CN105949364A - Novel photo-irradiation induced self-repairing precious metal nano composite hydrogel and preparation method thereof - Google Patents
Novel photo-irradiation induced self-repairing precious metal nano composite hydrogel and preparation method thereof Download PDFInfo
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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
- 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
- C08F120/52—Amides or imides
- C08F120/54—Amides, e.g. N,N-dimethylacrylamide or N-isopropylacrylamide
- C08F120/56—Acrylamide; Methacrylamide
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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
- C08F2/00—Processes of polymerisation
- C08F2/44—Polymerisation in the presence of compounding ingredients, e.g. plasticisers, dyestuffs, fillers
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- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/02—Elements
- C08K3/08—Metals
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K9/00—Use of pretreated ingredients
- C08K9/04—Ingredients treated with organic substances
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/02—Elements
- C08K3/08—Metals
- C08K2003/0831—Gold
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K2201/00—Specific properties of additives
- C08K2201/011—Nanostructured additives
Abstract
The invention discloses novel photo-irradiation induced self-repairing precious metal nano composite hydrogel. According to the hydrogel, a dynamic precious metal-sulfur coordination bond serves as a self-healing body which has a uniform mesh structure, that is, monomer has uniform polymerization reaction in the polymerization process, and accordingly the hydrogel has good stretchability and strength. The hydrogel has good notch sensitivity prevention capacity, that is, when notches or cracks exist in the surface of the hydrogel, hydrogel still has good stretchability. By means of the precious metal-sulfur coordination bond and good light-heat properties of precious metal, the hydrogel shows good self-repairing performance under stimulation of infrared laser.
Description
Technical field
The present invention relates to technical field of nano material, particularly relate to a kind of photo-thermal induction selfreparing noble metal nano composite aquogel and preparation method thereof.
Background technology
Hydrogel is a kind of with water as disperse medium, by the water-soluble polymer of the three-dimensional crosslinked network structure that certain chemistry or physical crosslinking are formed.As features such as a kind of softness and High water cut, hydrogel is widely used in sensing and detection, drug release, driver and organizational project etc. in recent years.For other " firmly " materials, hydrogel all stimulations to external world can have good response.Common macromolecule hydrogel is general in preparation process uses chemical small molecule as cross-linking agent, polymerization process is often based on atactic polymerization, thus crosslinking points dispersibility is poor in the cross-linked network formed, thus bring is that obtained hydrogel is bad to the energy dissipation of external force, apparent on show mechanical strength and draftability is poor.Nanometer composite hydrogel is that Japanese Scientists T. Takehisa put forward in 2002, this hydrogel uses nano-particle (clay flake) as cross-linking agent in preparation process, different from conventional hydrogel, its polymerization process happens is that homogeneous polymerization, crosslinking points is uniformly dispersed in whole network structure, plus the introducing of inorganic nano material, its Nanometer composite hydrogel formed has superpower mechanical strength and swelling behavior.
Selfreparing in recent years is looked at by people institute parent as a kind of typical characteristic being widely present in biomaterial.Biological tissue can pass through the self-regeneration of cell or tissue when by environmental damage thus recover its original function and structure.For common macromolecule hydrogel, usually do not possess this intelligent.For having the Nanometer composite hydrogel of high intensity, self-healing properties is particularly important, its service life and safety in utilization etc. of being possible not only to extend hydrogel, and the development and application tool for hydrogel has very important significance.Up to the present, people utilize various method to be allowed to possess self-healing properties to design hydrogel, such as introduce renovation agent, introduce dynamic or reversible covalently or non-covalently active force as selfreparing theme in hydrogel network.Dynamic or reversible active force mainly includes hydrogen bond, metal-nitrogen coordinate bond, boron-oxygen key and cystine linkage etc..But these selfreparing modes are the highest on repair time and remediation efficiency, and up to the present, also do not combine with the Nanometer composite hydrogel of high intensity.The most necessary selfreparing being combined with Nanometer composite hydrogel, research and development have the high-strength nano composite aquogel of self-healing properties quick, high efficiency.
Summary of the invention
The technical problem to be solved in the present invention is to provide a kind of photo-thermal induction selfreparing noble metal nano composite aquogel and preparation method thereof.
For solving above-mentioned technical problem, the technical solution used in the present invention is as follows.
