CN112980174B - Polymer composite material and preparation method thereof - Google Patents
Polymer composite material and preparation method thereof Download PDFInfo
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Abstract
The invention provides a polymer composite material and a preparation method thereof, wherein the polymer composite material comprises the following raw material components: conductive polymer, high molecular compound containing glycol structure, carboxylated polymethylsiloxane, heteropoly acid, glycerol, phytic acid, chitosan, polyethyleneimine and nano filler; wherein the mass ratio of the components comprises: the mass ratio of the macromolecular compound containing the glycol structure to the conductive macromolecule is 50-200 percent; the mass ratio of the carboxylated polymethylsiloxane to the conductive polymer is 15-30 percent; the mass ratio of the heteropoly acid to the conductive polymer is 10-30%.
Description
Technical Field
The invention belongs to the technical field of novel high polymer materials, and particularly relates to a high polymer composite material for impact protection and a preparation method thereof.
Background
In recent years, impact protection materials have received much attention due to their high utility value. The current commercial impact protection materials are mainly shear thickening materials, which increase the force bearing area by hardening under impact and thus reduce impact damage. However, shear thickening materials have poor creep resistance and require compounding with other creep resistant polymeric materials. Moreover, the impact protection mechanism of the shear thickening material is single, and the protection performance is insufficient.
Disclosure of Invention
In view of the above, in order to develop a polymer composite material having a novel impact protection mechanism, excellent impact protection performance, and good molding capability, the present invention provides a polymer composite material and a preparation method thereof, wherein the polymer composite material contains abundant dynamic intermolecular forces, so that the polymer composite material has good plasticity and impact protection capability.
In order to achieve the above object, in one aspect, the present invention provides a polymer composite material, which comprises the following raw material components: conductive polymer, high molecular compound containing glycol structure, carboxylated polymethylsiloxane, heteropoly acid, glycerol, phytic acid, chitosan, polyethyleneimine and nano filler; wherein the mass ratio of the components comprises: the mass ratio of the macromolecular compound containing the glycol structure to the conductive macromolecule is 50-200 percent; the mass ratio of the carboxylated polymethylsiloxane to the conductive polymer is 15-30 percent; the mass ratio of the heteropoly acid to the conductive polymer is 10-30%.
According to an embodiment of the invention, the mass ratio between the components further comprises: the mass ratio of the glycerol to the conductive polymer is 10-30 percent; the mass ratio of the phytic acid to the conductive polymer is 5-10 percent; the mass ratio of the chitosan to the conductive polymer is 2-10 percent; the mass ratio of the polyethyleneimine to the conductive polymer is 20-40%; the mass ratio of the nano filler to the conductive polymer is 10-30%.
According to an embodiment of the present invention, wherein the conductive polymer is formed by polymerizing a conductive polymer monomer.
According to an embodiment of the present invention, the conductive polymer monomer includes an aromatic conductive polymer monomer, and the aromatic conductive polymer monomer includes at least one of the following: pyrrole, aniline, thiophene and 3, 4-ethylenedioxythiophene.
According to an embodiment of the present invention, wherein the polymer compound containing an ethylene glycol structure includes at least one of: polyethylene glycol, ethoxylated pentaerythritol, ethoxylated trimethylolpropane; the molecular weight of the high molecular compound containing the ethylene glycol structure is 250-500.
According to an embodiment of the invention, wherein the heteropolyacid comprises a mixture of one or more of: silicomolybdic acid, phosphomolybdic acid, phosphotungstic acid, silicotungstic acid.
According to an embodiment of the invention, wherein the nano-filler comprises at least one of: nano silicon dioxide, nano titanium dioxide, nano clay, nano carbon spheres, nano iron oxide and nano cellulose.
In another aspect, the present invention further provides a method for preparing the polymer composite material, the method comprising: dissolving heteropoly acid in a high molecular compound containing an ethylene glycol structure to obtain a first mixed solution; uniformly mixing a conductive high-molecular monomer, a high-molecular compound containing an ethylene glycol structure, carboxylated polydimethylsiloxane, glycerol, phytic acid, chitosan and polyethylene amine according to a certain mass ratio to obtain a second mixed solution; and under the preset reaction condition, adding the first mixed solution into the second mixed solution which is continuously stirred, and simultaneously adding the nano filler, stirring and mixing to obtain the polymer composite material.
