CN110182768B - Method for forming CdSe nanorod by self-assembly by taking grafted block polymer as template - Google Patents
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- 229920000642 polymer Polymers 0.000 title claims abstract description 41
- 239000002073 nanorod Substances 0.000 title claims abstract description 25
- UHYPYGJEEGLRJD-UHFFFAOYSA-N cadmium(2+);selenium(2-) Chemical compound [Se-2].[Cd+2] UHYPYGJEEGLRJD-UHFFFAOYSA-N 0.000 title claims abstract description 23
- 238000000034 method Methods 0.000 title claims abstract description 21
- 238000001338 self-assembly Methods 0.000 title claims abstract description 11
- 238000010560 atom transfer radical polymerization reaction Methods 0.000 claims abstract description 16
- 230000002194 synthesizing effect Effects 0.000 claims abstract description 3
- 239000002243 precursor Substances 0.000 claims description 16
- BUGBHKTXTAQXES-UHFFFAOYSA-N Selenium Chemical compound [Se] BUGBHKTXTAQXES-UHFFFAOYSA-N 0.000 claims description 11
- YXFVVABEGXRONW-UHFFFAOYSA-N Toluene Chemical compound CC1=CC=CC=C1 YXFVVABEGXRONW-UHFFFAOYSA-N 0.000 claims description 9
- 239000000178 monomer Substances 0.000 claims description 9
- 238000006243 chemical reaction Methods 0.000 claims description 7
- 230000000977 initiatory effect Effects 0.000 claims description 7
- ISXSCDLOGDJUNJ-UHFFFAOYSA-N tert-butyl prop-2-enoate Chemical compound CC(C)(C)OC(=O)C=C ISXSCDLOGDJUNJ-UHFFFAOYSA-N 0.000 claims description 7
- PPBRXRYQALVLMV-UHFFFAOYSA-N Styrene Chemical compound C=CC1=CC=CC=C1 PPBRXRYQALVLMV-UHFFFAOYSA-N 0.000 claims description 6
- DTQVDTLACAAQTR-UHFFFAOYSA-N Trifluoroacetic acid Chemical compound OC(=O)C(F)(F)F DTQVDTLACAAQTR-UHFFFAOYSA-N 0.000 claims description 6
- 229910052793 cadmium Inorganic materials 0.000 claims description 6
- BDOSMKKIYDKNTQ-UHFFFAOYSA-N cadmium atom Chemical compound [Cd] BDOSMKKIYDKNTQ-UHFFFAOYSA-N 0.000 claims description 6
- 239000011669 selenium Substances 0.000 claims description 6
- 229910052711 selenium Inorganic materials 0.000 claims description 6
- RMZAYIKUYWXQPB-UHFFFAOYSA-N trioctylphosphane Chemical compound CCCCCCCCP(CCCCCCCC)CCCCCCCC RMZAYIKUYWXQPB-UHFFFAOYSA-N 0.000 claims description 5
- 229920002818 (Hydroxyethyl)methacrylate Polymers 0.000 claims description 4
- 238000005119 centrifugation Methods 0.000 claims description 4
- 239000003153 chemical reaction reagent Substances 0.000 claims description 4
- 229920002338 polyhydroxyethylmethacrylate Polymers 0.000 claims description 4
- 238000010992 reflux Methods 0.000 claims description 4
- 238000003756 stirring Methods 0.000 claims description 4
- 239000006228 supernatant Substances 0.000 claims description 4
- YOCIJWAHRAJQFT-UHFFFAOYSA-N 2-bromo-2-methylpropanoyl bromide Chemical compound CC(C)(Br)C(Br)=O YOCIJWAHRAJQFT-UHFFFAOYSA-N 0.000 claims description 3
- WOBHKFSMXKNTIM-UHFFFAOYSA-N Hydroxyethyl methacrylate Chemical compound CC(=C)C(=O)OCCO WOBHKFSMXKNTIM-UHFFFAOYSA-N 0.000 claims description 3
- ZMXDDKWLCZADIW-UHFFFAOYSA-N N,N-Dimethylformamide Chemical compound CN(C)C=O ZMXDDKWLCZADIW-UHFFFAOYSA-N 0.000 claims description 3
- XEHUIDSUOAGHBW-UHFFFAOYSA-N chromium;pentane-2,4-dione Chemical group [Cr].CC(=O)CC(C)=O.CC(=O)CC(C)=O.CC(=O)CC(C)=O XEHUIDSUOAGHBW-UHFFFAOYSA-N 0.000 claims description 3
- 238000010438 heat treatment Methods 0.000 claims description 3
- CUJRVFIICFDLGR-UHFFFAOYSA-N acetylacetonate Chemical compound CC(=O)[CH-]C(C)=O CUJRVFIICFDLGR-UHFFFAOYSA-N 0.000 claims description 2
- 230000003301 hydrolyzing effect Effects 0.000 claims description 2
- 239000003999 initiator Substances 0.000 claims description 2
- 239000000047 product Substances 0.000 claims description 2
- 230000035484 reaction time Effects 0.000 claims description 2
- 238000000926 separation method Methods 0.000 claims 2
- 230000031709 bromination Effects 0.000 claims 1
- 238000005893 bromination reaction Methods 0.000 claims 1
- 239000006185 dispersion Substances 0.000 claims 1
- 238000001556 precipitation Methods 0.000 claims 1
- 239000002086 nanomaterial Substances 0.000 abstract description 9
- 238000002360 preparation method Methods 0.000 abstract description 4