A kind of photo-thermal induction selfreparing noble metal nano composite aquogel, this hydrogel is using dynamic noble metal-sulfur coordinate bond as spontaneous recovery main body, it has uniform network structure, i.e. monomer occurs homogeneous polymerization to react in the course of the polymerization process, so that this hydrogel has good draftability and intensity；It has a good anti-notch sensitive performance, during i.e. jagged in hydrogel surface or crackle, still has good tensile property；It utilizes the light thermal property that noble metal is good with the dynamic coordination key of sulfur and noble metal, shows good self-healing properties under the stimulation of iraser.
The preparation method of a kind of photo-thermal induction selfreparing noble metal nano composite aquogel, comprises the following steps:
A, prepare noble metal nanometer material dispersion liquid: use zero dimension noble metal nano particles appearance structure dispersion liquid, one-dimensional noble metal nano wire appearance structure dispersion liquid or two-dimensional noble metal nanometer sheet appearance structure dispersion liquid；
B, the modification of noble metal nanometer material: weigh the functional modification body accounting for noble metal nanometer material dispersion liquid gross mass 0.002-0.02%, join in step A gained noble metal nanometer material dispersion liquid, it is sufficiently stirred for and ultrasonic mixing 10-30min, obtains surface-functionalized noble metal nanometer material；
The dissolving of C, hydrophilic monomer, initiator and accelerator: weigh and account for the hydrophilic monomer of noble metal nanometer material dispersion liquid gross mass 10-20%, account for the initiator of noble metal nanometer material dispersion liquid gross mass 0.1-0.5% and account for the accelerator of noble metal nanometer material dispersion liquid gross mass 0.0001-0.001% and join in step B gained solution, it is sufficiently stirred for and ultrasonic mixing 10-30min is to fully dissolving, it is passed through nitrogen 5-15min, in vacuum desiccator, then removes the gas dissolved in solution；
D, the preparation of hydrogel: by the mixed solution of step C prepolymerization 1-3h in the water-bath of 0 DEG C, after at room temperature continue polyase 13 0-60h, obtain light thermal induction self-healing, high-strength nano composite aquogel.
As a preferred technical solution of the present invention, in step A, the preparation method of noble metal nano particles dispersion liquid is: preparation solution 1:0.3-6 mmol/L noble metal salt aqueous solution and solution 2:40-800 mmol/L trisodium citrate aqueous solution respectively, then take 40-60 mL solution 1 and be heated to boiling, take 0.5-1.5 mL solution 2 again and join in solution 1 holding boiling reaction 3-7min, i.e. obtain noble metal through distilled water and ethanol centrifuge washing after natural cooling and receive particle dispersion.
As a preferred technical solution of the present invention, in step A, the preparation method of noble metal nano wire dispersion liquid is: take 0.05-0.2 g precious metal salt and 8-12 mL oleyl amine ultrasonic mix homogeneously in 1mL n-hexane, it is heated to 80-900 DEG C the most under nitrogen atmosphere and is stirred vigorously 5-15min, then under the conditions of 80-90 DEG C, stand 3-7h, take out solution after room temperature cooling, then use volume ratio acetone: the mixed solvent centrifuge washing of ethanol=1:3 i.e. obtains noble metal nano wire dispersion liquid；
As a preferred technical solution of the present invention, in step A, the preparation method of noble metal nano-plate dispersion liquid is: joined by 0.02-0.2 mol/L noble metal salt aqueous solution 1 mL in the polytetrafluoroethylcontainer container of 10-20 mL ethylene glycol, and add 0.01-0.1 g polyvinylpyrrolidone and 0.05-0.5g glucose, continuously stirred 3-7min, then reaction vessel is put in microwave reactor, reaction 10-30min, i.e. obtains noble metal nano-plate dispersion liquid with distilled water and ethanol centrifuge washing after natural cooling.
As a preferred technical solution of the present invention, in step A, described precious metal salt is the soluble precursor of synthesis noble metal nanometer material, and described noble metal uses one or several mixing in gold, silver, copper, platinum.
As a preferred technical solution of the present invention, in step B, described functional modification body uses water solublity mercaptides organic molecule, comprises polymerisable carbon-carbon double bond in small molecule structure therein.
As a preferred technical solution of the present invention, in step C, described hydrophilic monomer is acrylamide, N, N dimethyl acrylamide or acrylic acid；Described initiator is the persulfate derivant including Ammonium persulfate., potassium peroxydisulfate；Described accelerator is tetramethylethylenediamine.