According to an embodiment of the present invention, wherein the preset reaction conditions include: the reaction temperature is 0-5 ℃; the stirring reaction time is 4-10 h.
According to an embodiment of the present invention, the first mixed solution is used for promoting the polymerization of the conductive polymer monomer to form the conductive polymer, and building the reconstructed dynamic interaction between the conductive polymer monomer and other components.
According to the technical scheme, the polymer composite material and the preparation method thereof provided by the invention have the following beneficial effects:
(1) the polymer composite material has excellent impact protection performance and can dissipate 80% of impact energy;
(2) the polymer composite material of the invention shows special liquid-like rheological property, and can realize molding of complex shapes;
(3) the preparation method of the polymer composite material is simple, the raw materials are safe and cheap, and the polymer composite material can be prepared in a large scale.
Drawings
FIG. 1 is a flow chart schematically illustrating a method for preparing a polymer composite according to an embodiment of the present invention;
FIG. 2 is a schematic diagram showing a solid-liquid transition temperature of a polymer composite according to an embodiment of the present invention;
FIG. 3 is a graph schematically illustrating rheological data of a polymer composite according to a first embodiment of the present invention;
fig. 4 is a graph schematically illustrating experimental data of impact protection performance of a polymer composite according to a first embodiment of the present invention.
Detailed Description
The polymer composite material provided by the invention can form a novel polymer composite with very good plasticity and impact protection performance through abundant dynamic intermolecular acting force under the appropriate proportion of each component.
In order that the objects, technical solutions and advantages of the present invention will become more apparent, the present invention will be further described in detail with reference to the accompanying drawings in conjunction with the following specific embodiments.
The invention provides a polymer composite material and a preparation method thereof, in order to research a polymer composite material which has a novel impact protection mechanism, excellent impact protection performance and good molding capacity.
The invention provides a polymer composite material, which comprises the following raw material components: conductive polymer, high molecular compound containing glycol structure, glycerol, phytic acid, chitosan, polyethyleneimine, carboxylated polymethylsiloxane, heteropoly acid and nano filler; wherein the mass ratio of the components comprises: the mass ratio of the macromolecular compound containing the glycol structure to the conductive macromolecule is 50-200 percent; the mass ratio of the carboxylated polymethylsiloxane to the conductive polymer is 15-30 percent; the mass ratio of the heteropoly acid to the conductive polymer is 10-30%.
According to an embodiment of the present invention, the conductive polymer is formed by in-situ polymerization of a conductive polymer monomer. As the monomer of the conductive polymer, there is no particular limitation in the present invention as long as the monomer can be polymerized to form the conductive polymer.
According to the embodiment of the present invention, the conductive polymer monomer may be an aromatic conductive polymer monomer, which may include an aromatic conductive polymer monomer containing a benzene ring, and may also include a conductive polymer monomer containing a heterocycle. Specifically, one or more of the following are included, but not limited to: pyrrole, aniline, thiophene and 3, 4-ethylenedioxythiophene.
According to an embodiment of the present invention, the polymer compound having an ethylene glycol structure may include one or more of: ethoxylated pentaerythritol, polyethylene glycol, ethoxylated trimethylolpropane. Wherein, the molecular weight of the high molecular compound containing the glycol structure can be 250-500, and the preferable range is 270-350.
According to an embodiment of the present invention, the molecular weight of the high molecular compound having an ethylene glycol structure may be 250, 300, 350, 400, 450, 500.
According to the embodiment of the invention, the molecular weight of the macromolecular compound containing the glycol structure influences the mechanical property of the composite material. The molecular weight of the high molecular compound containing the ethylene glycol structure is too low, so that the strength of the obtained high molecular composite material is too low and the high molecular composite material is not easy to form a solid state; the molecular weight of the high molecular compound containing the ethylene glycol structure is too high, and the strength of the obtained high molecular composite material is too high, so that the plasticity is poor, and the impact protection performance is influenced. In conclusion, the molecular weight of the ethylene glycol-containing high molecular compound is selected to be suitable for the mechanical property, and the molding capability and the impact protection performance of the ethylene glycol-containing high molecular compound are simultaneously met according to the rheological data. Preferably, the molecular weight of the ethylene glycol-containing polymer compound may be 270 to 350.
