CN104387710A - Method for preparing microwave driving type interpenetrating network shape memory polymer - Google Patents
Method for preparing microwave driving type interpenetrating network shape memory polymer Download PDFInfo
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Abstract
The invention relates to a functional polymer material, and in particular relates to a method for preparing a microwave driving type interpenetrating network shape memory polymer. PAA (Poly Acrylic Acid) used as a cross-linking structure and PVA (Poly Vinyl Alcohol) are interpenetrated into a cross-linking network structure and are formed into an organic/inorganic composite material together with SiC. SiC which has a good absorption property on microwaves is modified by a silane coupling agent with double bonds at one end, so that the double bonds are introduced into the surfaces of inorganic particles, and monomers are initiated to polymerize on the surfaces. AA is cross-linked to form a network structure in a PVA solution in which modified SiC is dispersed by using a bisacrylamide cross-linking agent for in-situ polymerization, and thus the polymer network (PVA/PAA) nano composite material with interpenetrated PVA and PAA is prepared. The composite material provided by the invention is good in shape memory property, does not need to be preheated in the recovery process, and is short in response time and fast in recovery speed.
Description
Technical field
The present invention relates to a kind of functional high molecule material, particularly the preparation method of microwave-driven type interpenetrating(polymer)networks shape-memory polymer.
Background technology
The shape memory effect of shape-memory polymer (SMPs) is embodied in: after to the sample of figuration, (as temperature, light, moisture etc.) implement distortion under certain condition, this temporary shapes can be kept, when again heating material, illumination or other is when stimulating, sample can be returned to initial state again.
Current research more and obtained large-scale application mainly adopt direct heat source as the thermotropic SMPs of stimulation mode.But this mode in actual applications may be inconvenient or bring other bad problems, during as being used on medical material, when required transition temperature is higher than human body temperature, this too high and destroy tissue by thermograde heat exchange pattern Hui Shi local heating temperature from outside to inside.But other special external stimuluss such as infrared, laser and electromagnetic field were all once used as indirect heating source, they to the chemical constitution of SMPs and drive condition more harsh.Therefore, we propose the response stimulus that adopts this efficient, energy-conservation, timesaving type of drive of microwave as deformation recovery.
Although there is the SM-PVA of some water moleculess to have fast response time, response rate advantages of higher under microwave-driven, a small amount of water molecules of polymeric matrix inside obviously can reduce the mechanical strength of material.In addition, when material leaves the unstable easily volatilization of these water moleculess in the environment of relatively dry in, thus its shape memory effect cannot be embodied.
Summary of the invention
Technical problem to be solved by this invention is: how to introduce the stimuli responsive source that deformation recovery occurs a kind of made SMCs newly, and provide a kind of responding microwave type shape memory polymer composite material with interpenetrating polymer networks structure and preparation method thereof.
The technical solution adopted in the present invention is: the preparation method of microwave-driven type interpenetrating(polymer)networks shape-memory polymer, carries out according to following step:
Step one, the nanometer silicon carbide SiC after vacuum heat treatment is added in toluene, be warmed up to 30 ~ 100 DEG C, add the silanization coupling agent of SiC quality 1 ~ 10 %, stirring reaction 1 ~ 12h, product is vacuum filtration while hot, and successively with acetone and deionized water wash, centrifugation is then dry, obtain modified Nano SiC, then modified Nano SiC is scattered in water obtains the SiC dispersion liquid that mass content is 1 ~ 8 %;
Step 2, be 500 ~ 2400 by the polymerization degree, the alcoholysis degree PVAC polyvinylalcohol that is greater than 80% is dissolved in water that to obtain mass percent be 3 ~ 15 %PVA aqueous solution;
Step 3, mass ratio by SiC: PVA=1 ~ 10: 100, SiC dispersion liquid step one prepared joins step 2 and prepares in the PVA aqueous solution, stirs 0.5 ~ 1.5h;
Step 4, the AA adding PVA quality 20 ~ 80% successively, linking agent, initiator, 20 ~ 95 DEG C of crosslinking reaction 2 ~ 8h, obtain responding microwave type PVA/PAA interpenetrating polymer networks composite material of shape memory.