As a preferred technical solution of the present invention, in the preparation process of step D, the complex after noble metal nanometer material is combined with functional modification body carries out system crosslinking as multi-functional cross-linking agent, the most additionally adds cross-linking agent.
Use and have the beneficial effects that produced by technique scheme:
The present invention uses noble metal nanometer material complex that functional modification body modifies as cross-linking agent when preparing Nanometer composite hydrogel, wherein noble metal is combined by dynamic noble metal-sulfur coordinate bond with modifying body, this coordinate bond is the most special a kind of coordinate bond, it is highly stable under normal temperature condition, therefore the network structure of hydrogel has the highest intensity, when system is heated, this coordinate bond stability reduces；Utilize this feature and combine the light thermal property that noble metal is good, the three-dimensional net structure of hydrogel is when sustaining damage, can be under the induction of light or heat, free surface tracking is there is at damage interface, reach the effect of selfreparing, hydrogel after selfreparing still can reach the draftability before damage and intensity, and its self-repair efficiency reaches more than 96%.The structure of subject hydrogel is the network structure of a homogeneous polymerization, its mechanical strength is up to a MPa rank, elongation strain is up to more than 20 times, and in the presence of crackled, remain to show the tensile property of excellence, show the anti-notch sensitivity of uniqueness, utilizing the good light thermal property of noble metal nanometer material, hydrogel shows good self-healing performance under infrared light (808 nm) irradiates.Meanwhile, the whole synthesis technique of preparation method of the present invention is simple, and reaction condition is gentle, is suitable for various polymeric system.
To sum up, originally the invention provides a kind of brand-new selfreparing principle, i.e. noble metal-sulfur coordinate bond, this coordinate bond can issue fracture and the combination of biochemical key in the induction of light or heat, i.e. the reversibility of chemical bond, the selfreparing for material provides theoretical basis；Such photo-thermal induction selfreparing noble metal nano composite aquogel has a good application prospect in fields such as biomedicine and organizational projects.
Accompanying drawing explanation
Fig. 1 is the transmission electron microscope photo of gold nano grain.
Fig. 2 is the transmission electron microscope photo of gold nano grain/functionalized modification nanocrystal composition.
In Fig. 3, (a) is the optical photograph of gold nano grain/polyacrylamide nano composite aquogel；B () is the lyophilization stereoscan photograph of gold nano grain/polyacrylamide nano composite aquogel.
Fig. 4 is the optical photograph that Nanometer composite hydrogel prepared by embodiment 5 mentions 500mL water bottle.
Fig. 5 is the stretching optical photograph of the Nanometer composite hydrogel of embodiment 5 preparation.
Fig. 6 is the anti-notch sensitivity optical photograph of the Nanometer composite hydrogel of embodiment 5 preparation.
Fig. 7 be embodiment 5 preparation Nanometer composite hydrogel near-infrared laser under selfreparing optical photograph.
Detailed description of the invention
Following example are described in detail the present invention.Various raw material used in the present invention and items of equipment are conventional commercial product, all can be bought by market and directly obtain.
Embodiment 1, photo-thermal induction selfreparing noble metal nano composite aquogel.
The photo-thermal induction selfreparing noble metal nano composite aquogel of the present embodiment, using dynamic noble metal-sulfur coordinate bond as spontaneous recovery main body, it has uniform network structure, i.e. monomer occurs homogeneous polymerization to react in the course of the polymerization process, so that this hydrogel has good draftability and intensity, its mechanical strength is up to a MPa rank, and elongation strain is up to more than 20 times；It has a good anti-notch sensitive performance, during i.e. jagged in hydrogel surface or crackle, still has good tensile property, shows the anti-notch sensitivity of uniqueness；It utilizes the light thermal property that noble metal is good with the dynamic coordination key of sulfur and noble metal, shows good self-healing properties under the stimulation of 808 nm irasers.
Embodiment 2, the preparation of noble metal nanometer material dispersion liquid.
Noble metal nanometer material dispersion liquid has three kinds of forms on probation: zero dimension noble metal nano particles appearance structure dispersion liquid, one-dimensional noble metal nano wire appearance structure dispersion liquid or two-dimensional noble metal nanometer sheet appearance structure dispersion liquid.
