CN111849111A - Two-dimensional Janus nano material and preparation method thereof - Google Patents
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Abstract
The invention discloses a two-dimensional Janus nano material and a preparation method thereof. The two-dimensional Janus nano material is prepared by self-assembling a block copolymer on a two-dimensional structure model through crosslinking. The preparation method comprises the following steps: 1) growing metal particles on the surface of the silicon dioxide ball, and then modifying the silicon dioxide ball by using alkyl silane; removing the metal particles on the modified silicon dioxide spheres and loading imidazole groups to obtain a template A; 2) and mixing the block copolymer with the template A, carrying out self-assembly in a polar organic solvent, and then adding a cross-linking agent for cross-linking reaction to obtain the two-dimensional Janus nano material. The two-dimensional Janus nano material has the advantages of adjustable chemical composition, adjustable thickness and adjustable outer diameter; the preparation method has the advantages of simplicity, convenience, low cost, convenience in microstructure adjustment and the like. The method can realize rapid and batch preparation of the Janus material with multiple potential functionalities and accurately regulated and controlled composition and structure.
Description
Technical Field
The invention relates to a two-dimensional Janus nano material and a preparation method thereof, belonging to the field of macromolecules.
Background
Janus connotation is the two-sided spirit of the ancient Roman mystery. In 1991, de Gennes first proposed Janus's concept in the polymer field to describe particles composed of two materials with different chemical and physical properties (de Gennes, P.G. Soft Matter. science.1992,256(5056), 495-497). Janus materials with the characteristic of multiple functions are novel materials and have important application prospects in various fields. The existing method for preparing the two-dimensional Janus nano material still has a plurality of problems. The commonly used comminution methods for the production of two-dimensional sheet materials (Walther, A.; Andre, X.; Drechsler, M.; Abetz, V.; Mueller, A.H.E.Janus Discs. "Janus Discs", J.Am.Chem.Soc.2007,129,6187-6198.) achieve Janus structures, but the shape and size are difficult to control. The self-assembly method (Deng, R.H.; Liang, F.X.; Zhou, P.; Zhang C.L.; Qu X.Z.Wang, Q.; Li, J.L.; Zhuu, J.T.and Yang, Z.Z.Janus Nanodisc of diblock copolymers. adv. Mater.2014,26, 4469-. The printing processes commonly used to prepare two-dimensional loop materials (McLellan, J.M.; Geissler, M.; Xia, Y.N. "edge spreading Lithography and its Application to the Fabrication of the textile of the social gold and Silver Rings", J.am. chem. Soc.2004,126,10830-10831.) are costly. Etching (Xu, H.; Goedel, W.A. "meso Rings by Controlled etching of Particle Imprintedplates", Angew.chem., int.Ed.2003,42, 4696-. In addition, the methods do not prepare nanorings with Janus structures, and cannot prepare sheet materials.
Disclosure of Invention
The invention aims to provide a two-dimensional Janus nano material and a preparation method thereof, wherein the two-dimensional Janus nano material has adjustable chemical composition, adjustable thickness and adjustable outer diameter; the preparation method is simple and convenient, has low cost and is convenient for microstructure adjustment.
The two-dimensional Janus nano material provided by the invention is prepared by self-assembling a block copolymer on a two-dimensional structure model through crosslinking.
In the two-dimensional Janus nano material, the two-dimensional structure model is disc-shaped or circular;
the particle size of the two-dimensional Janus nano material can be 10-50 nm, and preferably 20-30 nm.
In the two-dimensional Janus nanomaterial, the block copolymer comprises a polyacrylic acid-polystyrene block copolymer or a sodium polystyrene sulfonate-polystyrene block copolymer;
the block ratio of the polyacrylic acid-polystyrene block copolymer can be 1: 0.2-12, specifically 1:12, 9:2.3, 9.8:2.3, 1:1 or 1: 0.23-12; the block ratio of the sodium polystyrene sulfonate-polystyrene block copolymer can be 1: 0.2-12, and specifically can be 9:2 and 1: 12.
