CN108619115B - Multifunctional hollow mesoporous SiO2Process for preparing nano composite material - Google Patents
Multifunctional hollow mesoporous SiO2Process for preparing nano composite material Download PDFInfo
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- 239000000463 material Substances 0.000 title claims abstract description 20
- 239000002114 nanocomposite Substances 0.000 title claims abstract description 18
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims abstract description 49
- 239000000377 silicon dioxide Substances 0.000 claims abstract description 41
- 229910052681 coesite Inorganic materials 0.000 claims abstract description 35
- 229910052906 cristobalite Inorganic materials 0.000 claims abstract description 35
- 229910052682 stishovite Inorganic materials 0.000 claims abstract description 35
- 229910052905 tridymite Inorganic materials 0.000 claims abstract description 35
- 238000000034 method Methods 0.000 claims abstract description 15
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 7
- 229910052799 carbon Inorganic materials 0.000 claims abstract description 7
- 239000011248 coating agent Substances 0.000 claims abstract description 7
- 238000000576 coating method Methods 0.000 claims abstract description 7
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- VQCBHWLJZDBHOS-UHFFFAOYSA-N erbium(III) oxide Inorganic materials O=[Er]O[Er]=O VQCBHWLJZDBHOS-UHFFFAOYSA-N 0.000 claims abstract description 5
- FIXNOXLJNSSSLJ-UHFFFAOYSA-N ytterbium(III) oxide Inorganic materials O=[Yb]O[Yb]=O FIXNOXLJNSSSLJ-UHFFFAOYSA-N 0.000 claims abstract description 5
- 238000003980 solgel method Methods 0.000 claims abstract description 4
- 238000003786 synthesis reaction Methods 0.000 claims abstract description 4
- 230000002194 synthesizing effect Effects 0.000 claims abstract description 4
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 33
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 24
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- 238000002360 preparation method Methods 0.000 claims description 8
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- LZZYPRNAOMGNLH-UHFFFAOYSA-M Cetrimonium bromide Chemical compound [Br-].CCCCCCCCCCCCCCCC[N+](C)(C)C LZZYPRNAOMGNLH-UHFFFAOYSA-M 0.000 claims description 5
- 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 4
- BOTDANWDWHJENH-UHFFFAOYSA-N Tetraethyl orthosilicate Chemical compound CCO[Si](OCC)(OCC)OCC BOTDANWDWHJENH-UHFFFAOYSA-N 0.000 claims description 4
- XSQUKJJJFZCRTK-UHFFFAOYSA-N Urea Chemical compound NC(N)=O XSQUKJJJFZCRTK-UHFFFAOYSA-N 0.000 claims description 4
- 239000004202 carbamide Substances 0.000 claims description 4
- 239000008103 glucose Substances 0.000 claims description 4
- 239000000376 reactant Substances 0.000 claims description 4
- 238000005303 weighing Methods 0.000 claims description 4
- 230000015572 biosynthetic process Effects 0.000 claims description 3
- 238000001354 calcination Methods 0.000 claims description 3
- -1 polytetrafluoroethylene Polymers 0.000 claims description 3
- 229920001343 polytetrafluoroethylene Polymers 0.000 claims description 3
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- 239000007795 chemical reaction product Substances 0.000 claims 1
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- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 description 2
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- 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 description 1
- 230000000975 bioactive effect Effects 0.000 description 1
- 239000000969 carrier Substances 0.000 description 1
- 239000012876 carrier material Substances 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 239000011247 coating layer Substances 0.000 description 1
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- 210000003734 kidney Anatomy 0.000 description 1
- 239000002502 liposome Substances 0.000 description 1
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- 238000004736 wide-angle X-ray diffraction Methods 0.000 description 1
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- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K9/00—Medicinal preparations characterised by special physical form
- A61K9/48—Preparations in capsules, e.g. of gelatin, of chocolate
