CN103588931B - Two in-situ synthetic methods of temperature-responsive nano silver composite hydrogel - Google Patents
Two in-situ synthetic methods of temperature-responsive nano silver composite hydrogel Download PDFInfo
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Abstract
The present invention relates to a kind of two in-situ synthetic methods of temperature-responsive nano silver composite hydrogel.The present invention adopts uv-radiation method, when not adding initiator and reductive agent, with dimethylaminoethyl methacrylate and 2-acrylamide-2-methylpro panesulfonic acid for monomer, N, N '-methylene-bisacrylamide is linking agent, poly(oxyethylene glycol) 400 is pore former, and Silver Nitrate is source metal, has synthesized temperature-responsive nanometer Ag/P (DMAEMA-g-AMPS) composite aquogel under nitrogen atmosphere.The nano silver particles of nano silver composite hydrogel prepared by the present invention is uniformly dispersed, chemically crosslinked good stability, and swelling capacity increases 294.8 than pure water gel, improves water-absorbent and the water-retentivity of hydrogel; Temperature-responsive strengthens, and is beneficial to the application such as medical medicine release; Heat decomposition temperature reduces 78 DEG C than pure water gel, is beneficial to the discarded aftertreatment of polymkeric substance.
Description
Technical field
The invention belongs to technological field of biochemistry, be specifically related to a kind of two in-situ synthetic methods of temperature-responsive nano silver composite hydrogel.
Background technology
Dimethylaminoethyl methacrylate is typical temperature sensitive monomer, and 2-acrylamide-2-methylpro panesulfonic acid is hydrophilic monomer, although the copolymer hydrogel of the two improves the swelling capacity of hydrogel, is deteriorated to the responsiveness of temperature.Nano silver particles can with the Sauerstoffatom of monomer amide group, nitrogen-atoms generation coordination, and three-dimensional netted polymeric matrix provides cyberspace for nano silver particles, silver not only can improve swelling capacity as cross-linking set, can also improve temperature-responsive, therefore the nano silver composite hydrogel of synthesis temperature responsiveness is a kind of material having prospect.But nano silver particles is large due to specific surface area, very easily reunites, makes it be difficult to mix with other material, limit the application of nanometer silver.At present, the main method preparing nano silver composite hydrogel Ag/P (DMAEMA-g-AMPS) is: mould hybrid system, reductive agent method, gamma Rays method.But there is synthetic product structural instability, silver particles skewness, impurity are difficult or synthetic method regulation and control difficulty is large, yield of radiation crosses high defect.The present invention adopt a kind of green, energy-conservation and environmental protection temperature-responsive nanometer Ag/P (DMAEMA-g-AMPS) composite aquogel prepared of uv-radiation method.
Summary of the invention
In order to solve the deficiency that above-mentioned prior art exists, the invention provides two in-situ synthetic methods of temperature-responsive nano silver composite hydrogel of a kind of green, energy-conserving and environment-protective.
Concrete technical scheme of the present invention is as follows:
Two in-situ synthetic methods of temperature-responsive nano silver composite hydrogel: adopt uv-radiation method, when not adding initiator and reductive agent, with dimethylaminoethyl methacrylate and 2-acrylamide-2-methylpro panesulfonic acid for monomer, N, N '-methylene-bisacrylamide is linking agent, poly(oxyethylene glycol) 400 is pore former, Silver Nitrate is source metal, temperature-responsive nano silver composite hydrogel has been synthesized under nitrogen atmosphere, described nano silver composite hydrogel macroscopic view presents beige g., jelly-like, microcosmic presents three-dimensional lamella reticulated structure, nano silver particles be evenly distributed and size within 50nm scope, this nano silver composite hydrogel swelling ratio is 336.29, minimum transformation temperature is 80 DEG C, heat decomposition temperature is 175 DEG C.