(1), the preparation of noble metal nano particles dispersion liquid: preparation solution 1:0.3 mmol/L aqueous solution of chloraurate and solution 2:40mmol/L trisodium citrate aqueous solution respectively, then take 50 mL solution 1 and be heated to boiling, take 1 mL solution 2 again and join in solution 1 holding boiling reaction 5min, i.e. obtain noble metal for 3 times through distilled water and ethanol centrifuge washing after natural cooling and receive particle dispersion；
(2), the preparation of noble metal nano wire dispersion liquid: take 0.1 g gold chloride and 10 mL oleyl amines ultrasonic mix homogeneously in 1mL n-hexane, it is heated to 85 DEG C the most under nitrogen atmosphere and is stirred vigorously 10min, then under the conditions of 85 DEG C, stand 5h, take out solution after room temperature cooling, then use volume ratio acetone: the mixed solvent centrifuge washing of ethanol=1:3 i.e. obtains noble metal nano wire dispersion liquid 3 times；
(3), the preparation of noble metal nano-plate dispersion liquid: 0.1 mol/L aqueous solution of chloraurate 1 mL is joined in the polytetrafluoroethylcontainer container of 15 mL ethylene glycol, and add 0.013 g polyvinylpyrrolidone and 0.144g glucose, continuously stirred 5min, then reaction vessel is put in microwave reactor, reaction 20min, i.e. obtains noble metal nano-plate dispersion liquid 3 times with distilled water and ethanol centrifuge washing after natural cooling.
Embodiment 3, the modification of noble metal nanometer material.
Weigh and account for the functional modification body of noble metal nanometer material dispersion liquid (use granule-morphology dispersion liquid) gross mass 0.02% and join in noble metal nanometer material dispersion liquid, be sufficiently stirred for and ultrasonic mixing 20min, obtain surface-functionalized noble metal nanometer material；Functional modification body therein uses water solublity mercaptides organic molecule, comprises polymerisable carbon-carbon double bond, such as allyl sulfhydrate in small molecule structure.
The dissolving of embodiment 4, hydrophilic monomer, initiator and accelerator.
Weigh and account for the hydrophilic monomer of noble metal nanometer material dispersion liquid (use granule-morphology dispersion liquid) gross mass 16%, account for the initiator of noble metal nanometer material dispersion liquid gross mass 0.4% and account for the accelerator of noble metal nanometer material dispersion liquid gross mass 0.0004 and join in embodiment 3 gained solution, it is sufficiently stirred for and ultrasonic mixing about 20min is to fully dissolving, it is passed through nitrogen 10min, in vacuum desiccator, then removes the gas dissolved in solution；Hydrophilic monomer therein is acrylamide, and initiator uses Ammonium persulfate., and accelerator uses tetramethylethylenediamine.
The preparation of embodiment 5, photo-thermal induction selfreparing noble metal nano composite aquogel.
Prepared by embodiment 4 mixed solution prepolymerization 2h in the water-bath of 0 DEG C, after at room temperature continue polymerization, complex after noble metal nanometer material is combined with functional modification body carries out system crosslinking as multi-functional cross-linking agent, the most additionally add cross-linking agent, after polymerized at normal temperature 48h, i.e. obtain light thermal induction self-healing, high-strength nano composite aquogel.
The structure of subject hydrogel is the network structure of a homogeneous polymerization, its mechanical strength is up to a MPa rank, elongation strain is up to more than 20 times, and in the presence of crackled, remain to show the tensile property of excellence, show the anti-notch sensitivity of uniqueness, utilizing the good light thermal property of noble metal nanometer material, hydrogel shows good self-healing performance under infrared light (808 nm) irradiates.
Foregoing description is only used as the enforceable technical scheme of the present invention and proposes, not as the single restrictive condition to its technical scheme itself.
Claims (9)
1. a photo-thermal induction selfreparing noble metal nano composite aquogel, it is characterized in that: this hydrogel is using dynamic noble metal-sulfur coordinate bond as spontaneous recovery main body, it has uniform network structure, i.e. monomer occurs homogeneous polymerization to react in the course of the polymerization process, so that this hydrogel has good draftability and intensity；It has a good anti-notch sensitive performance, during i.e. jagged in hydrogel surface or crackle, still has good tensile property；It utilizes the light thermal property that noble metal is good with the dynamic coordination key of sulfur and noble metal, shows good self-healing properties under the stimulation of iraser.