As a kind of optimal way: the silanization coupling agent in step one is any one in 3-(iso-butylene acyl-oxygen) propyl trimethoxy silicane, vinyltriethoxysilane, vinyltrimethoxy silane, vinyl three ('beta '-methoxy oxyethyl group) silane.
As a kind of optimal way: the reaction process of step one is carried out under nitrogen protection.
As a kind of optimal way: the linking agent in step 4 is the MBA of AA quality 0.5 ~ 3 wt%, initiator is the K of AA quality 0.5 ~ 3 wt%
2s
2o
8.
As a kind of optimal way: the vacuum heat treatment in step one refers to nano SiC vacuum heat treatment 24 h at 120 DEG C.
The invention has the beneficial effects as follows: the responding microwave type PVA/PAA interpenetrating polymer networks composite material of shape memory Recovery Process of this law manufacture does not need preheating, time of response is short, reply speed fast (then can complete in several seconds soon), there is the advantages such as efficient, energy-conservation, clean, also can realize remote control.
Accompanying drawing explanation
Fig. 1 nano SiC before modified after infrared spectra contrast figure.
The different SiC content of Fig. 2 is on the impact of SMCs dielectric properties.
The DSC curve of the different SiC content SMCs of Fig. 3.
The different SiC content SMCs storage modulus of Fig. 4 and temperature relation
The shape memory effect of the different SiC content SMCs of Fig. 5 under 400 W microwave exposures.
The shape memory effect of Fig. 6 SMCs under different microwave output power.
The thermogravimetric curve of Fig. 7 SMCs after different microwave exposure cycle index.
Embodiment
Embodiment 1
Get nano SiC 10g, vacuum heat treatment 24 h at 120 DEG C.Getting SiC micro mist 5 g after process adds in 50 ml toluene; be warming up to 50 DEG C and stir 1 h; drip 0.1g KH570 (whole process nitrogen protection); stir 5 h; product is vacuum filtration while hot; successively with acetone and deionized water wash, centrifugal and in 105 DEG C of baking ovens dry 12 h, obtain Modified SiC Powder.
Getting the 5 g polymerization degree is 1700, alcoholysis degree be 99% PVA add in 100 ml water, at 100 DEG C, dissolve 2.5 h, obtain the 5%PVA aqueous solution.
2 g modification SiC are dispersed in 50 ml water, get its 3 ml and be mixed in 100 ml polyvinyl alcohol water solutions, after stirring 1 h, add AA1.5 g, then MBA, K successively
2s
2o
8each 0.015 g.50 DEG C of crosslinking reaction 2 h., mixed solution is injected double glazing pipe that internal diameter is about 5mm and carries out into clubs and do; The mixed solution (guarantee does not have bubble as far as possible) measuring 6 mL injects the Teflon mould film forming of definite shape.Take out after all samples being put into refrigerator freezing 24 h, wherein rod-like samples need soak 12 h(and cements out to make the water molecules in sample in proper amount of methanol solution).All samples at room temperature dries naturally subsequently.
In order to the macroshape observing SMCs replys behavior, by there is original shape sample under the microwave of 200 W after irradiation 120 s under external force figuration, treat that sample is cooled to Room-temperature Shape and is fixed.Under the microwave exposure of 300 W, observe deformation recovery process, and adopt bending method to carry out quantitative test to shape-memory properties.Thermal stability test is carried out through the SMCs of different cycle index under microwave exposure.
Embodiment 2
Get nano SiC 10 g, vacuum heat treatment 24 h at 120 DEG C.Getting SiC micro mist 5 g after process adds in 50 ml toluene; be warming up to 60 DEG C and stir 2 h; drip 0.25 g A151 (whole process nitrogen protection); stir 5 h; product is vacuum filtration while hot; successively with acetone and deionized water wash, centrifugal and in 105 DEG C of baking ovens dry 12 h, obtain Modified SiC Powder.
