CN113429964A - Preparation method of fluorescent amino clay - Google Patents
Preparation method of fluorescent amino clay Download PDFInfo
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- CN113429964A CN113429964A CN202110713608.9A CN202110713608A CN113429964A CN 113429964 A CN113429964 A CN 113429964A CN 202110713608 A CN202110713608 A CN 202110713608A CN 113429964 A CN113429964 A CN 113429964A
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- amino clay
- fluorescent amino
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- ethanol
- aminoethylamino
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- 125000002924 primary amino group Chemical group [H]N([H])* 0.000 title claims abstract description 59
- 239000004927 clay Substances 0.000 title claims abstract description 57
- 238000002360 preparation method Methods 0.000 title claims abstract description 11
- 238000000034 method Methods 0.000 claims abstract description 16
- 229910052751 metal Inorganic materials 0.000 claims abstract description 11
- 239000002184 metal Substances 0.000 claims abstract description 11
- 150000001875 compounds Chemical class 0.000 claims abstract description 9
- 150000003839 salts Chemical class 0.000 claims abstract description 9
- FZHAPNGMFPVSLP-UHFFFAOYSA-N silanamine Chemical compound [SiH3]N FZHAPNGMFPVSLP-UHFFFAOYSA-N 0.000 claims abstract description 9
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 92
- 238000003756 stirring Methods 0.000 claims description 50
- 238000001035 drying Methods 0.000 claims description 23
- 238000005406 washing Methods 0.000 claims description 23
- 238000006243 chemical reaction Methods 0.000 claims description 21
- CDAWCLOXVUBKRW-UHFFFAOYSA-N 2-aminophenol Chemical compound NC1=CC=CC=C1O CDAWCLOXVUBKRW-UHFFFAOYSA-N 0.000 claims description 10
- QIGBRXMKCJKVMJ-UHFFFAOYSA-N Hydroquinone Chemical compound OC1=CC=C(O)C=C1 QIGBRXMKCJKVMJ-UHFFFAOYSA-N 0.000 claims description 10
- VYFYYTLLBUKUHU-UHFFFAOYSA-N dopamine Chemical compound NCCC1=CC=C(O)C(O)=C1 VYFYYTLLBUKUHU-UHFFFAOYSA-N 0.000 claims description 10
- INJVFBCDVXYHGQ-UHFFFAOYSA-N n'-(3-triethoxysilylpropyl)ethane-1,2-diamine Chemical compound CCO[Si](OCC)(OCC)CCCNCCN INJVFBCDVXYHGQ-UHFFFAOYSA-N 0.000 claims description 9
- 229930187593 rose bengal Natural products 0.000 claims description 9
- AZJPTIGZZTZIDR-UHFFFAOYSA-L rose bengal Chemical compound [K+].[K+].[O-]C(=O)C1=C(Cl)C(Cl)=C(Cl)C(Cl)=C1C1=C2C=C(I)C(=O)C(I)=C2OC2=C(I)C([O-])=C(I)C=C21 AZJPTIGZZTZIDR-UHFFFAOYSA-L 0.000 claims description 9
- 229940081623 rose bengal Drugs 0.000 claims description 9
- STRXNPAVPKGJQR-UHFFFAOYSA-N rose bengal A Natural products O1C(=O)C(C(=CC=C2Cl)Cl)=C2C21C1=CC(I)=C(O)C(I)=C1OC1=C(I)C(O)=C(I)C=C21 STRXNPAVPKGJQR-UHFFFAOYSA-N 0.000 claims description 9
- YCIMNLLNPGFGHC-UHFFFAOYSA-N catechol Chemical compound OC1=CC=CC=C1O YCIMNLLNPGFGHC-UHFFFAOYSA-N 0.000 claims description 8
- PHQOGHDTIVQXHL-UHFFFAOYSA-N n'-(3-trimethoxysilylpropyl)ethane-1,2-diamine Chemical compound CO[Si](OC)(OC)CCCNCCN PHQOGHDTIVQXHL-UHFFFAOYSA-N 0.000 claims description 8
- 229920000642 polymer Polymers 0.000 claims description 8
- 238000010992 reflux Methods 0.000 claims description 8
- GEYOCULIXLDCMW-UHFFFAOYSA-N 1,2-phenylenediamine Chemical compound NC1=CC=CC=C1N GEYOCULIXLDCMW-UHFFFAOYSA-N 0.000 claims description 7
- CWLKGDAVCFYWJK-UHFFFAOYSA-N 3-aminophenol Chemical compound NC1=CC=CC(O)=C1 CWLKGDAVCFYWJK-UHFFFAOYSA-N 0.000 claims description 6
- KRKNYBCHXYNGOX-UHFFFAOYSA-N citric acid Chemical compound OC(=O)CC(O)(C(O)=O)CC(O)=O KRKNYBCHXYNGOX-UHFFFAOYSA-N 0.000 claims description 6
- PPASLZSBLFJQEF-RKJRWTFHSA-M sodium ascorbate Substances [Na+].OC[C@@H](O)[C@H]1OC(=O)C(O)=C1[O-] PPASLZSBLFJQEF-RKJRWTFHSA-M 0.000 claims description 6
- 235000010378 sodium ascorbate Nutrition 0.000 claims description 6
- 229960005055 sodium ascorbate Drugs 0.000 claims description 6
- PPASLZSBLFJQEF-RXSVEWSESA-M sodium-L-ascorbate Chemical compound [Na+].OC[C@H](O)[C@H]1OC(=O)C(O)=C1[O-] PPASLZSBLFJQEF-RXSVEWSESA-M 0.000 claims description 6
- 239000000243 solution Substances 0.000 claims description 6
- SJECZPVISLOESU-UHFFFAOYSA-N 3-trimethoxysilylpropan-1-amine Chemical compound CO[Si](OC)(OC)CCCN SJECZPVISLOESU-UHFFFAOYSA-N 0.000 claims description 5
- 229960003638 dopamine Drugs 0.000 claims description 5
- PLIKAWJENQZMHA-UHFFFAOYSA-N 4-aminophenol Chemical compound NC1=CC=C(O)C=C1 PLIKAWJENQZMHA-UHFFFAOYSA-N 0.000 claims description 4
