CN108190896B - 一种有序介孔纳米二氧化硅微球的制备方法 - Google Patents
一种有序介孔纳米二氧化硅微球的制备方法 Download PDFInfo
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- CN108190896B CN108190896B CN201810056233.1A CN201810056233A CN108190896B CN 108190896 B CN108190896 B CN 108190896B CN 201810056233 A CN201810056233 A CN 201810056233A CN 108190896 B CN108190896 B CN 108190896B
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- ordered mesoporous
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- 238000002360 preparation method Methods 0.000 title claims description 15
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims abstract description 60
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 35
- 239000004094 surface-active agent Substances 0.000 claims abstract description 34
- 239000008367 deionised water Substances 0.000 claims abstract description 33
- 229910021641 deionized water Inorganic materials 0.000 claims abstract description 33
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 claims abstract description 24
- 229910052710 silicon Inorganic materials 0.000 claims abstract description 24
- 239000010703 silicon Substances 0.000 claims abstract description 24
- 238000003756 stirring Methods 0.000 claims abstract description 24
- 238000001035 drying Methods 0.000 claims abstract description 15
- 238000005406 washing Methods 0.000 claims abstract description 15
- 150000007529 inorganic bases Chemical class 0.000 claims abstract description 14
- 238000000034 method Methods 0.000 claims abstract description 12
- 239000004005 microsphere Substances 0.000 claims abstract description 11
- 239000003093 cationic surfactant Substances 0.000 claims abstract description 8
- 238000010438 heat treatment Methods 0.000 claims abstract description 5
- 238000002156 mixing Methods 0.000 claims abstract description 4
- 239000000377 silicon dioxide Substances 0.000 claims description 34
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 21
- LZZYPRNAOMGNLH-UHFFFAOYSA-M Cetrimonium bromide Chemical group [Br-].CCCCCCCCCCCCCCCC[N+](C)(C)C LZZYPRNAOMGNLH-UHFFFAOYSA-M 0.000 claims description 20
- BOTDANWDWHJENH-UHFFFAOYSA-N Tetraethyl orthosilicate Chemical group CCO[Si](OCC)(OCC)OCC BOTDANWDWHJENH-UHFFFAOYSA-N 0.000 claims description 18
- KWYUFKZDYYNOTN-UHFFFAOYSA-M Potassium hydroxide Chemical compound [OH-].[K+] KWYUFKZDYYNOTN-UHFFFAOYSA-M 0.000 claims description 9
- BWHMMNNQKKPAPP-UHFFFAOYSA-L potassium carbonate Substances [K+].[K+].[O-]C([O-])=O BWHMMNNQKKPAPP-UHFFFAOYSA-L 0.000 claims description 6
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical group N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 claims description 4
- CDBYLPFSWZWCQE-UHFFFAOYSA-L Sodium Carbonate Chemical compound [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 claims description 4
- 239000004115 Sodium Silicate Substances 0.000 claims description 3
- 239000006229 carbon black Substances 0.000 claims description 3
- PFKRTWCFCOUBHS-UHFFFAOYSA-N dimethyl(octadecyl)azanium;chloride Chemical compound [Cl-].CCCCCCCCCCCCCCCCCC[NH+](C)C PFKRTWCFCOUBHS-UHFFFAOYSA-N 0.000 claims description 3
- XJWSAJYUBXQQDR-UHFFFAOYSA-M dodecyltrimethylammonium bromide Chemical compound [Br-].CCCCCCCCCCCC[N+](C)(C)C XJWSAJYUBXQQDR-UHFFFAOYSA-M 0.000 claims description 3
- 229910000027 potassium carbonate Inorganic materials 0.000 claims description 3
- RMAQACBXLXPBSY-UHFFFAOYSA-N silicic acid Chemical compound O[Si](O)(O)O RMAQACBXLXPBSY-UHFFFAOYSA-N 0.000 claims description 3
- NTHWMYGWWRZVTN-UHFFFAOYSA-N sodium silicate Chemical compound [Na+].[Na+].[O-][Si]([O-])=O NTHWMYGWWRZVTN-UHFFFAOYSA-N 0.000 claims description 3
- 229910052911 sodium silicate Inorganic materials 0.000 claims description 3
- CXRFDZFCGOPDTD-UHFFFAOYSA-M Cetrimide Chemical compound [Br-].CCCCCCCCCCCCCC[N+](C)(C)C CXRFDZFCGOPDTD-UHFFFAOYSA-M 0.000 claims description 2