The concrete operation step of two fabricated in situ of temperature-responsive nano silver composite hydrogel is as follows:
1) in the four-hole boiling flask with inlet pipe and vapor pipe, add temperature sensitive monomer, hydrophilic monomer, linking agent, pore former and distilled water successively, each material to add quality as follows: 808ul temperature sensitive monomer, 1.0g hydrophilic monomer, 0.0088g linking agent, 346ul pore former, 10ml distilled water; Be fixed on by four-hole boiling flask in heating jacket, control temperature is 25 ~ 30 DEG C; Described temperature sensitive monomer is dimethylaminoethyl methacrylate, and described hydrophilic monomer is 2-acrylamide-2-methylpro panesulfonic acid, and described linking agent is N, N '-methylene-bisacrylamide, described pore former is poly(oxyethylene glycol) 400;
2) two other mouthful of place respectively fixed thermometer and the drop funnel of the four-hole boiling flask of material will be housed, wherein add silver nitrate solution in drop funnel, described silver nitrate solution by 0.8154g Silver Nitrate and 5ml distilled water formulated;
3) described inlet pipe is connected nitrogen bag and pass into nitrogen; vapor pipe exhaust 15min; then close vapor pipe, under nitrogen protection condition, drop funnel of outwarding winding drips silver nitrate solution; uv-radiation 10min simultaneously; take out nano silver composite hydrogel head product, with distilled water immersion, every 2h changes first water; repeat at least 20 times, obtain temperature-responsive nano silver composite hydrogel.
The mole number of described temperature sensitive monomer, the mole number of hydrophilic monomer are identical with the mole number of Silver Nitrate.
Linking agent N, N '-methylene-bisacrylamide accounts for 0.5% of monomer total mass, and described monomer total mass is the quality of temperature sensitive monomer and the quality sum of hydrophilic monomer.
Pore former poly(oxyethylene glycol) 400 is 10% of the total amount of substance of monomer, and the total amount of substance of described monomer is the mole number of temperature sensitive monomer and the mole number sum of hydrophilic monomer.
The liquid droping speed of drop funnel is 12/min.
The processing condition of uv-radiation are intensity 400mW/cm
2, wavelength 340nm, average output power 2000W, radiated time 10min.
Advantageous Effects of the present invention embodies in the following areas:
1. the temperature-responsive nano silver composite hydrogel that prepared by the present invention has the following advantages: the nanometer silver in (1) temperature-responsive nano silver composite hydrogel is uniformly dispersed in three-dimensional netted polymeric matrix, and particle diameter is within 50nm scope.(2) swelling capacity of temperature-responsive nano silver composite hydrogel is higher than pure water gel, increases 294.8, improves water-absorbent and the water-retentivity of hydrogel.(3) the minimum transformation temperature (LCST) of temperature-responsive nano silver composite hydrogel is 80 DEG C, same with pure water gel phase, but temperature-responsive strengthens, and is beneficial to the application such as medical medicine release.(4) heat decomposition temperature of temperature-responsive nano silver composite hydrogel is lower than pure water gel, reduces 78 DEG C, is beneficial to the discarded aftertreatment of polymkeric substance;
2. the method for the two fabricated in situ temperature-responsive nano silver composite hydrogel of uv-radiation method of the present invention is a kind of method of green, energy-conservation and environmental protection, productive rate and the distributive law of nano silver particles can be regulated and controled by the drop velocity of regulator solution water clock bucket and uv-radiation parameter, by regulating the ratio between monomer can regulate and control water-intake rate and temperature-responsive, be a kind of preparation method of convenient easy control.Experiment reaction conditions is simple, only needs a ultraviolet lamp, does not need other large-scale experiment equipment, be applicable to carrying out suitability for industrialized production.
Accompanying drawing explanation
Fig. 1 is the infrared spectrum of P (DMAEMA-g-AMPS) composite aquogel and nanometer Ag/P (DMAEMA-g-AMPS) composite aquogel.
Fig. 2 is the XRD spectra of nanometer Ag/P (DMAEMA-g-AMPS) composite aquogel.
Fig. 3 is the stereoscan photograph of P (DMAEMA-g-AMPS) composite aquogel and nanometer Ag/P (DMAEMA-g-AMPS) composite aquogel.
Fig. 4 is the transmission electron microscope photo of nanometer Ag/P (DMAEMA-g-AMPS) composite aquogel.
Fig. 5 is the swelling dynamic curve of P (DMAEMA-g-AMPS) composite aquogel and nanometer Ag/P (DMAEMA-g-AMPS) composite aquogel.
Fig. 6 is the temperature response curve of P (DMAEMA-g-AMPS) composite aquogel and nanometer Ag/P (DMAEMA-g-AMPS) composite aquogel.
Fig. 7 is the DSC spectrogram of P (DMAEMA-g-AMPS) composite aquogel and nanometer Ag/P (DMAEMA-g-AMPS) composite aquogel.
Fig. 8 is the thermogravimetric spectrogram of P (DMAEMA-g-AMPS) composite aquogel and nanometer Ag/P (DMAEMA-g-AMPS) composite aquogel.
Embodiment
Below in conjunction with embodiment, the present invention is further described.