- PAYRUJLWNCNPSJ-UHFFFAOYSA-N Aniline Chemical compound NC1=CC=CC=C1 PAYRUJLWNCNPSJ-UHFFFAOYSA-N 0.000 claims description 4
- CIWBSHSKHKDKBQ-JLAZNSOCSA-N Ascorbic acid Chemical compound OC[C@H](O)[C@H]1OC(=O)C(O)=C1O CIWBSHSKHKDKBQ-JLAZNSOCSA-N 0.000 claims description 4
- OAKJQQAXSVQMHS-UHFFFAOYSA-N Hydrazine Chemical compound NN OAKJQQAXSVQMHS-UHFFFAOYSA-N 0.000 claims description 4
- 229910052782 aluminium Inorganic materials 0.000 claims description 4
- -1 polytetrafluoroethylene Polymers 0.000 claims description 4
- 229920001343 polytetrafluoroethylene Polymers 0.000 claims description 4
- 239000004810 polytetrafluoroethylene Substances 0.000 claims description 4
- 239000000843 powder Substances 0.000 claims description 4
- GHMLBKRAJCXXBS-UHFFFAOYSA-N resorcinol Chemical compound OC1=CC=CC(O)=C1 GHMLBKRAJCXXBS-UHFFFAOYSA-N 0.000 claims description 4
- 239000007787 solid Substances 0.000 claims description 4
- WZCQRUWWHSTZEM-UHFFFAOYSA-N 1,3-phenylenediamine Chemical compound NC1=CC=CC(N)=C1 WZCQRUWWHSTZEM-UHFFFAOYSA-N 0.000 claims description 3
- 229940018563 3-aminophenol Drugs 0.000 claims description 3
- 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 3
- 239000008103 glucose Substances 0.000 claims description 3
- 229940018564 m-phenylenediamine Drugs 0.000 claims description 3
- 239000000047 product Substances 0.000 claims description 3
- WYTZZXDRDKSJID-UHFFFAOYSA-N (3-aminopropyl)triethoxysilane Chemical compound CCO[Si](OCC)(OCC)CCCN WYTZZXDRDKSJID-UHFFFAOYSA-N 0.000 claims description 2
- CBCKQZAAMUWICA-UHFFFAOYSA-N 1,4-phenylenediamine Chemical compound NC1=CC=C(N)C=C1 CBCKQZAAMUWICA-UHFFFAOYSA-N 0.000 claims description 2
- QTBSBXVTEAMEQO-UHFFFAOYSA-M Acetate Chemical compound CC([O-])=O QTBSBXVTEAMEQO-UHFFFAOYSA-M 0.000 claims description 2
- 229910052684 Cerium Inorganic materials 0.000 claims description 2
- VEXZGXHMUGYJMC-UHFFFAOYSA-M Chloride anion Chemical compound [Cl-] VEXZGXHMUGYJMC-UHFFFAOYSA-M 0.000 claims description 2
- 229910052693 Europium Inorganic materials 0.000 claims description 2
- 229910002651 NO3 Inorganic materials 0.000 claims description 2
- NHNBFGGVMKEFGY-UHFFFAOYSA-N Nitrate Chemical compound [O-][N+]([O-])=O NHNBFGGVMKEFGY-UHFFFAOYSA-N 0.000 claims description 2
- ISWSIDIOOBJBQZ-UHFFFAOYSA-N Phenol Chemical compound OC1=CC=CC=C1 ISWSIDIOOBJBQZ-UHFFFAOYSA-N 0.000 claims description 2
- QAOWNCQODCNURD-UHFFFAOYSA-L Sulfate Chemical compound [O-]S([O-])(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-L 0.000 claims description 2
- 229910052771 Terbium Inorganic materials 0.000 claims description 2
- 229910052775 Thulium Inorganic materials 0.000 claims description 2
- 239000007864 aqueous solution Substances 0.000 claims description 2
- 235000010323 ascorbic acid Nutrition 0.000 claims description 2
- 239000011668 ascorbic acid Substances 0.000 claims description 2
- 229960005070 ascorbic acid Drugs 0.000 claims description 2
- WQZGKKKJIJFFOK-VFUOTHLCSA-N beta-D-glucose Chemical compound OC[C@H]1O[C@@H](O)[C@H](O)[C@@H](O)[C@@H]1O WQZGKKKJIJFFOK-VFUOTHLCSA-N 0.000 claims description 2
- KGBXLFKZBHKPEV-UHFFFAOYSA-N boric acid Chemical compound OB(O)O KGBXLFKZBHKPEV-UHFFFAOYSA-N 0.000 claims description 2
- 239000004327 boric acid Substances 0.000 claims description 2
- 229910052793 cadmium Inorganic materials 0.000 claims description 2
- 229910052792 caesium Inorganic materials 0.000 claims description 2
- VYXSBFYARXAAKO-WTKGSRSZSA-N chembl402140 Chemical compound Cl.C1=2C=C(C)C(NCC)=CC=2OC2=C\C(=N/CC)C(C)=CC2=C1C1=CC=CC=C1C(=O)OCC VYXSBFYARXAAKO-WTKGSRSZSA-N 0.000 claims description 2
- 229910052804 chromium Inorganic materials 0.000 claims description 2
- 229910052802 copper Inorganic materials 0.000 claims description 2
- 239000008367 deionised water Substances 0.000 claims description 2
- 229910021641 deionized water Inorganic materials 0.000 claims description 2
- 238000001027 hydrothermal synthesis Methods 0.000 claims description 2
- 229910052738 indium Inorganic materials 0.000 claims description 2
- 229910052741 iridium Inorganic materials 0.000 claims description 2
- 229910052742 iron Inorganic materials 0.000 claims description 2
- 229910052745 lead Inorganic materials 0.000 claims description 2
- 229910052749 magnesium Inorganic materials 0.000 claims description 2
- 229910052750 molybdenum Inorganic materials 0.000 claims description 2
- 229910052759 nickel Inorganic materials 0.000 claims description 2
- 229910052758 niobium Inorganic materials 0.000 claims description 2
