection of illustrative plates shows, no matter be hollow structure or nucleocapsid structure, all contains elements such as Mg, Si and O in the product sample, and by more as can be seen, the Mg/Si value of Magnesium Silicate q-agent hollow ball is bigger than nucleocapsid ball, illustrates that hollow ball contains more Mg element.
Embodiment three
The preparation method of present embodiment may further comprise the steps:
One, in the mixed solution of ethanol and polyoxyethylene glycol, add the zinc nitrate solution of 0.2mol/L and the sodium silicate solution of 0.2mol/L successively, form mixing solutions, the volume parts of ethanol, polyoxyethylene glycol, zinc nitrate solution and sodium silicate solution is respectively 25 parts, 2 parts, 1 part and 1 part in this mixing solutions;
Two, in the mixing solutions that step 1 makes, add 4mol/LNaOH solution, NaOH solution is 1: 0.15 with nitrate solution volume parts ratio in the step 1, behind the magnetic agitation 30min, be transferred in the water heating kettle, react 24h under 120 ℃ of hydrothermal conditions, filtration drying obtains the zinc silicate hollow ball material.
Among Fig. 5: a-b is that the TEM and the SEM of embodiment 3 prepared zinc silicate products characterizes, and as can be seen from the figure the pattern of product is a hollow ball structure.
Embodiment four
The preparation method of present embodiment may further comprise the steps:
One, in the mixed solution of ethanol and polyoxyethylene glycol, add the aluminum nitrate solution of 0.2mol/L and the sodium silicate solution of 0.2mol/L successively, form mixing solutions, the volume parts of ethanol, polyoxyethylene glycol, aluminum nitrate solution and sodium silicate solution is respectively 27 parts, 2 parts, 1 part and 1.5 parts in this mixing solutions;
Two, in the mixing solutions that step 1 makes, add 4mol/LNaOH solution, NaOH solution is 1: 0.12 with nitrate solution volume parts ratio in the step 1, behind the magnetic agitation 15min, be transferred in the water heating kettle, react 12h under 160 ℃ of hydrothermal conditions, filtration drying obtains the hollow aluminosilicate ball material.
Among Fig. 5: c-d is that the TEM and the SEM of embodiment 4 prepared pure aluminium silicate products characterizes, and as can be seen from the figure the pattern of product is a hollow ball structure.
It is 106.42mg/L that the 0.05g Magnesium Silicate q-agent sample ultrasonic of embodiment one preparation is scattered in 10ml concentration, and pH value is 2 Pb (II) deionized water solution, is adsorbed on surperficial OH with nitre acid for adjusting pH value to 7 with neutralization again
-, when stirring, it is joined in the Pb that 10ml concentration is 106.42mg/L (II) solution then, stir after 3 hours, solid is separated from solution, and the concentration of staying Pb in the solution (II) is detected.
The sample of embodiment two preparation is detected as stated above equally, and as can be seen from Table 1, Magnesium Silicate q-agent hollow ball product and nucleocapsid ball product are respectively 64.79 and 47.51mg g to Pb (II) ionic removal ability
-1Nucleocapsid ball product is littler than hollow ball product to Pb (II) ionic exchange adsorptive power, this is because the nucleocapsid ball product of equivalent is compared with the hollow ball product and contained less Mg (II) ion (the EDS collection of illustrative plates can prove), makes it possible to that Mg (II) ion that replaced by Pb (II) ion exchange is less to be caused.
The BET data and the ion adsorption capacity of the prepared Magnesium Silicate q-agent product of table 1
In addition, table 2 has proved that Magnesium Silicate q-agent hollow ball product all has ion-exchange absorption effect to Cr (III), Cd (II) and Fe (III) plasma.
The prepared Magnesium Silicate q-agent hollow ball product of table 2 is to the absorption of different ions
Claims (5)
1. the preparation method of a silicate nano hollow structure material, it is characterized in that, may further comprise the steps: one, in the mixed solution of ethanol and polyoxyethylene glycol, add the nitrate solution of 0.2mol/L and the sodium silicate solution of 0.2mol/L successively, form mixing solutions, the volume parts of ethanol, polyoxyethylene glycol, nitrate solution and sodium silicate solution is respectively 20-30 part, 2-3 part, 1 part and 1-2 part in this mixing solutions; Two, in the mixing solutions that step 1 makes, add 4mol/L NaOH solution, NaOH solution is 1 with nitrate solution volume parts ratio in the step 1: 0.03-0.2, behind the magnetic agitation 15-30min, be transferred in the water heating kettle, react 12-48h under 100 ℃~200 ℃ hydrothermal conditions, filtration drying obtains silicate nano hollow structure material.
2. the preparation method of a kind of silicate nano hollow structure material according to claim 1, it is characterized in that, may further comprise the steps: one, in the mixed solution of ethanol and polyoxyethylene glycol, add the magnesium nitrate solution of 0.2mol/L and the sodium silicate solution of 0.2mol/L successively, form mixing solutions, the volume parts of ethanol, polyoxyethylene glycol, magnesium nitrate solution and sodium silicate solution is respectively 30 parts, 3 parts, 1 part and 1 part in this mixing solutions; Two, in the mixing solutions that step 1 makes, add 4mol/LNaOH solution, NaOH solution is 1: 0.03 with nitrate solution volume parts ratio in the step 1, behind the magnetic agitation 15min, be transferred in the water heating kettle, react 12h under 190 ℃ of hydrothermal conditions, filtration drying obtains Magnesium Silicate q-agent core-shell particles product.