The invention also provides a preparation method of the two-dimensional Janus nano material, which comprises the following steps:
1) Growing metal particles on the surface of the silicon dioxide ball, and then modifying the silicon dioxide ball by using alkyl silane; removing the metal particles on the modified silicon dioxide spheres and loading imidazole groups to obtain a template A;
2) and mixing the block copolymer with the template A, carrying out self-assembly in a polar organic solvent, and then adding a cross-linking agent for cross-linking reaction to obtain the two-dimensional Janus nano material.
In the above preparation method, step 2) further comprises a step of removing the template a by fractional centrifugation after the crosslinking reaction. The specific conditions can be heating reaction to 65 ℃, stirring reaction for 120min, and then carrying out fractional centrifugation.
In the above preparation method, the cross-linking reaction is performed with the polar organic solvent to obtain the disc-shaped two-dimensional Janus nanomaterial;
and the crosslinking reaction is carried out by adopting a nonpolar organic solvent to obtain the annular two-dimensional Janus nano material.
In the above preparation method, the metal particles include at least one of gold particles, silver particles, nickel particles, iron particles, and oxide particles thereof, specifically, the oxide particles are silver nitrate, nickel nitrate, and Fe3O4Particles of FeOOH;
The mass ratio of the silicon dioxide spheres to the metal particles can be 1: 0.3-1.5, and specifically can be 1: 0.9;
the alkyl silane is at least one of n-octyl trimethoxy silane, octadecyl triethoxy silane and n-octyl trimethoxy silane, and the alkyl silane accounts for 1-50% of the total mass of the silicon dioxide spheres after metal particles grow on the surfaces of the silicon dioxide spheres;
hydrochloric acid and/or nitric acid are adopted for removing the metal particles;
the loading capacity of the imidazole group loaded on the modified silicon dioxide ball can be 1-3%.
In the present invention, the alkylsilane-modified silica spheres are prepared by a method known to those skilled in the art.
In the above preparation method, the mass ratio of the template a to the block copolymer may be 1: 0.01-0.1, specifically 1:0.05, 1: 0.01-0.05, 1: 0.05-0.1 or 1: 0.02 to 0.08;
the block ratio of the polyacrylic acid-polystyrene block copolymer can be 1: 0.2-12, specifically 1:12, 9:2.3, 9.8:2.3, 1:1 or 1: 0.2-12; the block ratio of the sodium polystyrene sulfonate-polystyrene block copolymer can be 1: 0.2-12, and specifically can be 9:2 and 1: 12.
In the above preparation method, the polar organic solvent is at least one selected from tetrahydrofuran, N-dimethylformamide and dimethylsulfoxide;
The nonpolar organic solvent is selected from at least one of n-hexane, n-heptane, n-octane and n-decane;
the cross-linking agent is at least one of 1, 6-hexamethylene diisocyanate, 1, 8-octanedionate and 1, 10-decanedionate.
In the above preparation method, the mass ratio of the template a, the block copolymer, and the crosslinking agent is 1: 0.01-0.1: 0.001-0.1, specifically 1: 0.05: 0.005, 1: 0.05-0.1: 0.005-0.1, 1: 0.01-0.05: 0.001 to 0.005 or 1: 0.02-0.08: 0.002-0.075;
the total solid content of the block copolymer, the template A and the cross-linking agent in a reaction system of the cross-linking reaction can be 0.1-10%, preferably 1-5% by mass percent;
the conditions for the self-assembly are as follows: the temperature can be 0-50 ℃, preferably 20-40 ℃, and specifically can be normal temperature; the time can be 30-300 min, specifically 120min, 240min, 60-120 min or 120-240 min;
the conditions of the crosslinking reaction are as follows: the temperature can be 0-50 ℃, preferably 20-40 ℃, and specifically can be normal temperature; the time is 10-120 min, specifically 60min, 120min or 60-120 min.
In the invention, the normal temperature is common knowledge in the field, and is 0-30 ℃, and specifically can be 25 ℃.
The invention also provides the two-dimensional Janus nano material prepared by the preparation method.
The structure of the two-dimensional Janus nano material is disc-shaped or circular.