- 229910052763 palladium Inorganic materials 0.000 claims description 2
- VLTRZXGMWDSKGL-UHFFFAOYSA-M perchlorate Inorganic materials [O-]Cl(=O)(=O)=O VLTRZXGMWDSKGL-UHFFFAOYSA-M 0.000 claims description 2
- VLTRZXGMWDSKGL-UHFFFAOYSA-N perchloric acid Chemical compound OCl(=O)(=O)=O VLTRZXGMWDSKGL-UHFFFAOYSA-N 0.000 claims description 2
- 229910052697 platinum Inorganic materials 0.000 claims description 2
- 229920000767 polyaniline Polymers 0.000 claims description 2
- 239000002244 precipitate Substances 0.000 claims description 2
- HNJBEVLQSNELDL-UHFFFAOYSA-N pyrrolidin-2-one Chemical compound O=C1CCCN1 HNJBEVLQSNELDL-UHFFFAOYSA-N 0.000 claims description 2
- PYWVYCXTNDRMGF-UHFFFAOYSA-N rhodamine B Chemical compound [Cl-].C=12C=CC(=[N+](CC)CC)C=C2OC2=CC(N(CC)CC)=CC=C2C=1C1=CC=CC=C1C(O)=O PYWVYCXTNDRMGF-UHFFFAOYSA-N 0.000 claims description 2
- 229940043267 rhodamine b Drugs 0.000 claims description 2
- 229910052703 rhodium Inorganic materials 0.000 claims description 2
- 229910052707 ruthenium Inorganic materials 0.000 claims description 2
- 229910052709 silver Inorganic materials 0.000 claims description 2
- 239000001509 sodium citrate Substances 0.000 claims description 2
- NLJMYIDDQXHKNR-UHFFFAOYSA-K sodium citrate Chemical compound O.O.[Na+].[Na+].[Na+].[O-]C(=O)CC(O)(CC([O-])=O)C([O-])=O NLJMYIDDQXHKNR-UHFFFAOYSA-K 0.000 claims description 2
- 229910052718 tin Inorganic materials 0.000 claims description 2
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical group O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 2
- 238000005303 weighing Methods 0.000 claims description 2
- 229910052725 zinc Inorganic materials 0.000 claims description 2
- 238000003384 imaging method Methods 0.000 abstract description 49
- 230000001699 photocatalysis Effects 0.000 abstract description 23
- 238000007146 photocatalysis Methods 0.000 abstract description 23
- 238000002595 magnetic resonance imaging Methods 0.000 abstract description 10
- 206010028980 Neoplasm Diseases 0.000 abstract description 3
- 239000005416 organic matter Substances 0.000 abstract 1
- 238000001816 cooling Methods 0.000 description 21
- 238000000967 suction filtration Methods 0.000 description 21
- 229940050906 magnesium chloride hexahydrate Drugs 0.000 description 10
- DHRRIBDTHFBPNG-UHFFFAOYSA-L magnesium dichloride hexahydrate Chemical compound O.O.O.O.O.O.[Mg+2].[Cl-].[Cl-] DHRRIBDTHFBPNG-UHFFFAOYSA-L 0.000 description 10
- TWRXJAOTZQYOKJ-UHFFFAOYSA-L Magnesium chloride Chemical compound [Mg+2].[Cl-].[Cl-] TWRXJAOTZQYOKJ-UHFFFAOYSA-L 0.000 description 4
- 229910021380 Manganese Chloride Inorganic materials 0.000 description 4
- GLFNIEUTAYBVOC-UHFFFAOYSA-L Manganese chloride Chemical compound Cl[Mn]Cl GLFNIEUTAYBVOC-UHFFFAOYSA-L 0.000 description 4
- VSCWAEJMTAWNJL-UHFFFAOYSA-K aluminium trichloride Chemical compound Cl[Al](Cl)Cl VSCWAEJMTAWNJL-UHFFFAOYSA-K 0.000 description 4
- MEANOSLIBWSCIT-UHFFFAOYSA-K gadolinium trichloride Chemical compound Cl[Gd](Cl)Cl MEANOSLIBWSCIT-UHFFFAOYSA-K 0.000 description 4
- 239000011565 manganese chloride Substances 0.000 description 4
- 235000002867 manganese chloride Nutrition 0.000 description 4
- 229940099607 manganese chloride Drugs 0.000 description 4
- ZMANZCXQSJIPKH-UHFFFAOYSA-N Triethylamine Chemical compound CCN(CC)CC ZMANZCXQSJIPKH-UHFFFAOYSA-N 0.000 description 3
- 229940063656 aluminum chloride Drugs 0.000 description 2
- 238000001917 fluorescence detection Methods 0.000 description 2
- 229960002337 magnesium chloride Drugs 0.000 description 2
- 229910001629 magnesium chloride Inorganic materials 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 238000003541 multi-stage reaction Methods 0.000 description 2
- 239000002086 nanomaterial Substances 0.000 description 2
- JIAARYAFYJHUJI-UHFFFAOYSA-L zinc dichloride Chemical compound [Cl-].[Cl-].[Zn+2] JIAARYAFYJHUJI-UHFFFAOYSA-L 0.000 description 2
- BLRPTPMANUNPDV-UHFFFAOYSA-N Silane Chemical compound [SiH4] BLRPTPMANUNPDV-UHFFFAOYSA-N 0.000 description 1
- JGDITNMASUZKPW-UHFFFAOYSA-K aluminium trichloride hexahydrate Chemical compound O.O.O.O.O.O.Cl[Al](Cl)Cl JGDITNMASUZKPW-UHFFFAOYSA-K 0.000 description 1
- 229940009861 aluminum chloride hexahydrate Drugs 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 239000010949 copper Substances 0.000 description 1
- ORTQZVOHEJQUHG-UHFFFAOYSA-L copper(II) chloride Chemical compound Cl[Cu]Cl ORTQZVOHEJQUHG-UHFFFAOYSA-L 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 239000011777 magnesium Substances 0.000 description 1