Getting the 8 g polymerization degree is 500, alcoholysis degree be 88% PVA add in 100 ml water, at 100 DEG C, dissolve 2.5 h, obtain the 8% PVA aqueous solution.
2g modification SiC is dispersed in 50 ml water, gets its 10 ml and be mixed in the 100 ml PVA aqueous solution, after stirring 1.5 h, add AA2.4 g, then MBA, K successively
2s
2o
8each 0.048 g.60 DEG C of crosslinking reaction 2 h., mixed solution is injected double glazing pipe that internal diameter is about 5 mm and carries out into clubs and do; The mixed solution (guarantee does not have bubble as far as possible) measuring 6 mL injects the Teflon mould film forming of definite shape.Take out after all samples being put into refrigerator freezing 24 h, wherein rod-like samples need soak 12 h(and cements out to make the water molecules in sample in proper amount of methanol solution).All samples at room temperature dries naturally subsequently.
In order to the macroshape observing SMCs replys behavior, by there is original shape sample under the microwave of 200 W after irradiation 120 s under external force figuration, treat that sample is cooled to Room-temperature Shape and is fixed.Under the microwave exposure of 300 W, observe deformation recovery process, and adopt bending method to carry out quantitative test to shape-memory properties.Thermal stability test is carried out through the SMCs of different cycle index under microwave exposure.
Embodiment 3
Get nano SiC 10 g, vacuum heat treatment 24 h at 120 DEG C.Getting SiC micro mist 5 g after process adds in 50 ml toluene; be warming up to 85 DEG C and stir 1 h; drip 0.4 g A171 (whole process nitrogen protection); stir 6 h; product is vacuum filtration while hot; successively with acetone and deionized water wash, centrifugal and in 105 DEG C of baking ovens dry 12 h, obtain Modified SiC Powder.
Getting the 10 g polymerization degree is 2400, alcoholysis degree be 99% polyvinyl alcohol add in 100 ml water, at 100 DEG C, dissolve 2.5 h, obtain 10% polyvinyl alcohol water solution.
2 g modification SiC are dispersed in 50 ml water, get its 15 ml and be mixed in 100 ml polyvinyl alcohol water solutions, after stirring 1.5 h, add vinylformic acid 3.0 g, then MBA, K successively
2s
2o
8each 0.03 g.80 DEG C of crosslinking reaction 2 h., mixed solution is injected double glazing pipe that internal diameter is about 5 mm and carries out into clubs and do; The mixed solution (guarantee does not have bubble as far as possible) measuring 6 ml injects the Teflon mould film forming of definite shape.Take out after all samples being put into refrigerator freezing 24 h, wherein rod-like samples need soak 12 h(and cements out to make the water molecules in sample in proper amount of methanol solution).All samples at room temperature dries naturally subsequently.
In order to the macroshape observing SMCs replys behavior, by there is original shape sample under the microwave of 500W after irradiation 30s under external force figuration, treat that sample is cooled to Room-temperature Shape and is fixed.Under the microwave exposure of 400W, observe deformation recovery process, and adopt bending method to carry out quantitative test to shape-memory properties.Thermal stability test is carried out through the SMCs of different cycle index under microwave exposure.
Embodiment 4
Get nano SiC 10 g, vacuum heat treatment 12 h at 120 DEG C.Getting SiC micro mist 5 g after process adds in 50 ml toluene; be warming up to 85 DEG C and stir 1 h; drip 0.3 g K H570 (whole process nitrogen protection); stir 5 h; product is vacuum filtration while hot; successively with acetone and deionized water wash, centrifugal and in 105 DEG C of baking ovens dry 12 h, obtain Modified SiC Powder.
Getting the 8 g polymerization degree is 2400, alcoholysis degree be 99% polyvinyl alcohol add in 100 ml water, at 100 DEG C, dissolve 2.5 h, obtain 10% polyvinyl alcohol water solution.