- 239000002105 nanoparticle Substances 0.000 abstract description 2
- 230000001699 photocatalysis Effects 0.000 abstract 1
- 229920002125 Sokalan® Polymers 0.000 description 6
- 239000004793 Polystyrene Substances 0.000 description 4
- 238000005886 esterification reaction Methods 0.000 description 3
- 239000002904 solvent Substances 0.000 description 3
- 239000002253 acid Substances 0.000 description 2
- 230000032050 esterification Effects 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 239000000693 micelle Substances 0.000 description 2
- 238000012705 nitroxide-mediated radical polymerization Methods 0.000 description 2
- 229920002223 polystyrene Polymers 0.000 description 2
- 239000002244 precipitate Substances 0.000 description 2
- 238000010526 radical polymerization reaction Methods 0.000 description 2
- 238000012712 reversible addition−fragmentation chain-transfer polymerization Methods 0.000 description 2
- 230000002441 reversible effect Effects 0.000 description 2
- 241001264766 Callistemon Species 0.000 description 1
- 238000003917 TEM image Methods 0.000 description 1
- 238000004220 aggregation Methods 0.000 description 1
- 230000002776 aggregation Effects 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 229920001400 block copolymer Polymers 0.000 description 1
- 238000006555 catalytic reaction Methods 0.000 description 1
- 230000000536 complexating effect Effects 0.000 description 1
- 239000002131 composite material Substances 0.000 description 1
- 238000004132 cross linking Methods 0.000 description 1
- 230000009849 deactivation Effects 0.000 description 1
- 230000001419 dependent effect Effects 0.000 description 1
- 238000009826 distribution Methods 0.000 description 1
- 238000012377 drug delivery Methods 0.000 description 1
- 229920001971 elastomer Polymers 0.000 description 1
- 239000000806 elastomer Substances 0.000 description 1
- 230000002708 enhancing effect Effects 0.000 description 1
- 229920000578 graft copolymer Polymers 0.000 description 1
- 238000003306 harvesting Methods 0.000 description 1
- 230000003100 immobilizing effect Effects 0.000 description 1
- 238000011068 loading method Methods 0.000 description 1
- 239000000314 lubricant Substances 0.000 description 1
- 229920002521 macromolecule Polymers 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 239000002114 nanocomposite Substances 0.000 description 1
- 239000002071 nanotube Substances 0.000 description 1
- 239000002070 nanowire Substances 0.000 description 1
- 230000003287 optical effect Effects 0.000 description 1
- 230000035515 penetration Effects 0.000 description 1
- 239000011148 porous material Substances 0.000 description 1
- 238000003860 storage Methods 0.000 description 1
- 125000003011 styrenyl group Chemical group [H]\C(*)=C(/[H])C1=C([H])C([H])=C([H])C([H])=C1[H] 0.000 description 1
- 238000001308 synthesis method Methods 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
- 230000009897 systematic effect Effects 0.000 description 1
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y40/00—Manufacture or treatment of nanostructures
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B19/00—Selenium; Tellurium; Compounds thereof
- C01B19/007—Tellurides or selenides of metals
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F120/00—Homopolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and only one being terminated by only one carboxyl radical or a salt, anhydride, ester, amide, imide or nitrile thereof
- C08F120/02—Monocarboxylic acids having less than ten carbon atoms; Derivatives thereof
- C08F120/10—Esters
- C08F120/20—Esters of polyhydric alcohols or polyhydric phenols, e.g. 2-hydroxyethyl (meth)acrylate or glycerol mono-(meth)acrylate
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F265/00—Macromolecular compounds obtained by polymerising monomers on to polymers of unsaturated monocarboxylic acids or derivatives thereof as defined in group C08F20/00
- C08F265/04—Macromolecular compounds obtained by polymerising monomers on to polymers of unsaturated monocarboxylic acids or derivatives thereof as defined in group C08F20/00 on to polymers of esters