- 229910021645 metal ion Inorganic materials 0.000 description 1
- 238000005424 photoluminescence Methods 0.000 description 1
- 229910052761 rare earth metal Inorganic materials 0.000 description 1
- 150000002910 rare earth metals Chemical class 0.000 description 1
- 229910000077 silane Inorganic materials 0.000 description 1
- 239000011701 zinc Substances 0.000 description 1
- 239000011592 zinc chloride Substances 0.000 description 1
- 235000005074 zinc chloride Nutrition 0.000 description 1
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09K—MATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
- C09K11/00—Luminescent, e.g. electroluminescent, chemiluminescent materials
- C09K11/06—Luminescent, e.g. electroluminescent, chemiluminescent materials containing organic luminescent materials
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09K—MATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
- C09K11/00—Luminescent, e.g. electroluminescent, chemiluminescent materials
- C09K11/08—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials
- C09K11/59—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials containing silicon
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09K—MATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
- C09K11/00—Luminescent, e.g. electroluminescent, chemiluminescent materials
- C09K11/08—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials
- C09K11/64—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials containing aluminium
- C09K11/646—Silicates
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09K—MATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
- C09K11/00—Luminescent, e.g. electroluminescent, chemiluminescent materials
- C09K11/08—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials
- C09K11/77—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials containing rare earth metals
- C09K11/77062—Silicates
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- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Organic Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Luminescent Compositions (AREA)
- Medicines Containing Antibodies Or Antigens For Use As Internal Diagnostic Agents (AREA)
Abstract
The invention relates to a preparation method of fluorescent amino clay, which uses metal salt, aminosilane and micromolecular compound or organic matter to realize one-step preparation of the fluorescent amino clay. The method has the advantages of easy operation, good repeatability, high fluorescence intensity of the prepared amino clay, good light stability and the like, and can be popularized and used. The prepared fluorescent amino clay can be applied to the photoelectric fields of biochemical sensing, photocatalysis, cell imaging, tumor treatment, living body imaging, magnetic resonance imaging, biomedicine, anti-counterfeiting, LED and the like.
Description
Technical Field
The invention relates to the field of nano materials, in particular to a preparation method of fluorescent amino clay.
Background
The fluorescent amino clay is a fluorescent nano material formed by metal ions and silane, and is an important functional material, such as fluorescent sensing, cell imaging, tumor treatment, biomedicine, anti-counterfeiting, photoluminescence, photocatalysis and the like. The fluorescent amino clay is a nano-scale two-dimensional material, has larger specific surface area, abundant amino and very strong fluorescence, and can be used in the fields of fluorescence detection, cell imaging, magnetic resonance imaging, biomedicine, anti-counterfeiting, light-emitting diodes and the like.
Although nanoclays have long been prepared and utilized, fluorescent nanoclays are less studied. In recent years, the preparation of fluorescent amino clays has been mainly prepared by a complex multi-step reaction. Li and the like prepare water-soluble amino clay for fluorescence detection of triethylamine through rare earth complex modification, and the water-soluble amino clay is also modified by organic fluorescent groups and applied to cell imaging. These methods involve multi-step reactions and are complicated to operate.
Disclosure of Invention
The invention aims to solve the problems in the prior art and provides a preparation method for fluorescent amino clay. The method has the advantages of easy operation, good repeatability, high fluorescence intensity of the prepared amino clay, good light stability and the like, and can be popularized and used.