According to the examples of the present invention, the carboxylated polymethylsiloxane may be obtained by a known preparation method or may be commercially available. In the present invention, the skilled person obtains the carboxylated polymethylsiloxane by the preparation method. It is to be noted that there is no particular limitation in preparing the carboxylated polymethylsiloxane as long as the component can be obtained.
In the examples of the present invention, the preparation process for preparing the carboxylated polymethylsiloxane by the skilled person is as follows:
(a) adding 6g of polymethylhydrosiloxane, 12g of methyl methacrylate, 75mL of toluene and 150 mu L of platinum (0) -1, 3-divinyl-1, 1, 3, 3-tetramethyldisiloxane complex into a round-bottom flask, and stirring and refluxing for 12 hours at 80 ℃ under an inert atmosphere;
(b) removing solvent, adding 75ml tetrahydrofuran and LiOH aqueous solution, stirring and refluxing at 85 deg.C for 1 hr, standing, collecting lower water phase, and washing with tetrahydrofuran for 3 times;
(c) and adding 50mL of tetrahydrofuran into the obtained clear aqueous solution, adjusting the pH value to 1-2, standing for phase separation, collecting an upper tetrahydrofuran phase, and performing vacuum drying to obtain the carboxylated polymethylsiloxane.
According to embodiments of the invention, the heteropolyacid may comprise a mixture of one or more of: silicomolybdic acid, phosphomolybdic acid, phosphotungstic acid, silicotungstic acid.
In the embodiment of the invention, the addition of the heteropoly acid can promote the conductive polymer monomer to be polymerized into the conductive polymer, and change the valence state of the conductive polymer; it also promotes the formation of a number of dynamic interactions between the components that are free to fracture and reconfigure.
In the embodiment of the invention, the raw material components can form a polymer composite material capable of being repeatedly molded through the dynamic interaction between molecules at a certain mass ratio.
According to the embodiment of the invention, the mass ratio of the raw material components comprises:
according to the embodiment of the present invention, the mass ratio of the polymer compound having an ethylene glycol structure to the conductive polymer may be 50% to 200%, preferably 80% to 150%, and most preferably 90% to 150%.
According to the embodiment of the present invention, the mass ratio of the polymer compound having an ethylene glycol structure to the conductive polymer may be 50%, 100%, 150%, 200%.
According to the embodiment of the present invention, the mass ratio of the carboxylated polymethylsiloxane to the conductive polymer may be 15% to 30%, preferably 20% to 30%, and most preferably 25% to 30%.
According to an embodiment of the present invention, the mass ratio of the carboxylated polymethylsiloxane to the conductive polymer may be 15%, 18%, 22%, 25%, 27%, 30%.
According to the embodiment of the present invention, the mass ratio of the heteropoly acid to the conductive polymer may be 10% to 30%, preferably 12% to 25%, and most preferably 20% to 25%.
According to an embodiment of the present invention, the mass ratio of the heteropoly acid to the conductive polymer may be 10%, 15%, 20%, 25%, 30%.
According to an embodiment of the present invention, the mass ratio of the glycerin to the conductive polymer may be 10% to 30%, preferably 15% to 30%, and most preferably 20% to 25%.
According to the embodiment of the present invention, the mass ratio of the phytic acid to the conductive polymer may be 5% to 10%, preferably 5% to 8%, and most preferably 6% to 8%.
According to the embodiment of the present invention, the mass ratio of the chitosan to the conductive polymer may be 2% to 10%, preferably 4% to 8%, and most preferably 5% to 8%.
According to the embodiment of the present invention, the mass ratio of the polyethyleneimine to the conductive polymer may be 20% to 40%, preferably 25% to 40%, and most preferably 30% to 40%.