- A61K9/50—Microcapsules having a gas, liquid or semi-solid filling; Solid microparticles or pellets surrounded by a distinct coating layer, e.g. coated microspheres, coated drug crystals
- A61K9/51—Nanocapsules; Nanoparticles
- A61K9/5107—Excipients; Inactive ingredients
- A61K9/5115—Inorganic compounds
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- A—HUMAN NECESSITIES
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- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K49/00—Preparations for testing in vivo
- A61K49/001—Preparation for luminescence or biological staining
- A61K49/0013—Luminescence
- A61K49/0017—Fluorescence in vivo
- A61K49/0019—Fluorescence in vivo characterised by the fluorescent group, e.g. oligomeric, polymeric or dendritic molecules
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- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K49/00—Preparations for testing in vivo
- A61K49/001—Preparation for luminescence or biological staining
- A61K49/0063—Preparation for luminescence or biological staining characterised by a special physical or galenical form, e.g. emulsions, microspheres
- A61K49/0069—Preparation for luminescence or biological staining characterised by a special physical or galenical form, e.g. emulsions, microspheres the agent being in a particular physical galenical form
- A61K49/0089—Particulate, powder, adsorbate, bead, sphere
- A61K49/0091—Microparticle, microcapsule, microbubble, microsphere, microbead, i.e. having a size or diameter higher or equal to 1 micrometer
- A61K49/0093—Nanoparticle, nanocapsule, nanobubble, nanosphere, nanobead, i.e. having a size or diameter smaller than 1 micrometer, e.g. polymeric nanoparticle
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Abstract
The invention discloses a multifunctional hollow mesoporous SiO2Process for preparing nanocomposites with Y2O3、Yb2O3And Er2O3Synthesis of Y (OH) CO by coprecipitation method for raw material3Yb, Er, then hydrothermally in Y (OH) CO3Coating a carbon shell on the surface of a Yb and Er core structure, and coating Y (OH) CO by a sol-gel method3Yb, Er @ C surface-coated mesoporousmSiO2Finally synthesizing Y with hollow mesoporous structure2O3:Yb,Er@mSiO2(ii) a The method can be used for preparing the photoluminescent nanocomposite material with the hollow mesoporous structure and larger aperture and specific surface area.
Description
Technical Field
The invention relates to the technical field of nano materials, in particular to a method for preparing Y2O3:Yb,Er@mSiO2A method of making a nanocomposite.
Background
Controlling drug sustained release is one of the most important and attractive areas of research, and the carrier is most critical for controlling the drug storage capacity and its release rate. This research has been greatly enhanced in the last decade, and a large number of organic systems have been investigated as drug carriers in drug delivery systems, such as micelles, liposomes and polymers. However, these carriers have various limitations such as poor thermal and chemical stability and rapid decomposition in the immune system. CompareIn contrast, mesoporous silica materials have good biocompatibility, stable selectivity and no toxicity. In addition, it is degraded in the body to Si (OH)4，Si(OH)4Can be discharged out of the body through the kidney, so the material can be widely used as an adjuvant in pharmaceutical technology.
The mesoporous material has the characteristics of large specific surface area, ordered mesoporous structure, adjustable pore diameter and pore volume, and modifiable surface groups, which are attractive characteristics. These features facilitate the insertion of bioactive molecules into the pore structure and also provide a pathway for the subsequent diffusion of these molecules. Moreover, the hollow mesoporous silica spheres have high storage capacity due to the structure thereof; in addition, the hollow sphere with the mesoporous layer exhibits great advantages in large-scale diffusion and transportation compared to the conventional solid layer hollow sphere. Therefore, the hollow mesoporous silica attracts more and more attention in the aspect of drug slow release.
SUMMERY OF THE UTILITY MODEL
The invention aims to provide a hollow-structure multifunctional mesoporous Y2O3:Yb,Er@mSiO2 (wherein @ represents a coating layer,mrepresenting mesopores) nanocomposite.