In order to achieve the purpose, the technical scheme provided by the invention is as follows:
a preparation method of fluorescent amino clay comprises the following steps:
(1) weighing a certain amount of metal salt and dissolving in a certain amount of ethanol;
(2) dissolving a certain amount of aminosilane into the solution obtained in the step (1), and stirring for 1-48 h;
(3) adding a certain amount of small molecular compounds or polymers into the solution obtained in the step (2) under the condition of stirring, and stirring for 0.5-12 h; refluxing at 30-100 deg.C for 1-12 hr, or transferring into a reaction kettle with polytetrafluoroethylene lining at 110-200 deg.C
Reacting for 1-12h to obtain a fluorescent amino clay product;
(4) centrifuging and washing to obtain the precipitate, and drying to obtain the fluorescent amino clay solid powder.
In the step (1), the metal salt is selected from one or more of nitrate, chloride, sulfate, acetate or perchlorate.
Further, the metal is selected from one or more of Mg, Al, Zn, Fe, Co, Ni, Cu, Ag, Cd, Cs, Ba, Bi, Pb, Sn, Al, In, Pd, Pt, Au, Mn, Cr, Mo, Nb, Ru, Rh, Ir, Ce, Eu, Tb and Tm.
In the step (1), the mass/volume ratio of the metal salt to the ethanol is (0.01-0.1): 1 g/mL.
In the step (2), the mass/volume ratio of the metal salt to the aminosilane is (0.5-2.5): 1 g/mL.
Further, the aminosilane is selected from one or more of 3-aminopropyltrimethoxysilane, 3-aminopropyltriethoxysilane, 3- (2-aminoethylamino) propyltrimethoxysilane, 3- (2-aminoethylamino) propyltriethoxysilane, 3- [2- (2-aminoethylamino) ethylamino-trimethoxysilane, and 3- [2- (2-aminoethylamino) ethylamino-triethoxysilane.
Further, the fluorescent amino clay is obtained under the condition of a small molecular compound or a polymer; the micromolecular compound or polymer is selected from one or more of ascorbic acid, sodium ascorbate, citric acid, sodium citrate, glucose, boric acid, hydrazine, aniline, phenol, phenylenediamine, benzenediol, aminophenol, dopamine, rose bengal, rhodamine B, rhodamine 6G, polyalkyl pyrrolidone, oligomeric dopamine, polyaniline and the like; wherein the phenylenediamine comprises o-phenylenediamine, m-phenylenediamine and p-phenylenediamine; the diphenols include catechol, resorcinol, and hydroquinone; aminophenols include o-aminophenol, m-aminophenol, p-aminophenol; the ratio of the small molecular compound or the polymer to the aminosilane is 0.5-25 g/L.
In the step (3), the stirring is carried out for 0.5 to 12 hours; refluxing for 1-12h at 30-100 ℃, or transferring to a polytetrafluoroethylene lined reaction kettle, and then carrying out hydrothermal reaction at 110-200 ℃ for 1-12 h.
And dissolving the obtained fluorescent amino clay solid powder in secondary deionized water to obtain a fluorescent amino clay aqueous solution, wherein fluorescence can be observed under ultraviolet light.
Compared with the prior art, the invention has the beneficial effects that:
the method for preparing the fluorescent amino clay is easy to operate, can be completed in one step, and is low in cost, simple in preparation process, short in experimental period, good in repeatability, high in fluorescence intensity of a product and good in light stability.
The prepared fluorescent amino clay can be applied to the photoelectric fields of biochemical sensing, photocatalysis, cell imaging, tumor treatment, living body imaging, magnetic resonance imaging, biomedicine, anti-counterfeiting, LED and the like.
Drawings
FIG. 1: the flow diagram of the preparation method of the fluorescent amino clay is shown.
Detailed Description
The above-mentioned contents of the present invention are further described in detail by way of examples below, but it should not be understood that the scope of the above-mentioned subject matter of the present invention is limited to the following examples, and any technique realized based on the above-mentioned contents of the present invention falls within the scope of the present invention.
The experimental procedures used in the examples below are conventional procedures unless otherwise specified, and the reagents, methods and equipment used therein are conventional in the art unless otherwise specified.
Example 1
Dissolving 0.9g of magnesium chloride hexahydrate in 20mL of ethanol, dropwise adding 1.6mL of 3- (2-aminoethylamino) propyl trimethoxy silane, stirring for 12h, adding 20mg of hydroquinone, stirring for 0.5h, refluxing at 60 ℃ for 4h, cooling to room temperature, performing suction filtration, washing with ethanol for several times, and drying at 60 ℃ to obtain the fluorescent amino clay. Can be applied to the photoelectric fields of biochemical sensing, photocatalysis, cell imaging, living body imaging, anti-counterfeiting, LED and the like.
Example 2
Dissolving 1.5g of magnesium chloride hexahydrate in 30mL of ethanol, dropwise adding 1.8mL of 3- [2- (2-aminoethylamino) ethylamino-trimethoxy silane, stirring for 8h, then adding 25mg of m-phenylenediamine, stirring for 1h, transferring into a reaction kettle, keeping at 180 ℃ for 8h, cooling to room temperature, carrying out suction filtration, washing with ethanol for several times, and drying at 60 ℃ to obtain the fluorescent amino clay. Can be applied to the photoelectric fields of biochemical sensing, photocatalysis, cell imaging, living body imaging, anti-counterfeiting, LED and the like.