According to an embodiment of the present invention, the mass ratio of the nano-filler to the conductive polymer may be 10% to 30%, preferably 15% to 30%, and most preferably 20% to 30%. Wherein the nano-filler includes but is not limited to: nano silicon dioxide, nano titanium dioxide, nano clay, nano carbon spheres, nano iron oxide and nano cellulose.
According to the embodiment of the invention, under a certain mass ratio of each component, a polymer composite material capable of repeatedly molding is formed through abundant intermolecular dynamic interactions, and in the polymer composite material, a conductive polymer network can form a large amount of dynamic interactions capable of being freely fractured and reconstructed with other components, so that the polymer composite material has very good molding capability. In addition, due to the mechanical responsiveness of dynamic interaction, the polymer composite material can dissipate the external impact action through the reconstruction of internal dynamic interaction, so that the aim of impact protection is fulfilled.
According to the embodiment of the invention, the macromolecular composite material provided by the invention overcomes the essential defect that the traditional shear thickening material is easy to creep and cannot maintain a stable shape from the molecular angle, and has application in the field of impact protection.
The invention also provides a preparation method for preparing the polymer composite material. The preparation method includes operations S101 to S103.
In operation S101, a heteropoly acid is dissolved in a polymer compound having an ethylene glycol structure to obtain a first mixed solution.
According to the embodiment of the invention, the first mixed solution is prepared by dissolving heteropoly acid and a small amount of ammonium persulfate into a high molecular compound containing an ethylene glycol structure.
According to an embodiment of the present invention, the first mixed solution is used to promote the polymerization of the conductive polymer monomer to form the conductive polymer, and to build the restructured dynamic interaction between the conductive polymer monomer and other components. Wherein, a small amount of ammonium persulfate is added to have the redox effect and assist the heteropoly acid in promoting the conductive polymer monomer to polymerize to form the conductive polymer.
In operation S102, a conductive polymer monomer, a polymer compound containing an ethylene glycol structure, carboxylated polydimethylsiloxane, glycerol, phytic acid, chitosan, and polyethyleneimine are uniformly mixed according to a certain mass ratio to obtain a second mixed solution.
According to the embodiment of the invention, the components are uniformly mixed according to a certain mass ratio, the certain mass ratio comprises the mass ratio of each component to the conductive polymer, and the specific preferred ratio is described in detail in the foregoing, and is not described again.
In operation S103, under the preset reaction condition, the first mixed solution is added to the second mixed solution that is continuously stirred, and the nano filler is added to be stirred and mixed at the same time, so as to obtain the polymer composite material.
According to the embodiment of the invention, in an ice-water bath reaction device with the reaction temperature of 0-5 ℃, the first mixed solution is slowly added into the second mixed solution while stirring, and the black dough-like material is formed after stirring and reacting for 4-10 hours. And adding the nano filler and continuously mixing to finally obtain the polymer composite material.
According to an embodiment of the present invention, the preset reaction conditions include: the reaction temperature is 0-5 ℃, the stirring reaction time is 4-10 h, preferably 4-8 h, and most preferably 6-8 h. The polymerization reaction among the raw material components is influenced by proper reaction temperature and reaction time, the polymerization reaction can not be too fast due to the preferable reaction conditions, the reaction is mild, the polymerization effect is obvious, and the finally obtained polymer composite material has better plastic ability and impact protection performance.
According to the embodiment of the invention, by the preparation method of the polymer composite material provided by the invention, under the appropriate proportion of the components, a large amount of dynamic interactions which can be freely fractured and reconstructed are formed among the components, so that the prepared polymer composite material has very good plastic forming capability; due to the mechanical responsiveness of dynamic interaction, the polymer composite dissipates the external impact action through the reconstruction of internal dynamic interaction, and achieves the purpose of impact protection. The polymer composite material and the preparation method thereof overcome the defects that the traditional shear thickening material is easy to creep, difficult to maintain stable in properties and limited in impact protection performance, and the preparation method is simple and flexible and can be used for large-scale preparation.
In the embodiment of the invention, the prepared polymer composite material can be found to have liquid-like properties and have a solid-liquid transition temperature point through rheological tests at different temperatures.