2 g modification SiC are dispersed in 50 ml water, get its 15 ml and be mixed in 100 ml polyvinyl alcohol water solutions, after stirring 1 h, add vinylformic acid 4.0 g, then MBA, K successively
2s
2o
8each 0.02 g.80 DEG C of crosslinking reaction 3 h., mixed solution is injected double glazing pipe that internal diameter is about 5 mm and carries out into clubs and do; The mixed solution (guarantee does not have bubble as far as possible) measuring 6 ml injects the Teflon mould film forming of definite shape.Take out after all samples being put into refrigerator freezing 24 h, wherein rod-like samples need soak 12 h(and cements out to make the water molecules in sample in proper amount of methanol solution).All samples at room temperature dries naturally subsequently.
In order to the macroshape observing SMCs replys behavior, by there is original shape sample under the microwave of 300W after irradiation 60 s under external force figuration, treat that sample is cooled to Room-temperature Shape and is fixed.Under the microwave exposure of 400 W, observe deformation recovery process, and adopt bending method to carry out quantitative test to shape-memory properties.Thermal stability test is carried out through the SMCs of different cycle index under microwave exposure.
Embodiment 5
Get nano SiC 10 g, vacuum heat treatment 12 h at 120 DEG C.Getting SiC micro mist 5 g after process adds in 50 ml toluene; be warming up to 85 DEG C and stir 1 h; drip 0.3 g A151 (whole process nitrogen protection); stir 8 h; product is vacuum filtration while hot; successively with acetone and deionized water wash, centrifugal and in 105 DEG C of baking ovens dry 12 h, obtain Modified SiC Powder.
Getting the 15 g polymerization degree is 1700, alcoholysis degree be 85% polyvinyl alcohol add in 100 ml water, at 100 DEG C, dissolve 2.5 h, obtain 15% polyvinyl alcohol water solution.
2 g modification SiC are dispersed in 50 ml water, get its 15 ml and be mixed in 100 ml polyvinyl alcohol water solutions, after stirring 1.5 h, add vinylformic acid 9.0 g, then MBA, K successively
2s
2o
8each 0.27 g.80 DEG C of crosslinking reaction 6 h., mixed solution is injected double glazing pipe that internal diameter is about 5 mm and carries out into clubs and do; The mixed solution (guarantee does not have bubble as far as possible) measuring 6 ml injects the box of the tetrafluoroethylene of definite shape, carries out Film forming operations.Take out after all samples being put into refrigerator freezing 24 h, wherein rod-like samples need soak 12 h(and cements out to make the water molecules in sample in proper amount of methanol solution).All samples at room temperature dries naturally subsequently.
In order to the macroshape observing SMCs replys behavior, by there is original shape sample under the microwave of 500W after irradiation 20 s under external force figuration, treat that sample is cooled to Room-temperature Shape and is fixed.Under the microwave exposure of 500 W, observe deformation recovery process, and adopt bending method to carry out quantitative test to shape-memory properties.Thermal stability test is carried out through the SMCs of different cycle index under microwave exposure.
Embodiment 6
Get nano SiC 10 g, vacuum heat treatment 24 h at 120 DEG C.Getting SiC micro mist 5 g after process adds in 50 ml toluene; be warming up to 70 DEG C and stir 1 h; drip 0.5 g K H570 (whole process nitrogen protection); stir 6 h; product is vacuum filtration while hot; successively with acetone and deionized water wash, centrifugal and in 105 DEG C of baking ovens dry 12 h, obtain Modified SiC Powder.
Getting the 8 g polymerization degree is 1700, alcoholysis degree be 88% polyvinyl alcohol add in 100 ml water, at 100 DEG C, dissolve 2.5 h, obtain 8% polyvinyl alcohol water solution.
2 g modification SiC are dispersed in 50 ml water, get its 8 ml and be mixed in 100 ml polyvinyl alcohol water solutions, after stirring 0.5 h, add vinylformic acid 6.4 g, then MBA, K successively
2s
2o
8each 0.064 g.80 DEG C of crosslinking reaction 3 h., mixed solution is injected double glazing pipe that internal diameter is about 5 mm and carries out into clubs and do; The mixed solution (guarantee does not have bubble as far as possible) measuring 6 ml injects the Teflon mould film forming of definite shape.Take out after all samples being put into refrigerator freezing 24 h, wherein rod-like samples need soak 12 h(and cements out to make the water molecules in sample in proper amount of methanol solution), all samples at room temperature dries naturally subsequently.