The technical scheme adopted by the invention for solving the technical problems is as follows: multifunctional hollow mesoporous SiO2Preparation method of nano composite material, core-shell structure and material composition thereof are Y2O3:Yb,Er@mSiO2The steps are as follows
(1) Coprecipitation method for synthesizing Y (OH) CO3:Yb,Er：
Will Y2O3、Yb2O3And Er2O3Respectively dissolved in HNO3To obtain Y (NO)3)3、Yb(NO3)3And Er (NO)3)3Adding the solution into distilled water according to a certain proportion, adding urea, continuously stirring, transferring the mixture into a flask, reacting in a water bath at 90 ℃ for 3 h, and finally centrifuging, washing and drying to obtain Y (OH) CO3:Yb,Er；
(2) By hydrothermal method on Y (OH) CO3Coating a carbon shell on the surface of a Yb and Er core structure:
by reacting Y (OH) CO3Yb and Er are dispersed in distilled water and alcohol, glucose is added, and Y (OH) CO is obtained by centrifugal washing and drying after hydrothermal reaction3:Yb,Er@C；
(3) By sol-gel method on Y (OH) CO3Yb, Er @ C surface-coated mesoporousmSiO2：
Mixing Yb (OH) CO3Yb, Er @ C are dispersed in ethanol and distilled water, CTAB and ammonia water are added, tetraethoxysilane is slowly dripped, the mixture is stirred for 6 hours at room temperature, and Y (OH) CO is obtained by centrifugal washing and drying3:Yb,Er@C@mSiO2；
(4) Synthesis of Yb with hollow mesoporous structure2O3:Yb,Er@mSiO2：
The Y (OH) CO obtained above is reacted3:Yb,Er@C@mSiO2Calcining in a muffle furnace at 800 ℃ for 3 h, removing the carbon shell to obtain Y with a hollow structure2O3:Yb,Er@mSiO2。
The multifunctional hollow mesoporous SiO2A process for producing a nanocomposite, wherein in the step (1), Y is used in a molar ratio of 0.78:0.20:0.022O3,Yb2O3And Er2O3Dissolved in 2mol L-1HNO of (2)3。
The multifunctional hollow mesoporous SiO2Process for the preparation of a nanocomposite, wherein in step (1) Y (NO)3)3、Yb(NO3)3And Er (NO)3)3The solution was added to 200 ml of distilled water, followed by 12.1 g of urea and continued stirring, and after 2 h was transferred to the flask.
The multifunctional hollow mesoporous SiO2The preparation method of the nano composite material comprises the steps of centrifuging, washing and drying the solution in the step (1) at the speed of 4000 r/min, washing the solution with water and ethanol for three times respectively, and drying the solution in an oven at the temperature of 60 ℃ for 24 hours.
The multifunctional hollow mesoporous SiO2Nano composite materialThe preparation method of the material comprises the step (2) of accurately weighing 0.2 g Y (OH) CO3Yb and Er were dispersed in 20 mL of distilled water and 13 mL of ethanol, and 3.2 g of glucose was added, followed by continuous vigorous stirring for 0.5 h.
The multifunctional hollow mesoporous SiO2The hydrothermal reaction in the step (2) is to transfer the reactants into a 50 mL polytetrafluoroethylene reaction kettle and then react for 12 h at 180 ℃.
The multifunctional hollow mesoporous SiO2The preparation method of the nano composite material comprises the steps of centrifuging, washing and drying in the step (2) at the speed of 4000 r/min, washing with water and ethanol for three times respectively, and drying in an oven at the temperature of 60 ℃ for 24 hours.
The multifunctional hollow mesoporous SiO2The preparation method of the nano composite material comprises the step (3) of accurately weighing 0.4 g Y (OH) CO3Yb, Er @ C was dispersed in 100 mL of ethanol and 150 mL of distilled water, followed by addition of 0.5 g of CTAB and 1 mL of 1.0 mol L-1Then 200. mu.L of ethyl orthosilicate was slowly added dropwise.
The multifunctional hollow mesoporous SiO2The preparation method of the nano composite material comprises the steps of centrifuging, washing and drying in the step (3) at the speed of 4000 r/min, washing with water and ethanol for three times respectively, and drying in an oven at the temperature of 60 ℃ for 24 hours.
The invention has the beneficial effects that:
the invention adopts a coprecipitation method, a hydrothermal method and a sol-gel method to prepare Y with a hollow mesoporous structure with uniform particle size and good dispersibility2O3:Yb,Er@mSiO2A nanocomposite; CTAB is adopted as a surfactant to form an ordered mesoporous silicon dioxide layer, so that a large surface area is provided for introducing a large amount of functional molecular groups, and a large aperture is provided for absorbing and encapsulating biomolecules; by changing the quality of the reactants and the crystal growth time, the hollow ordered mesoporous structure nano composite material with different sizes can be synthesized.
The prepared nano composite material has the following characteristics:
the material has a cavity structure inside, and can be used for storing a large number of drug molecules; the surface of the material is provided with a mesoporous silica layer, so that an internal cavity of the material can be communicated with the external environment through a mesoporous pore canal, the exchange of internal and external substances can be realized, and in addition, the mesoporous silica pore canal can also store a large amount of drug molecules, so that the mesoporous silica material is a good drug sustained-release carrier material; the composite material emits strong up-conversion fluorescence under 980nm exciting light, and can be used for detecting the slow release process and the curative effect of the drug; toxic products are not generated in the experimental process, the environmental protection is realized, the experimental raw materials are low in price, the experimental process is simple and easy to implement, and the production and popularization of the experimental method are easy.