The particle size of the two-dimensional Janus nano material is 10-50 nm, and preferably 20-30 nm.
The two-dimensional Janus nano material disclosed by the invention is applied to the fields of catalysis, oil-water separation, water purification and cell identification.
The invention has the following advantages:
the two-dimensional Janus nano material has the advantages of adjustable chemical composition, adjustable thickness and adjustable outer diameter; the preparation method has the advantages of simplicity, convenience, low cost, convenience in microstructure adjustment and the like, and is a method for preparing the Janus two-dimensional nano material with uniform structure and adjustable microstructure. The invention can realize the quick and batch preparation of the Janus material with multiple potential functions, the composition and the structure of which are accurately regulated and controlled, and the Janus material has the excellent properties of various polymers and has important significance in the fields of catalysis, oil-water separation, water purification, cell identification and the like.
Drawings
FIG. 1 is a transmission and atomic force microscope image of a two-dimensional Janus nanodisk made in EXAMPLE 4 of this invention.
Fig. 2 is a transmission and atomic force microscope image of a two-dimensional Janus nanoring prepared in example 8 of the present invention.
Detailed Description
The experimental procedures used in the following examples are all conventional procedures unless otherwise specified.
Materials, reagents and the like used in the following examples are commercially available unless otherwise specified.
Example 1 preparation of template A
Ethanol (40mL) was added to silica microspheres (0.1g), ethanol (25mL) was added to silver nitrate (0.09g), the two were mixed at 50 ℃ and stirred for 15min, n-butylamine (0.05mL) was added, the reaction was carried out for 10min, the mixture was washed, and the sample was lyophilized. The above-mentioned product (0.1g) was reacted with dichloromethane (50mL) and n-octylethoxysilane (0.5mL) under stirring at ordinary temperature for 6 hours, and then washed. The above product was added to nitric acid (20mL) containing 32 wt% of water to react for 10min, and then washed with ethanol. The product is washed after the surface of the product is treated by using an imidazole silane coupling agent, the load capacity of the imidazole group loaded on the modified silicon dioxide ball is 2.3 percent, and the sample is freeze-dried. Obtaining a template A.
Example 2 preparation of template A
Ethanol (40mL) was added to silica microspheres (0.1g), ethanol (25mL) was added to nickel nitrate (0.09g), the two were mixed and stirred at 50 ℃ for 15min, n-butylamine (0.05mL) was added, the reaction was carried out for 60min, the mixture was washed, and the sample was lyophilized. Chloroform (50mL) and n-octylmethoxysilane (0.5mL) were added to the above product (0.1g), and the mixture was stirred at room temperature for 12 hours and then washed. The above product was added to nitric acid (20mL) containing 32 wt% of water to react for 10min, and then washed with ethanol. The product is washed after the surface of the product is treated by using an imidazole silane coupling agent, the loading capacity of the imidazole group loaded on the modified silicon dioxide ball is 2.4%, and a sample is freeze-dried. Obtaining a template A.
Example 3 preparation of template A
Ethanol (40mL) was added to silica microspheres (0.1g), ethanol (25mL) was added to nickel nitrate (0.09g), the two were mixed and stirred at 50 ℃ for 15min, n-butylamine (0.05mL) was added, the reaction was carried out for 40min, the mixture was washed, and the sample was lyophilized. Chloroform (50mL) and n-octylmethoxysilane (0.5mL) were added to the above product (0.1g), and the mixture was stirred at room temperature for 12 hours and then washed. The above product was added to nitric acid (20mL) containing 32 wt% of water to react for 10min, and then washed with ethanol. The product is washed after the surface of the product is treated by using an imidazole silane coupling agent, the loading capacity of the imidazole group loaded on the modified silicon dioxide ball is 2.9 percent, and a sample is freeze-dried. Obtaining a template A.
