CN112239593A - Multi-response shape memory polyurethane material and preparation method and application thereof - Google Patents
Multi-response shape memory polyurethane material and preparation method and application thereof Download PDFInfo
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Abstract
The invention belongs to the technical field of functional materials, and particularly relates to a multiple-response shape memory polyurethane material, which comprises the following components in percentage by total mass of 100 percent: 6.0-10.0% of thermoplastic polyurethane, 0.5-1.0% of acrylic crosslinked resin, 0.1-1.0% of nano reinforcing material, 0.2-1.0% of nano conductive material, 0.1-0.6% of organic antibacterial material and the balance of solvent. According to the invention, through the modification and enhancement effects of the components on the polyurethane material, the polyurethane material not only has an excellent shape memory function and response performance to stimulation of water, pH and electricity, but also has good conductivity and antibacterial performance, the stimulation response range of the shape memory polyurethane material is expanded, the polyurethane material has a multi-response shape memory function, the application requirements of a multifunctional flexible sensor are met, and the application range of the shape memory polyurethane material is expanded.
Description
Technical Field
The invention belongs to the technical field of functional materials, and particularly relates to a multiple-response shape memory polyurethane material and a preparation method thereof, a flexible sensor and a conductive textile.
Background
With the continuous progress and development of society and science and technology, people have higher and higher requirements on materials, various novel functional materials are applied, and the shape memory polymer intelligent material with the characteristics of self diagnosis, self adaptation, shape recovery and the like is an important one of the materials and has wide application prospect. Shape Memory Polymer (SMP) is a polymer which has an initial shape, can recover the initial shape after being deformed and fixed under the action of certain external conditions through external stimulation, has the advantages of light weight, low price, easy processing, large deformation amount, corrosion resistance and the like, has incomparable advantages in the aspects of biocompatibility, biodegradability and the like, and has been successfully applied in a plurality of technical fields. Polymers such as polyurethane, crosslinked polyethylene, modified epoxy resin and the like are all used for manufacturing shape memory materials, wherein polyurethane with shape memory performance is praised as an intelligent polymer with the most research value and application value by the largest technical society of eventitle in the united states.
Polyurethane (TPU) includes a soft segment and a hard segment, which are a type of polymer material having a two-phase structure (a stationary phase and a reversible phase), with the hard segment (crystalline portion) as the stationary phase and the soft segment (amorphous portion) as the reversible phase, thereby having excellent shape memory properties. The shape memory polyurethane material has wide application because of easy molding, large deformation rate and lower cost. However, the conventional shape memory polyurethane material cannot simultaneously have excellent mechanical properties, thermal stability, conductivity, antibacterial properties and the like, and the application of the shape memory polyurethane material in a sensor is limited, so that the shape memory polyurethane material needs to be modified.
Disclosure of Invention
The invention aims to provide a multiple-response shape memory polyurethane material, and aims to solve the technical problems that the existing shape memory polyurethane material cannot simultaneously have excellent mechanical property, conductivity, antibacterial property and other properties, and the application of the shape memory polyurethane material in a sensor is limited, and the like.
The invention also aims to provide a preparation method of the multi-response shape memory polyurethane material.
It is a further object of the present invention to provide a flexible sensor.
It is still another object of the present invention to provide a conductive textile
A multiple-response shape memory polyurethane material comprises the following components in percentage by mass based on the total mass of the multiple-response shape memory polyurethane as 100 percent:
preferably, the acrylic crosslinking resin is carbomer 940.
Preferably, the nanoreinforcement is selected from: hydroxymethyl nanocellulose and/or hydroxyethyl nanocellulose.
Preferably, the nano-conductive material is selected from: at least one of carbon nano tube, graphene, carbon black and silver nano wire.
Preferably, the organic antibacterial material is selected from: at least one of chloramphenicol, aloe vera gel, potassium sorbate, polyhexamethylene biguanide hydrochloride, povidone iodine, chlorhexidine gluconate, and benzalkonium chloride; and/or the presence of a gas in the gas,
the solvent is selected from: at least one of N, N-dimethylformamide, tetrahydrofuran, trichloromethane, dichloromethane and acetone.