- C08F265/06—Polymerisation of acrylate or methacrylate esters on to polymers thereof
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F285/00—Macromolecular compounds obtained by polymerising monomers on to preformed graft polymers
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F8/00—Chemical modification by after-treatment
- C08F8/18—Introducing halogen atoms or halogen-containing groups
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/10—Particle morphology extending in one dimension, e.g. needle-like
- C01P2004/16—Nanowires or nanorods, i.e. solid nanofibres with two nearly equal dimensions between 1-100 nanometer
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- Chemical & Material Sciences (AREA)
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- Chemical Kinetics & Catalysis (AREA)
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- Polymers & Plastics (AREA)
- Engineering & Computer Science (AREA)
- Nanotechnology (AREA)
- Physics & Mathematics (AREA)
- General Chemical & Material Sciences (AREA)
- Condensed Matter Physics & Semiconductors (AREA)
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- Graft Or Block Polymers (AREA)
Abstract
The invention discloses a method for forming a CdSe nanorod by self-assembly by taking a grafted block polymer as a template, relates to a method for synthesizing the grafted block polymer template and guiding and assembling the CdSe nanorod, and belongs to the technical field of preparation of nanostructures. Firstly, atom Transfer Radical Polymerization (ATRP) is utilized to obtain a graft block polymer PHEMA-g- [ PAA-b-PS ], and then nanoparticles are guided to carry out self-assembly on the graft block polymer to obtain the CdSe nanorod. The nano structure with proper size can be obtained by directly guiding the assembly through adjusting the molecular weight of the main chain and the side chain of the graft block polymer. Meanwhile, the synthesized CdSe nano material has excellent photocatalytic performance and good application prospect.
Description
Technical Field
The invention relates to a method for synthesizing a high molecular polymer template and guiding and assembling a nano structure, belonging to the technical field of nano structure preparation.
Background
Graft block polymers are macromolecules containing a long polymer backbone with densely grafted polymer side chains. Due to their unique structure, graft block polymers exhibit distinct properties, and have many potential applications, including photonics, lubricants, stimuli-responsive materials, ultra-soft elastomers, porous materials, and drug delivery systems. The grafted block polymer can be synthesized by three strategies: "graft", "graft to", "graft from". The development of the procedures of Reversible Deactivation Radical Polymerization (RDRP) or Controlled Radical Polymerization (CRP), including Atom Transfer Radical (ATRP), reversible addition-fragmentation chain transfer polymerization (RAFT) and Nitroxide Mediated Polymerization (NMP) provides a variety of routes to the preparation of grafted block polymers with backbone and side chains of controlled composition and molecular weight.
Although monomolecular in form, the size of the grafted block polymer is similar to some self-assembled nano objects, such as polymer micelles. Due to the strong steric repulsion between the densely grafted side chains, the grafted block polymer adopts an extended cylindrical configuration if the length of the backbone is significantly longer than the length of the side chains. This allows molecular bottle brushes with block copolymer side chains to be used as single-molecule templates for the fabrication of one-dimensional (1D) nanostructures, such as nanorods, nanowires, and nanotubes. Although a structure similar to a micelle is provided by reversible self-assembly, the graft block polymer is not dissociated when the external environment is changed, providing a unique opportunity for complexing inorganic precursors. Thus, a composite material having an anisotropically aligned inorganic content can be selectively formed in the graft block, thereby providing a layered structure in the radial direction.