Example 4 preparation of nanodisk-type Janus Material
Tetrahydrofuran (20mL) was added to template A (20mg) prepared in inventive example 1, and polyacrylic acid was added1.1k-styrene12kThe block copolymer (1mg) was stirred at room temperature (25 ℃ C.) for 120min, and then centrifuged to wash. The reaction product was dispersed in tetrahydrofuran (20mL), and 1, 6-hexamethylene diisocyanate (0.1mL) was added thereto, stirred at room temperature (25 ℃) and reacted for 120min, followed by centrifugal washing. Dispersing the product in tetrahydrofuran (20mL), adding hydrochloric acid (25 mu L), heating to react to 65 ℃, stirring to react for 120min, then carrying out fractional centrifugation, carrying out low-speed centrifugation, carrying out high-speed centrifugation again, and carrying out freeze-drying on the sample, wherein the supernatant contains the nano disc type Janus material. As shown in FIG. 1, the diameter of the nanodisc-type Janus material was found to be about 10nm by transmission electron microscopy, and the height thereof was 1nm by AFM.
Example 5 preparation of nanodisk-type Janus Material
Tetrahydrofuran (20mL) was added to template A (20mg) prepared in inventive example 2, and polyacrylic acid was added9k-polystyrene2.3kBlock copolymer (PAA for short)9k-b-PS2.3k1mg), stirred at normal temperature (25 ℃) for 120min, and then centrifuged to wash. The reaction product was dispersed in tetrahydrofuran (20mL), and 1, 6-hexamethylene diisocyanate (0.1mL) was added thereto, stirred at room temperature (25 ℃) and reacted for 120min, followed by centrifugal washing. Dispersing the product in tetrahydrofuran (20mL), adding hydrochloric acid (25 μ L), heating to 65 deg.C, stirring for reaction for 120min, centrifuging at low speed to obtain supernatant containing nanometer disc type Janus material, centrifuging at high speed,samples were lyophilized. The diameter of the nano-disc Janus material is about 30nm through a transmission electron microscope.
Example 6 preparation of nanodisk-type Janus Material
N, N-dimethylformamide (20mL) was added to the template A (20mg) prepared in inventive example 3, followed by addition of sodium polystyrene sulfonate9k-polystyrene2kBlock copolymer (PSS for short)9k-b-PS2k1mg) at normal temperature (25 ℃) for 120min, stirring for 240min, and centrifuging and washing. The reaction product was dispersed in N, N-dimethylformamide (20mL), and 1, 8-octanedionato (0.1mL) was added, stirred at room temperature (25 ℃ C.) for 60 minutes and then washed by centrifugation. Dispersing the product in N, N-dimethylformamide (20mL), adding hydrochloric acid (25 mu L), heating to react to 65 ℃, stirring to react for 120min, then carrying out fractional centrifugation, carrying out low-speed centrifugation, obtaining a supernatant containing the nano disc type Janus material, carrying out high-speed centrifugation, and carrying out sample freeze-drying. The diameter of the nano-disc Janus material is about 20nm through a transmission electron microscope.
Example 7 preparation of nanodisk-type Janus Material
Tetrahydrofuran (20mL) was added to template A (20mg) prepared in inventive example 1, and polyacrylic acid was added9.8k-polystyrene2.3kThe block copolymer (1mg) was stirred at room temperature (25 ℃ C.) for 120min, and then centrifuged to wash. The reaction product was dispersed in tetrahydrofuran (20mL), and 1, 6-hexamethylene diisocyanate (0.1mL) was added thereto, stirred at room temperature (25 ℃) and reacted for 120min, followed by centrifugal washing. Dispersing the product in tetrahydrofuran (20mL), adding hydrochloric acid (25 mu L), heating to react to 65 ℃, stirring to react for 120min, then carrying out fractional centrifugation, carrying out low-speed centrifugation, carrying out high-speed centrifugation again, and carrying out freeze-drying on the sample, wherein the supernatant contains the nano disc type Janus material. The diameter of the nano-disc Janus material is about 10nm through a transmission electron microscope. AFM characterized it to be 3nm in height.