Preferably, the method comprises the following steps:
obtaining a nano conductive material and a solvent, and dispersing the nano conductive material in the solvent to obtain a dispersion liquid of the nano conductive material;
obtaining thermoplastic polyurethane, acrylic crosslinked resin and a nano reinforcing material, and dispersing the thermoplastic polyurethane, the acrylic crosslinked resin and the nano reinforcing material in the solvent to obtain a mixed solution;
adding the dispersion liquid of the nano conductive material into the mixed liquid, and stirring to obtain a conductive shape memory polyurethane dispersion liquid;
and (3) obtaining an organic antibacterial material, adding the organic antibacterial material into the conductive shape memory polyurethane dispersion liquid, and performing dispersion treatment to obtain the multi-response shape memory polyurethane material with antibacterial performance.
Preferably, the step of dispersing the nano-conductive material in the solvent includes: adding the nano conductive material into the solvent, and performing ultrasonic dispersion for 30-60 minutes; and/or the presence of a gas in the gas,
the step of dispersing the thermoplastic polyurethane, the acrylic crosslinked resin, and the nanoreinforcement material in the solvent includes: and adding the thermoplastic polyurethane, the acrylic crosslinked resin and the nano reinforcing material into the solvent at the temperature of 75-90 ℃, and stirring at the speed of 200-600 r/min for 1-2 hours.
Preferably, the step of agitating treatment comprises: adding the dispersion liquid of the nano conductive material into the mixed liquid at the temperature of 75-90 ℃, and stirring at the speed of 200-600 r/min for 2-3 hours; and/or the presence of a gas in the gas,
the step of dispersion treatment comprises: adding the organic antibacterial material into the conductive shape memory polyurethane dispersion liquid at the temperature of 75-90 ℃, and stirring at the speed of 200-600 r/min for 0.5-1 hour.
A flexible sensor is prepared by obtaining the multi-response shape memory polyurethane material or the multi-response shape memory polyurethane material prepared by the method, pouring the multi-response shape memory polyurethane material into a mold, curing for 40-60 hours at the temperature of 75-90 ℃ to obtain a conductive polyurethane film, and performing a hot pressing process to obtain the flexible sensor.
A conductive textile obtains the multi-response shape memory polyurethane material or the multi-response shape memory polyurethane material prepared by the method, and the multi-response shape memory polyurethane material is made into shape memory polyurethane fibers by adopting a wet spinning process; the conductive textile contains the shape memory polyurethane fiber.
The invention provides a multiple response shape memory polyurethane material, which comprises the following components: 6.0-10.0% of thermoplastic polyurethane, 0.5-1.0% of acrylic crosslinked resin, 0.1-1.0% of nano conductive material, 0.2-1.0% of nano antibacterial material, 0.1-0.6% of organic antibacterial material and the balance of solvent. The acrylic crosslinked resin is combined with polyurethane, so that the soft segment of the polyurethane material can be increased, the mechanical strength of the shape memory polyurethane material is reduced, the ductility of the shape memory polyurethane material is improved, the cyclic tensile property of the polyurethane material is more excellent, and the shape memory effect of the polyurethane material is improved; the surface of the nano reinforced material contains a large number of active functional groups combined with polyurethane, and the nano reinforced material has a reinforcing effect on the mechanical property of the polyurethane material; the nano conductive material not only can further enhance the mechanical property of polyurethane, but also endows the polyurethane material with good conductive performance and enhances the flexible sensing performance of the polyurethane material; the organic antibacterial material enables the polyurethane material to have good antibacterial performance at the same time. According to the invention, through the modification and enhancement effects of the components on the polyurethane material, the polyurethane material not only has an excellent shape memory function and response performance to stimulation of water, pH and electricity, but also has good conductivity and antibacterial performance, the stimulation response range of the shape memory polyurethane material is expanded, the polyurethane material has a multi-response shape memory function, the application requirements of a multifunctional flexible sensor are met, and the application range of the shape memory polyurethane material is expanded.