- UIIMBOGNXHQVGW-DEQYMQKBSA-M Sodium bicarbonate-14C Chemical compound [Na+].O[14C]([O-])=O UIIMBOGNXHQVGW-DEQYMQKBSA-M 0.000 claims description 2
- 229910021529 ammonia Inorganic materials 0.000 claims description 2
- 229910000029 sodium carbonate Inorganic materials 0.000 claims description 2
- SZEMGTQCPRNXEG-UHFFFAOYSA-M trimethyl(octadecyl)azanium;bromide Chemical compound [Br-].CCCCCCCCCCCCCCCCCC[N+](C)(C)C SZEMGTQCPRNXEG-UHFFFAOYSA-M 0.000 claims description 2
- 239000011148 porous material Substances 0.000 abstract description 18
- 239000002245 particle Substances 0.000 abstract description 9
- 235000012239 silicon dioxide Nutrition 0.000 abstract description 7
- 230000015572 biosynthetic process Effects 0.000 abstract description 6
- 239000005543 nano-size silicon particle Substances 0.000 abstract description 5
- 238000003786 synthesis reaction Methods 0.000 abstract description 4
- 238000004519 manufacturing process Methods 0.000 abstract description 3
- 230000035484 reaction time Effects 0.000 abstract description 3
- 238000005265 energy consumption Methods 0.000 abstract description 2
- 230000007613 environmental effect Effects 0.000 abstract 1
- 238000006243 chemical reaction Methods 0.000 description 15
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 12
- 238000003917 TEM image Methods 0.000 description 7
- 239000000463 material Substances 0.000 description 7
- 239000000693 micelle Substances 0.000 description 7
- 239000000203 mixture Substances 0.000 description 7
- 230000006872 improvement Effects 0.000 description 5
- UIIMBOGNXHQVGW-UHFFFAOYSA-M Sodium bicarbonate Chemical group [Na+].OC([O-])=O UIIMBOGNXHQVGW-UHFFFAOYSA-M 0.000 description 4
- 238000001308 synthesis method Methods 0.000 description 4
- 239000002105 nanoparticle Substances 0.000 description 3
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical group [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 2
- 230000009471 action Effects 0.000 description 2
- 239000003513 alkali Substances 0.000 description 2
- 230000005540 biological transmission Effects 0.000 description 2
- 239000007810 chemical reaction solvent Substances 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000008569 process Effects 0.000 description 2
- 239000011734 sodium Substances 0.000 description 2
- 229910000030 sodium bicarbonate Inorganic materials 0.000 description 2
- 235000017557 sodium bicarbonate Nutrition 0.000 description 2
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 description 1
- 102220500397 Neutral and basic amino acid transport protein rBAT_M41T_mutation Human genes 0.000 description 1
- 229910020489 SiO3 Inorganic materials 0.000 description 1
- 238000005411 Van der Waals force Methods 0.000 description 1
- 239000000654 additive Substances 0.000 description 1
- 235000011114 ammonium hydroxide Nutrition 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000003054 catalyst Substances 0.000 description 1
- 238000006555 catalytic reaction Methods 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 230000008021 deposition Effects 0.000 description 1
- 239000003814 drug Substances 0.000 description 1
- 230000007062 hydrolysis Effects 0.000 description 1
- 238000006460 hydrolysis reaction Methods 0.000 description 1
- 238000001027 hydrothermal synthesis Methods 0.000 description 1
- 229910001867 inorganic solvent Inorganic materials 0.000 description 1
- 239000003049 inorganic solvent Substances 0.000 description 1
- 239000013335 mesoporous material Substances 0.000 description 1
- -1 methyl quaternary ammonium salt Chemical class 0.000 description 1
- 239000002808 molecular sieve Substances 0.000 description 1
- 238000003541 multi-stage reaction Methods 0.000 description 1
- 239000002086 nanomaterial Substances 0.000 description 1
- 238000005580 one pot reaction Methods 0.000 description 1
- 239000003960 organic solvent Substances 0.000 description 1
- 238000006116 polymerization reaction Methods 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