In order to the macroshape observing SMCs replys behavior, by there is original shape sample under the microwave of 800W after irradiation 10 s under external force figuration, treat that sample is cooled to Room-temperature Shape and is fixed.Under the microwave exposure of 800W, observe deformation recovery process, and adopt bending method to carry out quantitative test to shape-memory properties.Thermal stability test is carried out through the SMCs of different cycle index under microwave exposure.
Embodiment 7
Get nano SiC 10 g, vacuum heat treatment 24 h at 120 DEG C.Getting SiC micro mist 5 g after process adds in 50 ml toluene; be warming up to 85 DEG C and stir 1 h; drip 0.25 g A172 (whole process nitrogen protection); stir 8 h; product is vacuum filtration while hot; successively with acetone and deionized water wash, centrifugal and in 105 DEG C of baking ovens dry 12 h, obtain Modified SiC Powder.
Getting the 10 g polymerization degree is 2400, alcoholysis degree be 99% polyvinyl alcohol add in 100 ml water, at 100 DEG C, dissolve 2.5 h, obtain 10% polyvinyl alcohol water solution.
2 g modification SiC are dispersed in 50 ml water, get its 5 ml and be mixed in 100 ml polyvinyl alcohol water solutions, after stirring 0.5 h, add vinylformic acid 8 g, then MBA, K successively
2s
2o
8each 0.04 g.80 DEG C of crosslinking reaction 5 h., mixed solution is injected double glazing pipe that internal diameter is about 5 mm and carries out into clubs and do; The mixed solution (guarantee does not have bubble as far as possible) measuring 6mL injects the box of the tetrafluoroethylene of definite shape, carries out Film forming operations.Take out after all samples being put into refrigerator freezing 24 h, wherein rod-like samples need soak 12 h(and cements out to make the water molecules in sample in proper amount of methanol solution).All samples at room temperature dries naturally subsequently.
In order to the macroshape observing SMCs replys behavior, by there is original shape sample under the microwave of 600W after irradiation 120 s under external force figuration, treat that sample is cooled to Room-temperature Shape and is fixed.Under the microwave exposure of 500 W, observe deformation recovery process, and adopt bending method to carry out quantitative test to shape-memory properties.Thermal stability test is carried out through the SMCs of different cycle index under microwave exposure.
The present invention is by combining the physico-chemical property of SiC, the shape memory effect of polymkeric substance and microwave operational principle, and the reply for SMCs provides brand-new motivating force.Although at present the stimuli responsive mode of SMPs is diversified, also do not expand to using this for microwave efficiently, easily the energy reply motivating force as material deformation.Responding microwave type SMCs just can show change and the recovery effect of shape under the irradiation of microwave field, Recovery Process does not need preheating, deformation recovery whole process then just can complete soon in several seconds, had the advantages such as efficient, energy-conservation, clean, also can realize remote control.
The present invention is under 100 ~ 1000 W microwaves, to after responding microwave type PVA/PAA interpenetrating polymer networks composite material of shape memory sample irradiation 10 ~ 120 s prepared under External Force Acting figuration, and under 0 ~ 1000 W output rating, observe the deformation recovery performance of SMCs sample under microwave exposure, by measuring the angle change of bend specimen in Recovery Process, carry out the responding microwave type shape-memory properties parameter of quantitative description SMCs.Test finds, the shape-memory properties of SMCs is not only relevant with the nano SiC amount of filling, and is also subject to the impact of microwave output power simultaneously.In addition, SiC is introduced in the thermomechanical property that improve matrix material to a certain extent, and this is desired by preparation SMCs.SMPs research at present based on PVA is less, the present invention selects PVA to study as body material, not only widened the kind of SMPs, but also the polymkeric substance that discovery take PVA as matrix is one can make DEFORMATION RESPONSE intelligent macromolecule to four kinds of different stimulated modes (temperature, solvent, UV-light, microwave).