Example 3
Dissolving 1.1g of aluminum chloride in 25mL of ethanol, dropwise adding 1.5mL of 3- (2-aminoethylamino) propyl trimethoxy silane, stirring for 12h, adding 30mg of hydroquinone, stirring for 2h, transferring to a reaction kettle, keeping at 200 ℃ for 8h, cooling to room temperature, performing suction filtration, washing with ethanol for several times, and drying at 60 ℃ to obtain the fluorescent amino clay. Can be applied to the photoelectric fields of biochemical sensing, photocatalysis, cell imaging, living body imaging, anti-counterfeiting, LED and the like.
Example 4
Dissolving 1.1g of aluminum chloride in 25mL of ethanol, dropwise adding 1.6mL of 3- (2-aminoethylamino) propyl trimethoxy silane, stirring for 12h, adding 40mg of m-aminophenol, stirring for 0.5h, transferring to a reaction kettle, keeping at 120 ℃ for 12h, cooling to room temperature, performing suction filtration, washing with ethanol for several times, and drying at 60 ℃ to obtain the fluorescent amino clay. Can be applied to the photoelectric fields of biochemical sensing, photocatalysis, cell imaging, living body imaging, anti-counterfeiting, LED and the like.
Example 5
Dissolving 0.9g of magnesium chloride hexahydrate in 20mL of ethanol, dropwise adding 1.6mL of 3- (2-aminoethylamino) propyl trimethoxy silane, stirring for 12h, adding 40mg of o-aminophenol, stirring for 0.5h, refluxing at 70 ℃ for 6h, cooling to room temperature, performing suction filtration, washing with ethanol for several times, and drying at 60 ℃ to obtain the fluorescent amino clay. Can be applied to the photoelectric fields of biochemical sensing, photocatalysis, cell imaging, living body imaging, anti-counterfeiting, LED and the like.
Example 5
Dissolving 0.9g of zinc chloride in 20mL of ethanol, dropwise adding 3-aminopropyltrimethoxysilane of 1.6mL, stirring for 12h, then adding 20mg of hydroquinone, stirring for 0.5h, refluxing at 60 ℃ for 4h, cooling to room temperature, carrying out suction filtration, washing with ethanol for several times, and drying at 60 ℃ to obtain the yellowish-brown amino clay. Can be applied to the photoelectric fields of biochemical sensing, photocatalysis, cell imaging, living body imaging, anti-counterfeiting, LED and the like.
Example 6
Dissolving 0.9g of magnesium chloride hexahydrate in 20mL of ethanol, dropwise adding 3- [2- (2-aminoethylamino) ethylamino-trimethoxy silane in 1.8mL of the solution, stirring for 12h, adding glucose in an amount of 50mg, stirring for 0.5h, refluxing at 60 ℃ for 6h, cooling to room temperature, performing suction filtration, washing with ethanol for several times, and drying at 60 ℃ to obtain yellowish-brown amino clay. Can be applied to the photoelectric fields of biochemical sensing, photocatalysis, cell imaging, living body imaging, anti-counterfeiting, LED and the like.
Example 7
Dissolving 1g of magnesium chloride hexahydrate in 20mL of ethanol, dropwise adding 2mL of 3-aminopropyltrimethoxysilane, stirring for 1h, adding 30mg of sodium ascorbate, stirring for 0.5h, transferring into a reaction kettle, keeping at 160 ℃ for 8h, cooling to room temperature, performing suction filtration, washing with ethanol for several times, and drying at 60 ℃ to obtain light yellow amino clay. Can be applied to the photoelectric fields of biochemical sensing, photocatalysis, cell imaging, living body imaging, anti-counterfeiting, LED and the like.
Example 8
Dissolving 1g of magnesium chloride hexahydrate in 20mL of ethanol, dropwise adding 2mL of 3-aminopropyltrimethoxysilane, stirring for 1h, adding 30mg of sodium ascorbate, stirring for 0.5h, transferring into a reaction kettle, keeping the temperature at 180 ℃ for 4h, cooling to room temperature, performing suction filtration, washing with ethanol for several times, and drying at 60 ℃ to obtain light yellow amino clay. Can be applied to the photoelectric fields of biochemical sensing, photocatalysis, cell imaging, living body imaging, anti-counterfeiting, LED and the like.
Example 9
Dissolving 1g of magnesium chloride hexahydrate in 20mL of ethanol, dropwise adding 2.2mL of 3- (2-aminoethylamino) propyltriethoxysilane, stirring for 1h, then adding 30mg of sodium ascorbate, stirring for 0.5h, transferring into a reaction kettle, keeping at 180 ℃ for 4h, cooling to room temperature, performing suction filtration, washing with ethanol for several times, and drying at 60 ℃ to obtain light yellow amino clay. Can be applied to the photoelectric fields of biochemical sensing, photocatalysis, cell imaging, living body imaging, anti-counterfeiting, LED and the like.
Example 10
Dissolving 1g of magnesium chloride hexahydrate in 20mL of ethanol, dropwise adding 2.2mL of 3- (2-aminoethylamino) propyltriethoxysilane, stirring for 1h, adding 30mg of catechol, stirring for 0.5h, transferring to a reaction kettle, keeping at 180 ℃ for 4h, cooling to room temperature, performing suction filtration, washing with ethanol for several times, and drying at 60 ℃ to obtain light yellow amino clay. Can be applied to the photoelectric fields of biochemical sensing, photocatalysis, cell imaging, living body imaging, anti-counterfeiting, LED and the like.