Drawings
FIG. 1 shows Y (OH) CO3:Yb,Er@C@mSiO2And Y2O3:Yb,Er@mSiO2@mSiO2X-ray diffraction pattern of (a);
FIG. 2 is Y2O3:Yb,Er@mSiO2Transmission electron microscope photograph of (1);
FIG. 3 is Y2O3Yb, Er and Y2O3:Yb,Er@mSiO2The upconversion emission spectrum of the sample.
Detailed Description
The technical solution and effects of the present invention will be further described with reference to the following examples. However, the specific methods, formulations and descriptions used are not intended to be limiting.
The implementation process comprises the following steps:
(1) coprecipitation method for synthesizing Y (OH) CO3:Yb,Er。
Y in a molar ratio of 0.78:0.20:0.022O3,Yb2O3And Er2O3Dissolved in 2mol L-1HNO of (2)3In (1). Obtained Y (NO)3)3、Yb(NO3)3And Er (NO)3)3The solution was added to 200 ml of distilled water. 12.1 g of urea are subsequently added and stirring is continued. After 2 h, the mixture was transferred to a flask and reacted in a water bath at 90 ℃ for 3 h. Finally, the reacted solution is centrifuged at 4000 r/min, washed with water and ethanol three times respectively, and dried in an oven at 60 ℃ for 24 hoursTo obtain Y (OH) CO3:Yb,Er。
(2) By hydrothermal method on Y (OH) CO3The surface of Yb and Er is coated with a carbon shell.
Accurately weigh 0.2 g of above Y (OH) CO3Yb and Er are dispersed in 20 mL of distilled water and 13 mL of ethanol, a certain amount of glucose is added, the mixture is continuously stirred vigorously for 0.5 h, and then the reactants are transferred into a 50 mL polytetrafluoroethylene reaction kettle and reacted for 12 h at 180 ℃. Finally, centrifuging at 4000 r/min, washing with water and ethanol for three times respectively, and oven-drying at 60 deg.C for 24 hr to obtain Y (OH) CO3:Yb,Er@C。
(3) Synthesis of Y (OH) CO3:Yb,Er@C@SiO2。
Accurately weighing 0.4 g Y (OH) CO3Yb, Er @ C was dispersed in 100 mL of ethanol and 150 mL of distilled water. 0.5 g CTAB and 1 mL of 1.0 mol L‒1200 mu.L of ethyl orthosilicate is slowly dropped into the ammonia water, and the mixture is stirred for 6 hours at room temperature. Finally, centrifuging at 4000 r/min, washing with water and ethanol for three times respectively, and oven-drying at 60 deg.C for 24 hr to obtain Y (OH) CO3:Yb,Er@C@mSiO2。
(4) Synthetic hollow structure Y2O3:Yb,Er@mSiO2。
Y (OH) CO obtained by the above reaction3:Yb,Er@C@mSiO2Calcining in a muffle furnace at 800 ℃ for 3 h, burning off the carbon shell to obtain Y with a hollow structure2O3:Yb,Er@mSiO2。
FIG. 1 is a wide angle X-ray diffraction pattern of a sample, JCPDS 25-1011 being a standard card; from the figure, it can be confirmed that the phases before firing are all amorphous phases. And for Y2O3:Yb,Er@mSiO2We can see four sharp peaks at 2 θ =29.2 °, 33.4 °, 48.5 ° and 57 °, being Y2O3Characteristic peak of (2), and Y2O3The relative intensity position and diffraction position of the standard X-ray diffraction card (JCPDS No.25-1011) are consistent, so that the powder calcined at 800 ℃ does not generate impurity phase, and can be classified as amorphous SiO at 2 theta =22 DEG2Characteristic peak of (JCPDS 29-0085). ByThis can explain SiO2The coating to the powder surface has been successful, and four sharp peaks of 2 theta =29.2 °, 33.4 °, 48.5 ° and 57 ° indicate SiO2The coating of (2) has no influence on the crystal structure of the powder.