Example 8 preparation of Nanocyclic Janus Material
Tetrahydrofuran (20mL) was added to template A (20mg) prepared in inventive example 1, and polyacrylic acid was added1k-polystyrene1kBlock copolymer (PAA for short)1k-b-PS1k1mg) was stirred at room temperature (25 ℃ C.) for 120min, and then centrifugedAnd (6) washing. The reaction product was dispersed in n-hexane (20mL), and 1, 6-hexamethylene diisocyanate (0.1mL) was added thereto, stirred at room temperature (25 ℃) and reacted for 120min, and then centrifuged and washed. Dispersing the product in tetrahydrofuran (20mL), adding hydrochloric acid (25 mu L), heating to react to 65 ℃, stirring to react for 120min, then carrying out fractional centrifugation, carrying out low-speed centrifugation, obtaining a supernatant containing the nano ring type Janus material, carrying out high-speed centrifugation, and carrying out sample freeze-drying. As shown in FIG. 2, the outer diameter of the nano-ring type Janus material is about 10nm as found by transmission electron microscopy.
Example 9 preparation of Nanocyclic Janus Material
N, N-dimethylformamide (20mL) was added to the template A (20mg) prepared in inventive example 2, followed by addition of sodium polystyrene sulfonate9k-polystyrene2kBlock copolymer (PSS for short)9k-b-PS2k1mg), stirred at normal temperature for 240min, and then centrifuged. The reaction product was dispersed in n-decane (20mL), and 1, 8-octanedionato (0.1mL) was added thereto, stirred at room temperature for 60min and then centrifuged to wash the mixture. Dispersing the product in N, N-dimethylformamide (20mL), adding hydrochloric acid (25 mu L), heating to 65 ℃, stirring to react for 120min, then carrying out fractional centrifugation, carrying out low-speed centrifugation, obtaining a supernatant containing the nano ring type Janus material, carrying out high-speed centrifugation, and carrying out sample freeze-drying. The outer diameter of the nano ring type Janus material is about 30nm through a transmission electron microscope.
Example 10 preparation of Nanocyclic Janus Material
N, N-dimethylformamide (20mL) was added to the template A (20mg) prepared in inventive example 3, followed by addition of sodium polystyrene sulfonate1k-polystyrene12kBlock copolymer (PSS for short)1k-b-PS12k1mg), stirred at normal temperature for 240min, and then centrifuged. The reaction product was dispersed in n-decane (20mL), and 1, 8-octanedionato (0.1mL) was added thereto, stirred at room temperature for 60min and then centrifuged to wash the mixture. Dispersing the product in N, N-dimethylformamide (20mL), adding hydrochloric acid (25 mu L), heating to 65 ℃, stirring to react for 120min, then carrying out fractional centrifugation, carrying out low-speed centrifugation, obtaining a supernatant containing the nano ring type Janus material, carrying out high-speed centrifugation, and carrying out sample freeze-drying. The outer diameter of the nano ring type Janus material is about 20nm through a transmission electron microscope 。
According to the embodiment, the two-dimensional Janus nano-material is prepared by cross-linking the segmented copolymer after the limited-domain self-assembly in the patch area, the structural model is a disc or a circular ring, the chemical composition of the two-dimensional Janus nano-material is adjustable, the thickness of the two-dimensional Janus nano-material is adjustable, and the outer diameter of the two-dimensional Janus nano-material is adjustable.
The foregoing is only a preferred embodiment of the present invention, and it should be noted that, for those skilled in the art, various modifications and improvements can be made without departing from the principle of the present invention, and such modifications and improvements should also be considered within the scope of the present invention.
Claims (10)
1. A two-dimensional Janus nanomaterial, which is characterized in that: the two-dimensional Janus nano material is prepared by self-assembling a block copolymer on a two-dimensional structure model through crosslinking.
2. The two-dimensional Janus nanomaterial as recited in claim 1, wherein: the two-dimensional structure model is disc-shaped or circular;
the particle size of the two-dimensional Janus nano material is 10-50 nm.
3. The two-dimensional Janus nanomaterial as recited in claim 1 or 2, wherein: the block copolymer comprises polyacrylic acid-polystyrene block copolymer or sodium polystyrene sulfonate-polystyrene block copolymer;
The block ratio of the polyacrylic acid-polystyrene block copolymer is 1: 0.2-12; the block ratio of the sodium polystyrene sulfonate-polystyrene block copolymer is 1: 0.2-12.