SiC has higher dielectric loss coefficient, effectively can absorb microwave and produce heat effect under low temperature, is that desirable microwave causes heat-dissipating inorganic materials.But because its nanoparticle surface can be high, easily reunite, therefore need to carry out surface modification and make its dispersion even, stable in polymeric matrix, improve the performance of matrix material.The present invention uses the silane coupling agent with double bond group to carry out hydrophilic modifying 60XSB type Fourier infrared spectrograph to silicon carbide and analyzes the nano SiC surface after before modified respectively.As seen from Figure 1, modified SiC is at 1720cm
-1there is the stretching vibration absorption peak that C=O and C=C is weak in place; And wave number is at 2983 cm
-1, 2928 cm
-1there is the C-H stretching vibration peak on methylene radical; 1172 cm
-1neighbouring absorption peak obviously strengthens main owing to CH
3absorption peak.These phenomenons show that coupling agent is successfully connected in surface of SiC.
After the silane coupling agent hydrophilic modifying of nano SiC particle band double bond group, improve the water dispersible of inorganic particulate, recycling double bond causes AA monomer and is polymerized at particle surface, nanoparticle can be connected on polymer chain by covalent linkage.Therefore, SMCs prepared by the present invention, due to the constitutional features of its uniqueness, dielectric properties, thermomechanical property etc. all improve.
Automatic network analyzer Aglient E8362B is adopted to measure the specific inductivity (ε ') of SMCs of the present invention and dissipation factor (ε 〃) under 2450MHz room temperature environment.Electromagnetic energy is that the parameter of heat energy ability is relevant with loss tangent angle tan σ by material, is tan σ=ε 〃/ε ' by the Representation Equation. measuring result is listed in table 1, and visible specific inductivity and dissipation factor increase with SiC content and increase.As Fig. 2 display, increase SiC content and can significantly improve tan σ value, show that the SiC added is more, the heat energy of generation is more.Material composition not only affects its dielectric properties also affects the thermomechanical property such as Tg and storage modulus.
NETZSCH DSC 204 instrument is used to carry out differential scanning calorimetric analysis to SMCs of the present invention.Test condition: 5-10 mg sample is elevated to 275 ° of C with the temperature rise rate of 10 ° of C/min from-50 ° of C under nitrogen atmosphere.Fig. 3 shows, and sample baseline slightly upwards drift near 130 ° of C of all filling SiC micro mists, SiC, owing to the glass transition of PAA, is introduced the elasticity that can reduce macromolecular chain in polymeric matrix by this phenomenon, thus makes baseline upwards drift.Appear at the crystalline melting peak that 230 ° of sharp endotherm(ic)peaks in C place are PVA, show that SiC serves as nucleus and contributes to macromolecular chain crystallization, because PVA inherently a kind of typical partially crystalline polymer.
Use DMA Q800 V7.1 Dynamic thermo-mechanical property tester, under stretch mode, thermodynamic performance test is carried out to SMCs of the present invention.Test condition: frequency is 1 Hz, heat-up rate 2 ° of C/min, nitrogen atmosphere.Fig. 4 shows, and storage modulus increases with SiC content and increases, and shows that sample hardness and mechanical stability all increase.
Can launch 2450MHz electromagnetic energy at magnetron, output voltage observes SMCs of the present invention within the scope of 0 ~ 1000 W macroshape in continuously adjustable Whirlpool T120 microwave oven replys behavior.Carry out quantitative test with bending method to the Shape memory behavior of matrix material, SiC content and the deformation recovery performance of microwave output power to SMCs all have a significant effect.Fig. 5 shows, and under certain power irradiance, all samples response rate is all up to 95%, but turnaround time is obviously different.SiC content is more, and sample is shorter for turnaround time.Fig. 6 shows, when microwave exposure power is less than 200 W, deformation recovery behavior is very slow.But the microwave power of 400 W is enough to stimulate the reply making a concentrated effort to finish deformation, under this power after irradiation 18 s, material recovers rate can reach more than 95%.When microwave power is more than 600 W, in very short time, (10 s) just can complete deformation recovery.This result means can by regulating the deformation recovery speed of the output rating control SMCs of microwave.