3. the preparation method of a kind of silicate nano hollow structure material according to claim 1, it is characterized in that, may further comprise the steps: one, in the mixed solution of ethanol and polyoxyethylene glycol, add the magnesium nitrate solution of 0.2mol/L and the sodium silicate solution of 0.2mol/L successively, form mixing solutions, the volume parts of ethanol, polyoxyethylene glycol, magnesium nitrate solution and sodium silicate solution is respectively 30 parts, 3 parts, 1 part and 1 part in this mixing solutions; Two, in the mixing solutions that step 1 makes, add 4mol/LNaOH solution, NaOH solution is 1: 0.1 with nitrate solution volume parts ratio in the step 1, behind the magnetic agitation 15min, be transferred in the water heating kettle, react 12h under 190 ℃ of hydrothermal conditions, filtration drying obtains Magnesium Silicate q-agent tiny balloon product.
4. the preparation method of a kind of silicate nano hollow structure material according to claim 1, it is characterized in that, may further comprise the steps: one, in the mixed solution of ethanol and polyoxyethylene glycol, add the zinc nitrate solution of 0.2mol/L and the sodium silicate solution of 0.2mol/L successively, form mixing solutions, the volume parts of ethanol, polyoxyethylene glycol, zinc nitrate solution and sodium silicate solution is respectively 25 parts, 2 parts, 1 part and 1 part in this mixing solutions; Two, in the mixing solutions that step 1 makes, add 4mol/LNaOH solution, NaOH solution is 1: 0.15 with nitrate solution volume parts ratio in the step 1, behind the magnetic agitation 30min, be transferred in the water heating kettle, react 24h under 120 ℃ of hydrothermal conditions, filtration drying obtains the zinc silicate hollow ball material.
5. the preparation method of a kind of silicate nano hollow structure material according to claim 1, it is characterized in that, may further comprise the steps: one, in the mixed solution of ethanol and polyoxyethylene glycol, add the aluminum nitrate solution of 0.2mol/L and the sodium silicate solution of 0.2mol/L successively, form mixing solutions, the volume parts of ethanol, polyoxyethylene glycol, aluminum nitrate solution and sodium silicate solution is respectively 27 parts, 2 parts, 1 part and 1.5 parts in this mixing solutions; Two, in the mixing solutions that step 1 makes, add 4mol/LNaOH solution, NaOH solution is 1: 0.12 with nitrate solution volume parts ratio in the step 1, behind the magnetic agitation 15min, be transferred in the water heating kettle, react 12h under 160 ℃ of hydrothermal conditions, filtration drying obtains the hollow aluminosilicate ball material.
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CN103071438A (en) * | 2013-01-07 | 2013-05-01 | 中国科学院合肥物质科学研究院 | Preparation method of core-shell structured micro-nanosphere comprising magnetic core and magnesium silicate nano-sheet shell |
CN103359749A (en) * | 2013-07-22 | 2013-10-23 | 东北师范大学 | Preparation method for porous rare earth silicate hollow spheres |
CN103635426A (en) * | 2011-03-11 | 2014-03-12 | 日立化成株式会社 | Aluminum silicate, metal ion adsorbent, and method for producing same |
CN104445228A (en) * | 2014-10-21 | 2015-03-25 | 中国建筑材料科学研究总院 | Hollow spherical type serpentine superfine powder and preparation method thereof |
CN106237975A (en) * | 2016-08-09 | 2016-12-21 | 北京化工大学 | A kind of high-ratio surface big pore volume adsorption of magnesium silicate material and its preparation method and application |
CN107500303A (en) * | 2017-08-14 | 2017-12-22 | 曲阜师范大学 | A kind of mesoporous magnesium silicate microballoon and its hydro-thermal thermal transition preparation method |
CN109796021A (en) * | 2019-04-04 | 2019-05-24 | 河北工业大学 | Utilize the method for iron tailings preparation ellipsoid zinc silicate compound adsorbent |
CN113716576A (en) * | 2021-07-29 | 2021-11-30 | 浙江工业大学 | Method for preparing hollow spherical zeolite by using natural zeolite |
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CN103635426A (en) * | 2011-03-11 | 2014-03-12 | 日立化成株式会社 | Aluminum silicate, metal ion adsorbent, and method for producing same |
CN103635426B (en) * | 2011-03-11 | 2017-03-01 | 日立化成株式会社 | Aluminosilicate, metal ion adsorbent and their manufacture method |
CN103071438A (en) * | 2013-01-07 | 2013-05-01 | 中国科学院合肥物质科学研究院 | Preparation method of core-shell structured micro-nanosphere comprising magnetic core and magnesium silicate nano-sheet shell |
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CN104445228A (en) * | 2014-10-21 | 2015-03-25 | 中国建筑材料科学研究总院 | Hollow spherical type serpentine superfine powder and preparation method thereof |
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CN109796021B (en) * | 2019-04-04 | 2022-04-05 | 河北工业大学 | Method for preparing ellipsoidal zinc silicate composite adsorbent by using iron tailings |
CN113716576A (en) * | 2021-07-29 | 2021-11-30 | 浙江工业大学 | Method for preparing hollow spherical zeolite by using natural zeolite |
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