Example 11
Dissolving 1g of magnesium chloride hexahydrate in 20mL of ethanol, dropwise adding 2.2mL of 3- (2-aminoethylamino) propyltriethoxysilane, stirring for 1h, adding 30mg of o-phenylenediamine, stirring for 0.5h, transferring into a reaction kettle, keeping at 180 ℃ for 8h, cooling to room temperature, performing suction filtration, washing with ethanol for several times, and drying at 60 ℃ to obtain light yellow amino clay. Can be applied to the photoelectric fields of biochemical sensing, photocatalysis, cell imaging, living body imaging, anti-counterfeiting, LED and the like.
Example 12
Dissolving 1g of aluminum chloride hexahydrate in 20mL of ethanol, dropwise adding 2.2mL of 3- (2-aminoethylamino) propyltriethoxysilane, stirring for 1h, adding 30mg of dopamine, stirring for 0.5h, transferring to a reaction kettle, keeping at 160 ℃ for 8h, cooling to room temperature, performing suction filtration, washing with ethanol for several times, and drying at 60 ℃ to obtain light yellow amino clay. Can be applied to the photoelectric fields of biochemical sensing, photocatalysis, cell imaging, living body imaging, anti-counterfeiting, LED and the like.
Example 13
Dissolving 1g of magnesium chloride hexahydrate in 20mL of ethanol, dropwise adding 2.2mL of 3- (2-aminoethylamino) propyl triethoxysilane, stirring for 1h, then adding 20mg of rose bengal, stirring for 0.5h, transferring into a reaction kettle, keeping at 180 ℃ for 4h, cooling to room temperature, performing suction filtration, washing with ethanol for several times, and drying at 60 ℃ to obtain light yellow amino clay which shows strong yellow green fluorescence under an ultraviolet lamp. Can be applied to the photoelectric fields of biochemical sensing, photocatalysis, cell imaging, living body imaging, anti-counterfeiting, LED and the like.
Example 14
Dissolving 1g of gadolinium chloride in 20mL of ethanol, dropwise adding 2.2mL of 3- (2-aminoethylamino) propyltriethoxysilane, stirring for 1h, adding 20mg of rose bengal, stirring for 0.5h, transferring to a reaction kettle, keeping at 180 ℃ for 8h, cooling to room temperature, performing suction filtration, washing with ethanol for several times, and drying at 60 ℃ to obtain the amino clay. Can be applied to the photoelectric fields of biochemical sensing, cell imaging, living body imaging, magnetic resonance imaging, biomedicine, LED and the like.
Example 15
Dissolving 1.1g of manganese chloride in 20mL of ethanol, dropwise adding 2.2mL of 3- (2-aminoethylamino) propyltriethoxysilane, stirring for 1h, adding 30mg of sodium ascorbate, stirring for 0.5h, transferring to a reaction kettle, keeping at 180 ℃ for 8h, cooling to room temperature, performing suction filtration, washing with ethanol for several times, and drying at 60 ℃ to obtain the amino clay. Can be applied to the photoelectric fields of biochemical sensing, photocatalysis, cell imaging, living body imaging, magnetic resonance imaging, biomedicine, anti-counterfeiting, LED and the like.
Example 16
Dissolving 1.1g of manganese chloride in 20mL of ethanol, dropwise adding 1.5mL of 3- [2- (2-aminoethylamino) ethylamino-triethoxysilane, stirring for 1h, then adding 20mg of rose bengal, stirring for 0.5h, transferring into a reaction kettle, keeping at 180 ℃ for 4h, cooling to room temperature, performing suction filtration, washing with ethanol for several times, and drying at 60 ℃ to obtain the amino clay. Can be applied to the photoelectric fields of biochemical sensing, photocatalysis, cell imaging, living body imaging, magnetic resonance imaging, biomedicine, anti-counterfeiting, LED and the like.
Example 17
Dissolving 0.5g of manganese chloride and 0.3g of gadolinium chloride in 20mL of ethanol, dropwise adding 1.5mL of 3- [2- (2-aminoethylamino) ethylamino-triethoxysilane, stirring for 1h, then adding 20mg of rose bengal, stirring for 0.5h, transferring into a reaction kettle, keeping at 180 ℃ for 4h, cooling to room temperature, carrying out suction filtration, washing with ethanol for several times, and drying at 60 ℃ to obtain the amino clay. Can be applied to the photoelectric fields of biochemical sensing, photocatalysis, cell imaging, living body imaging, magnetic resonance imaging, biomedicine, anti-counterfeiting, LED and the like.
Example 18
Dissolving 0.4g of copper chloride and 0.3g of gadolinium chloride in 20mL of ethanol, dropwise adding 1.5mL of 3- [2- (2-aminoethylamino) ethylamino-triethoxysilane, stirring for 1h, then adding 20mg of rose bengal, stirring for 0.5h, transferring into a reaction kettle, keeping at 180 ℃ for 4h, cooling to room temperature, carrying out suction filtration, washing with ethanol for several times, and drying at 60 ℃ to obtain the amino clay. Can be applied to the photoelectric fields of biochemical sensing, photocatalysis, cell imaging, living body imaging, magnetic resonance imaging, biomedicine, anti-counterfeiting, LED and the like.