For example, fig. 2 schematically shows a solid-liquid transition temperature diagram of a polymer composite according to an embodiment of the present invention.
As shown in fig. 2, the polymer composite material exhibits a solid-like property at a lower temperature when the storage modulus is larger than the loss energy; at higher temperatures, the loss modulus is greater than the storage modulus, showing a liquid-like behavior. The temperature point of the transition is the solid-liquid transition temperature point of the polymer composite material.
Referring again to fig. 2, the polymer composite exhibits very good plastic-type processability when the temperature is higher than the solid-liquid transition point; the polymer composite material has good shape retention capability when the temperature is lower than the solid-liquid transition temperature point. It should be noted that, at the same time, the solid-liquid transition temperature point can be adjusted by changing the content of each raw material component, and the higher the general content is, the higher the solid-liquid transition temperature point is, so that the final material can directly design the polymer composite materials with different performances at room temperature according to the requirements of application conditions to realize the molding and processing of the final material into the target shape and structure, and the excellent impact protection performance is shown based on a large amount of dynamic molecular acting force existing in the obtained composite material.
The present invention is further illustrated in detail by the following specific examples. It should be noted that the present invention is not limited to these specific embodiments, and modifications and variations can be made to these specific embodiments based on the gist of the present invention, and the present invention is also within the scope of the present invention.
Example 1
Mixing 0.5g of silicomolybdic acid and 0.5g of ammonium persulfate in 2g of polyethylene glycol (Mn ═ 300) to obtain a first mixed solution;
uniformly mixing 2g of thiophene, 1g of polyethylene glycol, 2g of a mixed solution of carboxylated polymethylsiloxane, 0.4g of glycerol, 0.15 g of phytic acid, 0.1g of chitosan and 0.8g of polyethyleneimine to obtain a second mixed solution;
and slowly adding the first mixed solution into the second mixed solution while stirring in an ice-water bath reaction device with the reaction temperature of 0-5 ℃, stirring for 6 hours to react to form a black bulk material, and further adding 0.1g of nano silicon dioxide, 0.05g of nano titanium dioxide, 0.05g of nano clay, 0.1g of nano carbon spheres, 0.1g of nano iron oxide and 0.1g of nano cellulose, and continuously mixing to obtain the final polymer composite material.
And performing rheological test and drop hammer test on the obtained polymer composite material to represent the plastic ability and the impact protection performance of the polymer composite material.
For example, fig. 3 schematically shows a graph of rheological data of a polymer composite according to a first embodiment of the present invention.
As shown in fig. 3, at room temperature, the loss modulus of the composite is greater than the elastic modulus, showing a liquid-like behavior, indicating that the composite has very good moldability capability.
It should be noted that, according to the embodiments of the present invention, if other conditions are not changed, only silicomolybdic acid is changed into other heteropoly acids with similar structures such as: silicotungstic acid, phosphomolybdic acid, phosphotungstic acid and the like can obtain the polymer composite material with similar rheological properties.
According to the embodiment of the present invention, if other conditions are not changed, a polymer composite material with similar properties can be obtained by changing polyethylene glycol into a polymer containing an ethylene glycol structure such as ethoxylated pentaerythritol (Mn 270) and ethoxylated trimethylolpropane (Mn 450).
According to the embodiment of the invention, if other conditions are not changed, the polymer composite material with similar properties can be obtained only by changing thiophene into conductive polymer monomers such as aniline, pyrrole, 3, 4-ethylenedioxythiophene and the like.
Fig. 4 is a graph schematically illustrating experimental data of impact protection performance of a polymer composite according to a first embodiment of the present invention.
The materials used in fig. 4 are classified into front and rear mechanical output signal changes in which the polymer composite of the present invention is not added as a buffer layer and in which the polymer composite of the present invention is added as a buffer layer.
According to the embodiment of the invention, the preparation method of the buffer material with the polymer composite material as the buffer layer comprises the following steps: the polymer composite material is molded into a circular material with the thickness of 0.5cm and the diameter of 4cm, and the output signal of an acceleration sensor on a drop hammer after the drop hammer of 500g falls from the height of 1m is tested so as to carry out drop hammer experiment test on the impact protection of the drop hammer.