As shown in FIG. 2, the material was uniform in size and no agglomeration occurred. We can observe that there is a layer of darker shell around the sphere, which is an obvious hollow shell-core structure.
FIG. 3 is Y2O3Yb, Er and Y2O3:Yb,Er@mSiO2The upconversion emission spectrum of the sample. Under excitation of a 980nm laser, the sample showed strong green and red light emission. From FIG. A, it can be seen thatH-Y2O3Yb, Er samples present three different Er3+Characteristic emission peaks, generated in Er at green emission between 520nm and 538nm and between 540nm and 560nm3+Is/are as follows2H11/2To4I15/2And4S3/2to4I15/2The red light emission between 640nm and 680nm is due to4F9/2To4I15/2And (4) transition. I.e. Er under excitation of 980nm3+Is excited to the ground state electron by absorbing a photon4I11/2Energy level, further excited upon absorption of a second photon4F7/2Energy level in the visible region, Er3+Non-radiative relaxation by rapid phonon decay processes to2H11/2And4S3/2energy level, generation2H11/2To4I15/2And4S3/2to4I115/2Green emission, electrons can be further relaxed and arranged to4F9/2Energy level, generation4F9/2To4I15/2Red light emission of (a). FIG. B isH-Y2O3:Yb,Er@mSiO2The up-conversion emission spectrum of the sample, from which we can see that there is no change in the pattern except for the significant decrease in the intensity of the emission peak, which is the coating SiO2The result is.
The above-described embodiments are merely illustrative of the principles and effects of the present invention, and some embodiments may be applied, and it will be apparent to those skilled in the art that various changes and modifications may be made without departing from the inventive concept of the present invention, and these embodiments are within the scope of the present invention.
Claims (1)
1. Multifunctional hollow mesoporous SiO2The preparation method of the nano composite material is characterized by comprising the following steps: comprises the steps of
(1) Coprecipitation method for synthesizing Y (OH) CO3:Yb,Er：
Mixing Y with the molar ratio of 0.78:0.20:0.022O3,Yb2O3And Er2O3The dissolution concentration is 2 mol.L-1HNO of (2)3To obtain Y (NO)3)3、Yb(NO3)3And Er (NO)3)3Adding the solution into 200 ml of distilled water according to a certain proportion, then adding 12.1 g of urea and continuously stirring, transferring into a flask after 2 h, carrying out water bath reaction at 90 ℃ for 3 h, and finally, centrifuging, washing and drying to obtain Y (OH) CO3Yb, Er; the centrifugal washing and drying is that the solution is centrifuged at the speed of 4000 r/min, and is washed by water and ethanol for three times respectively, and is dried in an oven at the temperature of 60 ℃ for 24 hours;
(2) by hydrothermal method on Y (OH) CO3Coating a carbon shell on the surface of a Yb and Er core structure:
accurately weigh 0.2 g Y (OH) CO3Yb and Er are dispersed in 20 mL of distilled water and 13 mL of ethanol, then 3.2 g of glucose is added, then the mixture is continuously and vigorously stirred for 0.5 h, the reactant is transferred into a 50 mL of polytetrafluoroethylene reaction kettle, then the reaction is carried out for 12 h at 180 ℃, then the reaction is centrifuged at the speed of 4000 r/min and is respectively washed with water and ethanol for three times, and then the reaction product is dried in an oven at 60 ℃ for 24 h to obtain Y (OH) CO3:Yb,Er@C；
(3) By sol-gel method on Y (OH) CO3Yb, Er @ C surface-coated mesoporousmSiO2：
Accurately weighing 0.4 g Y (OH) CO3Yb, Er @ C was dispersed in 100 mL of ethanol and 150 mL of distilled water, followed by addition of 0.5 g of CTAB and 1 mL of 1.0 mol · L-1Slowly dropwise adding 200 mu L of tetraethoxysilane, stirring at room temperature for 6 h, centrifuging at the speed of 4000 r/min, washing with water and ethanol for three times respectively, and drying in an oven at 60 ℃ for 24 h to obtain Y (OH) CO3:Yb,Er@C@mSiO2；
(4) Synthesis of Yb with hollow mesoporous structure2O3:Yb,Er@mSiO2：
The Y (OH) CO obtained above is reacted3:Yb,Er@C@mSiO2Calcining in a muffle furnace at 800 ℃ for 3 h, removing the carbon shell to obtain Y with a hollow structure2O3:Yb,Er@mSiO2。
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