Example 19
Dissolving 0.4g of magnesium chloride and 0.3g of gadolinium chloride in 20mL of ethanol, dropwise adding 1.5mL of 3- (2-aminoethylamino) propyltrimethoxysilane, stirring for 1h, then adding 20mg of rose bengal, stirring for 0.5h, transferring into a reaction kettle, keeping at 180 ℃ for 4h, cooling to room temperature, carrying out suction filtration, washing with ethanol for several times, and drying at 60 ℃ to obtain the amino clay. Can be applied to the photoelectric fields of biochemical sensing, photocatalysis, cell imaging, living body imaging, magnetic resonance imaging, biomedicine, anti-counterfeiting, LED and the like.
Example 20
Dissolving 0.4g of magnesium chloride and 0.5g of manganese chloride in 20mL of ethanol, dropwise adding 1.5mL of 3- (2-aminoethylamino) propyltrimethoxysilane, stirring for 1h, then adding 20mg of rose bengal, stirring for 0.5h, transferring into a reaction kettle, keeping the temperature at 180 ℃ for 4h, cooling to room temperature, carrying out suction filtration, washing with ethanol for several times, and drying at 60 ℃ to obtain the amino clay. Can be applied to the photoelectric fields of biochemical sensing, photocatalysis, cell imaging, living body imaging, magnetic resonance imaging, biomedicine, anti-counterfeiting, LED and the like.
The above description is only a preferred embodiment of the present invention, and should not be taken as limiting the invention in any way, and any person skilled in the art can make any simple modification, equivalent replacement, and improvement on the above embodiment without departing from the technical spirit of the present invention, and still fall within the protection scope of the technical solution of the present invention.
Claims (9)
1. A preparation method of fluorescent amino clay is characterized by comprising the following steps: the method comprises the following steps:
(1) weighing a certain amount of metal salt and dissolving in a certain amount of ethanol;
(2) dissolving a certain amount of aminosilane into the solution obtained in the step (1), and stirring for 1-48 h;
(3) adding a certain amount of small molecular compounds or polymers into the solution obtained in the step (2) under the condition of stirring, and stirring for 0.5-12 h; refluxing for 1-12h at 30-100 ℃, or transferring into a polytetrafluoroethylene lined reaction kettle, and reacting for 1-12h at 110-200 ℃ to obtain a fluorescent amino clay product;
(4) centrifuging and washing to obtain the precipitate, and drying to obtain the fluorescent amino clay solid powder.
2. The method for preparing fluorescent amino clay according to claim 1, wherein: in the step (1), the metal salt is selected from one or more of nitrate, chloride, sulfate, acetate or perchlorate.
3. The method for preparing fluorescent amino clay according to claim 2, wherein: wherein the metal is selected from one or more of Mg, Al, Zn, Fe, Co, Ni, Cu, Ag, Cd, Cs, Ba, Bi, Pb, Sn, Al, In, Pd, Pt, Au, Mn, Cr, Mo, Nb, Ru, Rh, Ir, Ce, Eu, Tb and Tm.
4. The method for preparing fluorescent amino clay according to claim 1, wherein: in the step (1), the mass/volume ratio of the metal salt to the ethanol is (0.01-0.1): 1 g/mL.
5. The method for preparing fluorescent amino clay according to claim 1, wherein: in the step (2), the mass/volume ratio of the metal salt to the aminosilane is (0.5-2.5): 1 g/mL.
6. The method for preparing fluorescent amino clay according to claim 1, wherein: the aminosilane is selected from one or more of 3-aminopropyltrimethoxysilane, 3-aminopropyltriethoxysilane, 3- (2-aminoethylamino) propyltrimethoxysilane, 3- (2-aminoethylamino) propyltriethoxysilane, 3- [2- (2-aminoethylamino) ethylamino-trimethoxysilane and 3- [2- (2-aminoethylamino) ethylamino-triethoxysilane.
7. The method for preparing fluorescent amino clay according to claim 1, wherein: the fluorescent amino clay is obtained under the condition of a small molecular compound or a polymer; the micromolecular compound or polymer is selected from one or more of ascorbic acid, sodium ascorbate, citric acid, sodium citrate, glucose, boric acid, hydrazine, aniline, phenol, phenylenediamine, benzenediol, aminophenol, dopamine, rose bengal, rhodamine B, rhodamine 6G, polyalkyl pyrrolidone, oligomeric dopamine, polyaniline and the like; wherein the phenylenediamine comprises o-phenylenediamine, m-phenylenediamine and p-phenylenediamine; the diphenols include catechol, resorcinol, and hydroquinone; aminophenols include o-aminophenol, m-aminophenol, p-aminophenol; the ratio of the small molecular compound or the polymer to the aminosilane is 0.5-25 g/L.
8. The method for preparing fluorescent amino clay according to claim 1, wherein: in the step (3), the stirring is carried out for 0.5 to 12 hours; refluxing for 1-12h at 30-100 ℃, or transferring to a polytetrafluoroethylene lined reaction kettle, and then carrying out hydrothermal reaction at 110-200 ℃ for 1-12 h.
9. The method for preparing fluorescent amino clay according to claim 1, wherein: and dissolving the obtained fluorescent amino clay solid powder in secondary deionized water to obtain a fluorescent amino clay aqueous solution, wherein fluorescence can be observed under ultraviolet light.
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