In this way, nanorods can be prepared using a graft block polymer template, where the boundaries of the nanocore reactor are defined by the graft inner block (core) and the graft outer block (shell), respectively. Due to their unique geometry and size dependent optical, electronic, magnetic, 1D nanostructures are useful for potential applications in the fields of nanoelectronics, sensors, catalysis, energy harvesting, storage and conversion. The synthesis of branched inorganic nanostructures is an important direction of research to generate hierarchical nanostructured networks with enhanced interconnectivity and nanoparticle penetration.
Disclosure of Invention
The invention provides a method for forming a CdSe nanorod by self-assembly by taking a grafted block polymer as a template.
The graft block polymer with poly (acrylic acid) -block-polystyrene (PAA-b-PS) side chain is synthesized by the method of 'grafting from' and is used as a template for self-assembly to form the CdSe nano rod. The structural characteristics of the template are also effectively transferred into the hybrid nano composite material, and the CdSe nano rod with regular shape and uniform size distribution can be controllably synthesized.
The invention provides a method for forming a CdSe nanorod by self-assembly by taking a grafted block polymer as a template
Preferably: the graft block polymer consists of a main chain and a side chain; wherein the main chain is obtained by Atom Transfer Radical Polymerization (ATRP) of a monomer, the main chain is an initiation site for forming ATRP on a side chain by an esterification method, the side chain comprises two block polymers A and B, and the two block polymers A and B are obtained by Atom Transfer Radical Polymerization (ATRP) of the monomer on the initiation site of the main chain.
Preferably: the monomer that synthesizes the backbone is hydroxyethyl methacrylate (HEMA).
Preferably: the polyhydroxyethyl methacrylate (PHEMA) main chain is arranged at a main chain side group point through an esterification reaction with a brominating reagent to form a plurality of initiation sites; and the brominating reagent is 2-bromoisobutyryl bromide.
Preferably: the monomer of the block polymer A synthesized by the side chain is tert-butyl acrylate (PtBA), and the monomer of the block polymer B is styrene (St).
Preferably: the block polymer a poly (tert-butyl acrylate) (PtBA) can be hydrolyzed by strong acid to poly (acrylic acid) (PAA); and the strong acid is trifluoroacetic acid.
Preferably: in the guided assembly method of the CdSe nanorod, the solvent is N-N-Dimethylformamide (DMF); the precursor of cadmium is chromium acetylacetonate (Cd (acac) 2 ) (ii) a The precursor solution of the selenium is a selenium powder solution of trioctylphosphine.
Preferably: the volume of the solvent is 10mL; the mass of the precursor of cadmium is 108mg; the mass of selenium powder in the selenium precursor solution is 28mg, and the volume of trioctylphosphine is 2mL.
Preferably: in the guided assembly method of the CdSe nanorod, the stirring time at normal temperature is 2 hours, the heating temperature is 180 ℃, and the reflux reaction time is 2 hours. Standing the reaction solution for 7d, and performing fractional centrifugation by centrifuging at 1000 rpm for 5 min to obtain supernatant, centrifuging at 5000 rpm for 5 min to obtain precipitate, and dispersing with toluene.
Compared with the prior art, the invention has the advantages that: the invention discloses a method for forming a CdSe nanorod by self-assembly by taking a grafted block polymer as a template. The graft-block polymer with poly (acrylic acid) -block-polystyrene (PAA-b-PS) side chains is synthesized by a method of "grafting from" and used as a template for self-assembly to form CdSe nanorods. The PS segments not only define the boundary of the PAACdSe nanorod core, but also act as a shell outside the CdSe nanorod, preventing cross-linking, aggregation and enhancing its processability. The synthetic strategy of "grafting from" allows systematic adjustment of the length and morphology of the grafted block polymer during the preparation of the backbone by ATRP. Compared with previous work, the use of poly (acrylic acid) (PAA) as a compartment for immobilizing precursors has better universality, ensuring the feasibility of loading templates with most inorganic precursors at ambient temperature. Secondly, the precise and unique coordination of the precursors with the PS shell compartments makes it possible to manufacture homogeneous nanomaterials.