The required equipment of reaction:
Four-hole boiling flask, there-necked flask, thermometer, nitrogen bag, heating jacket, microsyringe, UV-A340 ultra-violet lamp, vacuum drying oven, freeze drying box.
The source of raw material:
Monomer: dimethylaminoethyl methacrylate (DMAEMA), 99%, the brilliant pure reagent company limited in Shanghai; 2-acrylamide-2-methylpro panesulfonic acid (AMPS), 98%, the brilliant pure reagent company limited in Shanghai;
Linking agent: N, N '-methylene-bisacrylamide (BIS), 97%, CP, the brilliant pure reagent company limited in Shanghai;
Pore former: poly(oxyethylene glycol) 400 (PEG), Wuxi City Ya Wei Chemical Co., Ltd.;
Silver source: Silver Nitrate (AgNO
3), AR, Shanghai Shen Bo Chemical Co., Ltd..
embodiment 1
The concrete operation step of two in-situ synthetic methods of temperature-responsive nano silver composite hydrogel is as follows:
1) measure the dimethylaminoethyl methacrylate of 808ul, weigh the 2-acrylamide-2-methylpro panesulfonic acid of 1.0g, the N of 0.0088g, N '-methylene-bisacrylamide, measure 346ul poly(oxyethylene glycol) 400,10ml distilled water joins in four-hole boiling flask successively, is uniformly dissolved;
2) thermometer, drop funnel, nitrogen tube, vapor pipe on fixing four-hole boiling flask, be then fixed on four-hole boiling flask in the heating jacket of 30 DEG C;
3) a bite of four-hole boiling flask passes into nitrogen, flatly exhaust, and lasting 15min guarantees that air is divided, then closed exhaust pipe, and continuing nitrogen is protected;
4) in drop funnel, 0.8154g Silver Nitrate and 5ml distilled water is added;
5) utilize UV-A340 ultra-violet lamp radiation four-hole boiling flask, control drop funnel liquid droping speed 12/min, the processing condition of uv-radiation are intensity 400mW/cm
2, wavelength 340nm, average output power 2000W, radiated time 10min;
6), after reaction terminates, sample presents brown g., jelly-like.Add a large amount of distilled water immersion, every 2h changes first water, obtains temperature-responsive nano silver composite hydrogel after repeating at least 20 times.Be cut into bulk and carry out vacuum-drying, lyophilize, characterize stand-by.
See Fig. 1, curve b and a compares, the position of C-N stretching vibration peak blue shift 7cm respectively in the stretching vibration peak (amide Ⅰ) of secondary amide C=O and amide group
-1and 19cm
-1.This is because in nano silver particles and polymkeric substance on amide group Sauerstoffatom and nitrogen-atoms there is coordination, the electronics in nanometer silver shifts to amide group.Illustrate to there is coordination between nano silver particles and polymkeric substance, chemically composited stable.
See Fig. 2, in 2 θ=38.32 °, 44.23 °, 64.48 °, 77.48 ° place's appearance, four obvious diffraction peaks, on contrast JCPDS card 04-0783 silver-colored simple substance base peak position data (2 θ are 38. 096 °, 44. 257 °, 64. 406 °, 77. 452 °), experimental data is basically identical with it, correspond respectively to (111), (200), (220) of isometric system silver, (311) crystal face, the pure metallic silver simple substance containing isometric system in interpret sample.And diffraction peak is relatively more sharp-pointed, illustrate that the crystal property of middle silver-colored simple substance prepared by uv-radiation reduction Silver Nitrate is good.
Obviously see that spherical particle is dispersed in the three-dimensional network of hydrogel see Fig. 3, Fig. 3 b, distribute comparatively even.
See Fig. 4, can see that silver particles is coated in polymkeric substance with the form of spheroid, and be uniformly dispersed.This is because silver ions the Sauerstoffatom of amide group and nitrogen-atoms may be combined by weak electrostatic interaction in the hydrogel network chain existed, formation O-Ag
+and N-Ag
+type coordinate bond.Fig. 4 a can obviously find out three-dimensional netted polymkeric substance also present one interesting spherical greatly.Fig. 4 b obviously can find out that the particle diameter of silver particles is all at below 50nm, proves that uv-radiation obtains silver particles and meets Nano grade.