4. A method of preparing the two-dimensional Janus nanomaterial of any of claims 1-3, comprising the steps of:
1) growing metal particles on the surface of the silicon dioxide ball, and then modifying the silicon dioxide ball by using alkyl silane; removing the metal particles on the modified silicon dioxide spheres and loading imidazole groups to obtain a template A;
2) and mixing the block copolymer with the template A, carrying out self-assembly in a polar organic solvent, and then adding a cross-linking agent for cross-linking reaction to obtain the two-dimensional Janus nano material.
5. The method of claim 4, wherein: the step 2) also comprises a step of removing the template A by fractional centrifugation after the crosslinking reaction.
6. The production method according to claim 4 or 5, characterized in that: when the cross-linking reaction is carried out by adopting the polar organic solvent, the disc-shaped two-dimensional Janus nano material is obtained;
and when the crosslinking reaction is carried out by adopting a nonpolar organic solvent, the annular two-dimensional Janus nano material is obtained.
7. The production method according to any one of claims 4 to 6, characterized in that: the metal particles include at least one of gold particles, silver particles, nickel particles, iron particles, and oxide particles thereof;
the mass ratio of the silicon dioxide balls to the metal particles is 1: 0.3-1.5;
the alkyl silane is at least one of n-octyl trimethoxy silane, octadecyl triethoxy silane and n-octyl trimethoxy silane, and the alkyl silane accounts for 1-50% of the total mass of the silicon dioxide spheres after metal particles grow on the surfaces of the silicon dioxide spheres;
hydrochloric acid and/or nitric acid are adopted for removing the metal particles;
the loading amount of the imidazole groups loaded on the modified silicon dioxide spheres is 1-3%.
8. The production method according to any one of claims 4 to 7: the mass ratio of the template A to the block copolymer is 1: 0.01 to 0.1;
the block ratio of the polyacrylic acid-polystyrene block copolymer is 1: 0.20-12; the block ratio of the sodium polystyrene sulfonate-polystyrene block copolymer is 1: 0.2-12.
9. The production method according to any one of claims 6 to 8: the polar organic solvent is at least one selected from tetrahydrofuran, N-dimethylformamide and dimethyl sulfoxide;
The nonpolar organic solvent is selected from at least one of n-hexane, n-heptane, n-octane and n-decane;
the cross-linking agent is at least one of 1, 6-hexamethylene diisocyanate, 1, 8-octanedionate and 1, 10-decanedionate.
10. The production method according to any one of claims 4 to 6: the mass ratio of the template A, the block copolymer and the cross-linking agent is 1: 0.01-0.1: 0.001 to 0.1;
the total solid content of the block copolymer, the template A and the cross-linking agent in a reaction system of the cross-linking reaction is 0.1-10% by mass percent;
the conditions for the self-assembly are as follows: the temperature is 0-50 ℃; the time is 30-300 min;
the conditions of the crosslinking reaction are as follows: the temperature is 0-50 ℃; the time is 10-120 min.
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| CN101885813A (en) * | 2009-05-14 | 2010-11-17 | 中国科学院化学研究所 | Compound Janus colloid particle and modified Janus colloid particle as well as preparation methods thereof |
| CN108311067A (en) * | 2017-01-16 | 2018-07-24 | 中国科学院理化技术研究所 | Oil-water microemulsion separation method based on composite Janus microspheres |
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| CN101885813A (en) * | 2009-05-14 | 2010-11-17 | 中国科学院化学研究所 | Compound Janus colloid particle and modified Janus colloid particle as well as preparation methods thereof |
| CN108311067A (en) * | 2017-01-16 | 2018-07-24 | 中国科学院理化技术研究所 | Oil-water microemulsion separation method based on composite Janus microspheres |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN115181277A (en) * | 2021-04-02 | 2022-10-14 | 中国科学院化学研究所 | Preparation method of metal composite polymer single-chain nano-particles |
| CN115181277B (en) * | 2021-04-02 | 2023-12-01 | 中国科学院化学研究所 | Preparation method of metal composite polymer single-chain nano particles |
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