2. the preparation method of a photo-thermal induction selfreparing noble metal nano composite aquogel, it is characterised in that: the method comprises the following steps:
A, prepare noble metal nanometer material dispersion liquid: use zero dimension noble metal nano particles appearance structure dispersion liquid, one-dimensional noble metal nano wire appearance structure dispersion liquid or two-dimensional noble metal nanometer sheet appearance structure dispersion liquid；
B, the modification of noble metal nanometer material: weigh the functional modification body accounting for noble metal nanometer material dispersion liquid gross mass 0.002-0.02%, join in step A gained noble metal nanometer material dispersion liquid, it is sufficiently stirred for and ultrasonic mixing 10-30min, obtains surface-functionalized noble metal nanometer material；
The dissolving of C, hydrophilic monomer, initiator and accelerator: weigh and account for the hydrophilic monomer of noble metal nanometer material dispersion liquid gross mass 10-20%, account for the initiator of noble metal nanometer material dispersion liquid gross mass 0.1-0.5% and account for the accelerator of noble metal nanometer material dispersion liquid gross mass 0.0001-0.001% and join in step B gained solution, it is sufficiently stirred for and ultrasonic mixing 10-30min is to fully dissolving, it is passed through nitrogen 5-15min, in vacuum desiccator, then removes the gas dissolved in solution；
D, the preparation of hydrogel: by the mixed solution of step C prepolymerization 1-3h in the water-bath of 0 DEG C, after at room temperature continue polyase 13 0-60h, obtain light thermal induction self-healing, high-strength nano composite aquogel.
The preparation method of photo-thermal the most according to claim 2 induction selfreparing noble metal nano composite aquogel, it is characterized in that: in step A, the preparation method of noble metal nano particles dispersion liquid is: preparation solution 1:0.3-6 mmol/L noble metal salt aqueous solution and solution 2:40-800 mmol/L trisodium citrate aqueous solution respectively, then take 40-60 mL solution 1 and be heated to boiling, then take 0.5-1.5
ML solution 2 joins in solution 1 holding boiling reaction 3-7min, i.e. obtains noble metal through distilled water and ethanol centrifuge washing and receive particle dispersion after natural cooling.
The preparation method of photo-thermal the most according to claim 2 induction selfreparing noble metal nano composite aquogel, it is characterized in that: in step A, the preparation method of noble metal nano wire dispersion liquid is: take 0.05-0.2 g precious metal salt and 8-12 mL oleyl amine ultrasonic mix homogeneously in 1mL n-hexane, it is heated to 80-900 DEG C the most under nitrogen atmosphere and is stirred vigorously 5-15min, then under the conditions of 80-90 DEG C, stand 3-7h, take out solution after room temperature cooling, then use volume ratio acetone: the mixed solvent centrifuge washing of ethanol=1:3 i.e. obtains noble metal nano wire dispersion liquid.
The preparation method of photo-thermal the most according to claim 2 induction selfreparing noble metal nano composite aquogel, it is characterized in that: in step A, the preparation method of noble metal nano-plate dispersion liquid is: joined by 0.02-0.2 mol/L noble metal salt aqueous solution 1 mL in the polytetrafluoroethylcontainer container of 10-20 mL ethylene glycol, and add 0.01-0.1 g polyvinylpyrrolidone and 0.05-0.5g glucose, continuously stirred 3-7min, then reaction vessel is put in microwave reactor, reaction 10-30min, noble metal nano-plate dispersion liquid is i.e. obtained with distilled water and ethanol centrifuge washing after natural cooling.
The preparation method of photo-thermal the most according to claim 2 induction selfreparing noble metal nano composite aquogel, it is characterized in that: in step A, described precious metal salt is the soluble precursor of synthesis noble metal nanometer material, and described noble metal uses one or several mixing in gold, silver, copper, platinum.
The preparation method of photo-thermal the most according to claim 2 induction selfreparing noble metal nano composite aquogel, it is characterized in that: in step B, described functional modification body uses water solublity mercaptides organic molecule, comprises polymerisable carbon-carbon double bond in small molecule structure therein.
The preparation method of photo-thermal the most according to claim 2 induction selfreparing noble metal nano composite aquogel, it is characterised in that: in step C, described hydrophilic monomer is acrylamide, N, N dimethyl acrylamide or acrylic acid；Described initiator is the persulfate derivant including Ammonium persulfate., potassium peroxydisulfate；Described accelerator is tetramethylethylenediamine.
The preparation method of photo-thermal the most according to claim 2 induction selfreparing noble metal nano composite aquogel, it is characterized in that: in the preparation process of step D, complex after noble metal nanometer material is combined with functional modification body carries out system crosslinking as multi-functional cross-linking agent, the most additionally adds cross-linking agent.
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