Observe microwave exposure with thermogravimetic analysis (TGA) method whether to impact the thermostability of SMCs of the present invention.Fig. 7 shows the thermogravimetric curve crossing sample through different cycle index (1,3,5) microwave exposure, the first stage degraded occurred near 100 ~ 200 DEG C is main, and what occur is PVA pendant hydroxyl group removing at high temperature, in the main chain thermal destruction that 275 ~ 400 DEG C of subordinate phase degradeds occur, can find out that the thermal degradation process of these three samples is not obviously distinguished, although mean through repeatedly microwave exposure test, the inierpeneirating network structure of matrix material is not subject to obvious impact, still keeps the thermostability that it is good.
Upper table is dielectric properties and the recoverability of different SiC content SMCs of the present invention, and SiC% refers to that SiC accounts for the mass percent of polymkeric substance.
Claims (5)
1. the preparation method of microwave-driven type interpenetrating(polymer)networks shape-memory polymer, is characterized in that carrying out according to following step:
Step one, the nanometer silicon carbide SiC after vacuum heat treatment is added in toluene, be warmed up to 30 ~ 100 DEG C, add the silanization coupling agent of SiC quality 1 ~ 10 %, stirring reaction 1 ~ 12h, product is vacuum filtration while hot, and successively with acetone and deionized water wash, centrifugation is then dry, obtain modified Nano SiC, then modified Nano SiC is scattered in water obtains the SiC dispersion liquid that mass content is 1 ~ 8 %;
Step 2, be 500 ~ 2400 by the polymerization degree, the alcoholysis degree PVAC polyvinylalcohol that is greater than 80% is dissolved in water that to obtain mass percent be 3 ~ 15 %PVA aqueous solution;
Step 3, mass ratio by SiC: PVA=1 ~ 10: 100, SiC dispersion liquid step one prepared joins step 2 and prepares in the PVA aqueous solution, stirs 0.5 ~ 1.5h;
Step 4, the AA adding PVA quality 20 ~ 80% successively, linking agent, initiator, 20 ~ 95 DEG C of crosslinking reaction 2 ~ 8h, obtain responding microwave type PVA/PAA interpenetrating polymer networks composite material of shape memory.
2. the preparation method of microwave-driven type interpenetrating(polymer)networks shape-memory polymer according to claim 1, is characterized in that: the silanization coupling agent in step one is any one in 3-(iso-butylene acyl-oxygen) propyl trimethoxy silicane, vinyltriethoxysilane, vinyltrimethoxy silane, vinyl three ('beta '-methoxy oxyethyl group) silane.
3. the preparation method of microwave-driven type interpenetrating(polymer)networks shape-memory polymer according to claim 1, is characterized in that: the reaction process of step one is carried out under nitrogen protection.
4. the preparation method of microwave-driven type interpenetrating(polymer)networks shape-memory polymer according to claim 1, it is characterized in that: the linking agent in step 4 is the MBA of AA quality 0.5 ~ 3 wt%, initiator is the K of AA quality 0.5 ~ 3 wt%
2s
2o
8.
5. the preparation method of any microwave-driven type interpenetrating(polymer)networks shape-memory polymer according to claim 1-4, is characterized in that: the vacuum heat treatment in step one refers to nano SiC vacuum heat treatment 24 h at 120 DEG C.
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| CN113004497A (en) * | 2019-01-22 | 2021-06-22 | 苏州大学 | Shape memory recovery method of thermoadaptive shape memory polymer |
| CN113004497B (en) * | 2019-01-22 | 2022-06-21 | 苏州大学 | Shape memory recovery method of thermoadaptive shape memory polymer |
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