See Fig. 5, the swelling ratio of curve b is 336.29.This is because N, N '-dimethylaminoethyl is not only a hydrophobic grouping, or the Hydrogen Bond Acceptors that is very strong.Silver is as cross-linking set, add the side chain node of polymkeric substance, coordination can be formed with Sauerstoffatom, nitrogen-atoms in amide group, the more difficult generation of macromolecular chain relaxes, the effect of hydrogen bond is obvious, water strengthens to the diffusion in gel network structure, causes the wetting ability of nano silver composite hydrogel to strengthen, higher than the swelling behavior degree of not adding nano-Ag particles.
See Fig. 6, the equilibrium swelling ratio (ESR) of curve b is all reduce along with the increase of temperature, illustrates that hydrogel has temperature-responsive.This is because the N in monomer DMAEMA, N '-dimethylaminoethyl is not only a hydrophobic grouping, or the Hydrogen Bond Acceptors that very strong.When temperature is low, hydrogen bond action accounts for leading, and the higher hydrogen bond action of temperature weakens and hydrophobicity strengthens.Experimental temperature is from 30 DEG C of tests to 80 DEG C, and the ESR of the two reduces gradually, all declines rapidly when at 75 DEG C.But it is strong 75 DEG C of downtrendings that curve b shows nano silver composite hydrogel, although illustrate that the compound of silver particles does not affect the minimum transformation temperature (LCST) of hydrogel, considerably increases the temperature-responsive of hydrogel.
See Fig. 7, the minimum transformation temperature (LCST) that curve b records is 81.8 DEG C, tests with Fig. 6 the temperature close recorded.
See Fig. 8, the heat decomposition temperature of curve b nanometer Ag/P (DMAEMA-g-AMPS) composite aquogel is 175 DEG C.This wherein weightless composition is polymkeric substance and P (DMAEMA-g-AMPS).Due to the compound of nanometer silver, the heat decomposition temperature of polymkeric substance reduces, this is because silver has the effect of catalytic polymer thermolysis.
embodiment 2
The concrete operation step of two in-situ synthetic methods of temperature-responsive composite aquogel is as follows:
1) measure the dimethylaminoethyl methacrylate of 808ul, weigh the 2-acrylamide-2-methylpro panesulfonic acid of 1.0g, the N of 0.0088g, N '-methylene-bisacrylamide, measure 346ul poly(oxyethylene glycol) 400,15ml distilled water joins in there-necked flask successively, is uniformly dissolved;
2) thermometer, nitrogen tube, vapor pipe on fixing there-necked flask, be then fixed on there-necked flask in the heating jacket of 30 DEG C;
3) a bite of there-necked flask passes into nitrogen, flatly exhaust, and lasting 15min guarantees that air is divided, then closed exhaust pipe, and continuing nitrogen is protected;
Utilize UV-A340 ultra-violet lamp radiation there-necked flask, the processing condition of uv-radiation are intensity 400mW/cm
2, wavelength 340nm, average output power 2000W, radiated time 10min;
After reaction terminates, sample presents transparent g., jelly-like.Add a large amount of distilled water immersion, every 2h changes first water, obtains temperature-responsive composite aquogel after repeating at least 20 times.Be cut into bulk and carry out vacuum-drying, lyophilize, characterize stand-by.
See Fig. 1, on curve a, known 3438cm
-1the stretching vibration peak of the N-H of lactan, 2924cm
-13 neighbouring peaks are the stretching vibration peak of C-H, at 1731cm
-1and 1162cm
-1there is the absorption peak (C=O stretching vibration and C-O stretching vibration) of ester group in place, 1640cm
-1for the stretching vibration peak of secondary amide C=O, 1554cm
-1the flexural vibration peak of secondary amide N-H, 1468cm
-1the flexural vibration peak of C-H in-CH2-, at 1390cm
-1near there is tertiary amine groups absorption peak, 1188cm
-1c-N stretching vibration peak in acid amides, 1162cm
-1for S=O symmetrical stretching vibration peak, these peaks and position and standard spectrogram basically identical.1637cm in the stretching vibration absorption peak of unsaturated double-bond and DMAEMA
-1the 1613cm of place and AMPS
-1disappear, this shows that sample is polymerized polymer network completely, does not have unreacted monomer small molecules.
Can find out see Fig. 3, Fig. 3 a, this sample presents the three-dimensional net structure of lamella mesh, compound with regular structure.
See Fig. 5, curve a can find out that the swelling ratio of hydrogel is 41.49, well below nano silver composite hydrogel.
See Fig. 6, curve a can find out that equilibrium swelling ratio (ESR) is all reduce along with the increase of temperature, illustrates that hydrogel has temperature-responsive.To record minimum transformation temperature (LCST) be 75 DEG C in experiment, but fall is very low, to the responsiveness of temperature well below nano silver composite hydrogel.