Drawings
FIG. 1 is a Transmission Electron Microscopy (TEM) image of the CdSe nanorods incorporated in an example of the present invention.
Detailed Description
A method for forming CdSe nanorods by self-assembling with a grafted block polymer as a template comprises the following steps:
(1) A synthesis method of a graft block polymer PHEMA-g- [ PAA-b-PS ] comprises the steps of using a single-molecule initiator to polymerize (ATRP) atom transfer radical of a monomer (hydroxyethyl methacrylate) to obtain a polyhydroxyethyl methacrylate main chain, forming an ATRP initiation site at a side end of the main chain by an esterification method with a brominating reagent (2-bromoisobutyryl bromide), then sequentially carrying out ATRP on the initiation site at the side end of the main chain by using tert-butyl acrylate (tBA) and styrene (St) as monomers to form the graft block polymer, and finally hydrolyzing the tert-butyl acrylate of the side chain by using trifluoroacetic acid to obtain a product PHEMA-g- [ PAA-b-PS ].
(2) The guided assembly of the CdSe nanorod is carried out by adding 108mg of cadmium precursor (chromium acetylacetonate) into a three-neck round-bottom flask with magnetons, injecting a grafting block polymer template solution (dissolved in 10mL of N-N-dimethylformamide solvent) under inert atmosphere, stirring at normal temperature for 2h, heating at 180 ℃, injecting a selenium precursor solution (selenium powder of 28mg dissolved in 2mL of trioctylphosphine solution), and carrying out reflux reaction for 2h. And standing the reaction solution for 7d, centrifuging for 5 minutes at 1000 rpm, taking supernatant, centrifuging for 5 minutes at 5000 rpm, taking precipitate, and dispersing with toluene to obtain CdSe nanorods, wherein the CdSe nanorods are uniform in size and can reach 300nm, as shown in FIG. 1, thereby proving the feasibility of guided assembly of the polymer template in the invention.
Claims (1)
1. A method for forming a CdSe nanorod by self-assembly by taking a grafted block polymer as a template is characterized by comprising the following steps of: the method comprises the following steps:
(1) A method for synthesizing a graft block polymer PHEMA-g- [ PAA-b-PS ] comprises the steps of using a single-molecule initiator to prepare a polyhydroxyethyl methacrylate main chain through atom transfer radical polymerization of monomer hydroxyethyl methacrylate, forming an ATRP (atom transfer radical polymerization) initiation site on the side end of the main chain by a method of esterifying the main chain with a bromination reagent 2-bromoisobutyryl bromide, then sequentially carrying out ATRP on the initiation site on the side end of the main chain by taking tert-butyl acrylate and styrene as monomers to form the graft block polymer, and finally hydrolyzing the tert-butyl acrylate of the side chain with trifluoroacetic acid to obtain a product PHEMA-g- [ PAA-b-PS ];
(2) The guided assembly of CdSe nano-rod, in three-neck round-bottom flask equipped with magneton, add precursor of cadmium, inject graft block polymer template solution under inert atmosphere, stir, heat at room temperature, inject precursor solution of selenium, reflux reaction; standing the reaction solution, and carrying out graded centrifugal dispersion to obtain the CdSe nanorod;
the grafting block polymer template solution is prepared by dissolving N-N-Dimethylformamide (DMF); the precursor of cadmium is chromium acetylacetonate (Cd (acac) 2 ) (ii) a The precursor solution of selenium is a selenium powder solution of trioctylphosphine;
the volume of the grafting block polymer template solution is 10mL; the mass of the precursor of cadmium is 108mg; the mass of selenium powder in the selenium precursor solution is 28mg, and the volume of trioctylphosphine is 2mL;
the stirring time at normal temperature is 2 hours, the heating temperature is 180 ℃, and the reflux reaction time is 2 hours; and the reaction solution is kept standing for 7d, and the specific process of fractional centrifugation is that supernatant is taken after centrifugation is carried out for 5 minutes at 1000 revolutions/separation, precipitation is taken after centrifugation is carried out for 5 minutes at 5000 revolutions/separation of the supernatant, and toluene is used for dispersing.
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