As shown in fig. 4, in the drop hammer test, the mechanical output signal changes before and after the polymer material prepared by the present invention is added as the protective layer and before and after the polymer material prepared by the present invention is not added as the protective layer, and it can be seen that the material with the polymer material prepared by the present invention as the protective layer can dissipate about 80% of the impact force.
According to the embodiment of the invention, the invention provides a high polymer composite material for impact protection and a preparation method thereof. The polymer composite material overcomes the defects that the traditional shear thickening material is easy to creep, difficult to maintain stable shape and limited impact protection performance, and has important research significance and application value.
The above embodiments are provided to further explain the objects, technical solutions and advantages of the present invention in detail, and it should be understood that the above embodiments are only examples of the present invention and are not intended to limit the present invention, and any modifications, equivalents, improvements and the like made within the spirit and principle of the present invention should be included in the protection scope of the present invention.
Claims (10)
1. A polymer composite material comprises the following raw material components: conductive polymer, high molecular compound containing glycol structure, carboxylated polymethylsiloxane, heteropoly acid, glycerol, phytic acid, chitosan, polyethyleneimine and nano filler;
wherein the mass ratio of the components comprises: the mass ratio of the high molecular compound containing the glycol structure to the conductive high molecular is 50-200%;
the mass ratio of the carboxylated polymethylsiloxane to the conductive polymer is 15-30%;
the mass ratio of the heteropoly acid to the conductive polymer is 10-30%.
2. The polymeric composite material of claim 1, further comprising, in mass ratios between the components:
the mass ratio of the glycerol to the conductive polymer is 10-30%;
the mass ratio of the phytic acid to the conductive polymer is 5-10%;
the mass ratio of the chitosan to the conductive polymer is 2-10%;
the mass ratio of the polyethyleneimine to the conductive polymer is 20-40%;
the mass ratio of the nano filler to the conductive polymer is 10-30%.
3. The polymer composite according to claim 1, wherein the conductive polymer is formed by polymerizing a conductive polymer monomer.
4. The polymer composite according to claim 3, wherein the conductive polymer monomer comprises an aromatic conductive polymer monomer comprising at least one of: pyrrole, aniline, thiophene and 3, 4-ethylenedioxythiophene.
5. The polymer composite according to claim 1, wherein the polymer compound having an ethylene glycol structure includes at least one of: polyethylene glycol, ethoxylated pentaerythritol, ethoxylated trimethylolpropane; the molecular weight of the high molecular compound containing the ethylene glycol structure is 250-500.
6. The polymeric composite of claim 1, wherein the heteropoly acid comprises a mixture of one or more of: silicomolybdic acid, phosphomolybdic acid, phosphotungstic acid, silicotungstic acid.
7. The polymeric composite of claim 1, wherein the nanofiller comprises at least one of: nano silicon dioxide, nano titanium dioxide, nano clay, nano carbon spheres, nano iron oxide and nano cellulose.
8. A method for preparing a polymer composite material according to any one of claims 1 to 7, comprising:
dissolving heteropoly acid in a high molecular compound containing an ethylene glycol structure to obtain a first mixed solution;
uniformly mixing a conductive high-molecular monomer, a high-molecular compound containing an ethylene glycol structure, carboxylated polydimethylsiloxane, glycerol, phytic acid, chitosan and polyethyleneimine according to a certain mass ratio to obtain a second mixed solution;
and under the preset reaction condition, adding the first mixed solution into the second mixed solution which is continuously stirred, and simultaneously adding the nano filler, stirring and mixing to obtain the polymer composite material.
9. The production method according to claim 8, wherein the preset reaction conditions include:
the reaction temperature is 0-5 ℃; the stirring reaction time is 4-10 h.
10. The method according to claim 8, wherein the first mixed solution is used to promote polymerization of a conductive polymer monomer to form a conductive polymer and to establish a dynamic interaction of the conductive polymer monomer with other components.
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| CN112980174A (en) | 2021-06-18 |
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