See Fig. 7, it is 78.4 DEG C that curve a records minimum transformation temperature (LCST), tests with Fig. 6 the temperature close recorded.
See Fig. 8, the heat decomposition temperature that curve a records P (DMAEMA-g-AMPS) hydrogel is 253 DEG C.
Claims (6)
1. two in-situ synthetic methods of temperature-responsive nano silver composite hydrogel, it is characterized in that: adopt uv-radiation method, when not adding initiator and reductive agent, with dimethylaminoethyl methacrylate and 2-acrylamide-2-methylpro panesulfonic acid for monomer, N, N '-methylene-bisacrylamide is linking agent, poly(oxyethylene glycol) 400 is pore former, Silver Nitrate is source metal, temperature-responsive nano silver composite hydrogel has been synthesized under nitrogen atmosphere, described nano silver composite hydrogel macroscopic view presents beige g., jelly-like, microcosmic presents three-dimensional lamella reticulated structure, nano silver particles be evenly distributed and size within 50nm scope, this nano silver composite hydrogel swelling ratio is 336.29, minimum transformation temperature is 80 DEG C, heat decomposition temperature is 175 DEG C,
Concrete operation step is as follows: 1) in the four-hole boiling flask with inlet pipe and vapor pipe, add temperature sensitive monomer, hydrophilic monomer, linking agent, pore former and distilled water successively, each material to add quality as follows: 808ul temperature sensitive monomer, 1.0g hydrophilic monomer, 0.0088g linking agent, 346ul pore former, 10ml distilled water; Be fixed on by four-hole boiling flask in heating jacket, control temperature is 25 ~ 30 DEG C; Described temperature sensitive monomer is dimethylaminoethyl methacrylate, and described hydrophilic monomer is 2-acrylamide-2-methylpro panesulfonic acid, and described linking agent is N, N '-methylene-bisacrylamide, described pore former is poly(oxyethylene glycol) 400; 2) two other mouthful of place respectively fixed thermometer and the drop funnel of the four-hole boiling flask of material will be housed, wherein add silver nitrate solution in drop funnel, described silver nitrate solution by 0.8154g Silver Nitrate and 5ml distilled water formulated; 3) described inlet pipe is connected nitrogen bag and pass into nitrogen; vapor pipe exhaust 15min; then close vapor pipe, under nitrogen protection condition, drop funnel of outwarding winding drips silver nitrate solution; uv-radiation 10min simultaneously; take out nano silver composite hydrogel head product, with distilled water immersion, every 2h changes first water; repeat at least 20 times, obtain temperature-responsive nano silver composite hydrogel.
2. two in-situ synthetic methods of nano silver composite hydrogel according to claim 1, is characterized in that: the mole number of described temperature sensitive monomer, the mole number of hydrophilic monomer are identical with the mole number of Silver Nitrate.
3. two in-situ synthetic methods of nano silver composite hydrogel according to claim 1, it is characterized in that: linking agent N, N '-methylene-bisacrylamide accounts for 0.5% of monomer total mass, and described monomer total mass is the quality of temperature sensitive monomer and the quality sum of hydrophilic monomer.
4. two in-situ synthetic methods of nano silver composite hydrogel according to claim 1, it is characterized in that: pore former poly(oxyethylene glycol) 400 is 10% of the total amount of substance of monomer, the total amount of substance of described monomer is the mole number of temperature sensitive monomer and the mole number sum of hydrophilic monomer.
5. two in-situ synthetic methods of nano silver composite hydrogel according to claim 1, is characterized in that: the liquid droping speed of drop funnel is 12/min.
6. two in-situ synthetic methods of nano silver composite hydrogel according to claim 1, is characterized in that: the processing condition of uv-radiation are intensity 400mW/cm
2, wavelength 340nm, average output power 2000W, radiated time 10min.
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| CN102432974A (en) * | 2011-09-05 | 2012-05-02 | 同济大学 | Polymer vesica with antibacterial nano silver deposited on surface and preparation method thereof |
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| CN102226029A (en) * | 2011-04-28 | 2011-10-26 | 东华大学 | Preparation method of temperature responsive nanohydrogel carrying silver nanoparticles |
| CN102432974A (en) * | 2011-09-05 | 2012-05-02 | 同济大学 | Polymer vesica with antibacterial nano silver deposited on surface and preparation method thereof |
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