- URGAHOPLAPQHLN-UHFFFAOYSA-N sodium aluminosilicate Chemical compound [Na+].[Al+3].[O-][Si]([O-])=O.[O-][Si]([O-])=O URGAHOPLAPQHLN-UHFFFAOYSA-N 0.000 description 1
- 238000001179 sorption measurement Methods 0.000 description 1
- 238000006557 surface reaction Methods 0.000 description 1
Images
Classifications
-
- 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
- C01B33/18—Preparation of finely divided silica neither in sol nor in gel form; After-treatment thereof
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/01—Particle morphology depicted by an image
- C01P2004/04—Particle morphology depicted by an image obtained by TEM, STEM, STM or AFM
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/60—Particles characterised by their size
- C01P2004/62—Submicrometer sized, i.e. from 0.1-1 micrometer
-
- 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
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Silicon Compounds (AREA)
- Silicates, Zeolites, And Molecular Sieves (AREA)
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Families Citing this family (10)
Publication number | Priority date | Publication date | Assignee | Title |
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CN109052416B (zh) * | 2018-08-13 | 2021-05-11 | 江西农业大学 | 一种层状有序超微孔材料及其合成方法 |
CN109607552B (zh) * | 2019-01-15 | 2021-10-22 | 河北工业大学 | 一种制备三维球链状结构二氧化硅的方法 |
CN109824053A (zh) * | 2019-03-08 | 2019-05-31 | 华南协同创新研究院 | 一种超小二氧化硅纳米链的制备方法 |
CN110591543B (zh) * | 2019-09-12 | 2021-02-12 | 陕西科技大学 | 一种二氧化硅负载壳聚糖改性水性聚氨酯丙烯酸酯复合乳液及其制备方法和应用 |
RU2740995C1 (ru) * | 2020-05-22 | 2021-01-22 | Федеральное государственное бюджетное образовательное учреждение высшего образования «Национальный исследовательский Мордовский государственный университет им. Н.П. Огарёва» | Способ получения микрокремнезема из природного диатомита осаждением раствора азотной кислоты |
CN111704458B (zh) * | 2020-05-24 | 2022-05-27 | 福建华夏金刚科技股份有限公司 | 一种含有二氧化硅纳米晶体的精细功能陶瓷及其制备方法 |
CN112174148B (zh) * | 2020-10-04 | 2022-02-25 | 贵州师范学院 | 一种合成高纯度六方柱形二氧化硅纳米多孔材料的方法 |
CN112226221B (zh) * | 2020-10-19 | 2022-03-01 | 河南大学 | 一种纳米二氧化硅驱油剂及其制备方法和应用 |
CN113800528A (zh) * | 2021-09-22 | 2021-12-17 | 蚌埠学院 | 一种以石英砂尾矿为原料制备功能化介孔纳米SiO2材料的方法及其应用 |
CN115676838B (zh) * | 2022-10-17 | 2024-05-03 | 广东粤港澳大湾区国家纳米科技创新研究院 | 纳米二氧化硅溶液及其制备方法与应用 |
Citations (7)
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US5425930A (en) * | 1993-09-17 | 1995-06-20 | Alliedsignal Inc. | Process for forming large silica spheres by low temperature nucleation |
CN101214962A (zh) * | 2008-01-11 | 2008-07-09 | 东南大学 | 复合模板法制备介孔二氧化硅微球的方法 |
CN101475183A (zh) * | 2009-01-15 | 2009-07-08 | 北京航空航天大学 | 空腔直径连续变化的中空介孔二氧化硅球的制备方法 |
CN101708853A (zh) * | 2009-07-08 | 2010-05-19 | 济南大学 | 不同表面形态的中空二氧化硅微球及其制备方法 |
CN102432024A (zh) * | 2011-09-14 | 2012-05-02 | 中山大学 | 一种中空介孔二氧化硅微球及其制备方法和用途 |
CN102718225A (zh) * | 2012-07-18 | 2012-10-10 | 中国人民解放军***南京总医院 | 一种空心结构的有序介孔二氧化硅微球的制备方法 |
CN106276925A (zh) * | 2016-08-12 | 2017-01-04 | 西北大学 | 一种制备介孔二氧化硅核壳微球的方法 |
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2018
- 2018-01-20 CN CN201810056233.1A patent/CN108190896B/zh active Active
Patent Citations (7)
Publication number | Priority date | Publication date | Assignee | Title |
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US5425930A (en) * | 1993-09-17 | 1995-06-20 | Alliedsignal Inc. | Process for forming large silica spheres by low temperature nucleation |
CN101214962A (zh) * | 2008-01-11 | 2008-07-09 | 东南大学 | 复合模板法制备介孔二氧化硅微球的方法 |
CN101475183A (zh) * | 2009-01-15 | 2009-07-08 | 北京航空航天大学 | 空腔直径连续变化的中空介孔二氧化硅球的制备方法 |
CN101708853A (zh) * | 2009-07-08 | 2010-05-19 | 济南大学 | 不同表面形态的中空二氧化硅微球及其制备方法 |
CN102432024A (zh) * | 2011-09-14 | 2012-05-02 | 中山大学 | 一种中空介孔二氧化硅微球及其制备方法和用途 |
CN102718225A (zh) * | 2012-07-18 | 2012-10-10 | 中国人民解放军***南京总医院 | 一种空心结构的有序介孔二氧化硅微球的制备方法 |
CN106276925A (zh) * | 2016-08-12 | 2017-01-04 | 西北大学 | 一种制备介孔二氧化硅核壳微球的方法 |
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