The preparation method of the multiple response shape memory polyurethane material provided by the invention comprises the steps of dispersing a nano conductive material in a solvent to form a dispersion liquid of the conductive material, and then dispersing the thermoplastic polyurethane, the acrylic cross-linked resin and the nano reinforcing material in the solvent to form a mixed liquid; and stirring and mixing the dispersion liquid of the nano conductive material and the mixed liquid, adding the organic antibacterial material, and uniformly dispersing to obtain the multi-response shape memory polyurethane material. The preparation method adopted by the invention can avoid the agglomeration phenomenon of the nano material to the maximum extent by the mixing and dissolving sequence of the components, achieves the effects of full dissolution and dispersion, enables the components of the materials to exert the optimal effect, has simple preparation process flow and low cost, and can realize industrialized production.
The flexible sensor provided by the invention takes the multi-response shape memory polyurethane material as a raw material, is cured and molded in a mold under the conditions that the temperature is 75-90 ℃ and the curing time is 40-60 hours to obtain a conductive polyurethane film, and is prepared into the flexible sensor with a certain thickness through a hot pressing process. The flexible sensor adopts the multi-response shape memory polyurethane material which not only has an excellent shape memory function, but also has good conductivity, antibacterial property and stability, so that the prepared flexible sensor has the excellent shape memory function, the good conductivity, the antibacterial property, the excellent sensitivity and the excellent flexibility, and can realize the deformation sensing function.
The conductive textile provided by the invention adopts the shape memory polyurethane fiber made of the multi-response shape memory polyurethane material, and the adopted multi-response shape memory polyurethane material not only has an excellent shape memory function, but also has good conductivity, antibacterial property and stability, so that the shape memory polyurethane fiber made of the material also has the excellent characteristics. Furthermore, the textile made of the fiber also has excellent shape memory function, good conductivity, antibacterial property, stability, excellent sensitivity and flexibility, and can realize deformation sensing function.
Drawings
FIG. 1 is a graph comparing the mechanical properties of a polyurethane film provided by an embodiment of the present invention.
Fig. 2 is a sensing performance test chart of a polyurethane film provided by an embodiment of the present invention.
FIG. 3 is a comparative graph of the antibacterial performance test of the polyurethane material provided by the embodiment of the invention.
Fig. 4 is a diagram illustrating a shape recovery of a polyurethane film according to an embodiment of the present invention.
Detailed Description
In order to make the purpose, technical solution and technical effect of the embodiments of the present invention clearer, the technical solution in the embodiments of the present invention is clearly and completely described, and it is obvious that the described embodiments are a part of the embodiments of the present invention, but not all embodiments. All other embodiments obtained by a person of ordinary skill in the art without any inventive step in connection with the embodiments of the present invention shall fall within the scope of protection of the present invention.
In the description of the present invention, it is to be understood that the terms "first", "second" and the like are used for descriptive purposes only and are not to be construed as indicating or implying relative importance or implying any number of technical features indicated. Thus, a feature defined as "first" or "second" may explicitly or implicitly include one or more of that feature. In the description of the present invention, "a plurality" means two or more unless specifically defined otherwise.
The weight of the related components mentioned in the description of the embodiments of the present invention may not only refer to the specific content of each component, but also represent the proportional relationship of the weight among the components, and therefore, the content of the related components is scaled up or down within the scope disclosed in the description of the embodiments of the present invention as long as it is in accordance with the description of the embodiments of the present invention. Specifically, the weight described in the description of the embodiment of the present invention may be a unit of mass known in the chemical industry field, such as μ g, mg, g, and kg.
The embodiment of the invention provides a multiple-response shape memory polyurethane material, which comprises the following components in percentage by mass based on 100% of the total mass of the multiple-response shape memory polyurethane:
the embodiment of the invention provides a multiple response shape memory polyurethane material, which comprises the following components: 6.0-10.0% of thermoplastic polyurethane, 0.5-1.0% of acrylic crosslinked resin, 0.1-1.0% of nano reinforcing material, 0.2-1.0% of nano conductive material, 0.1-0.6% of organic antibacterial material and the balance of solvent. The acrylic crosslinked resin is combined with polyurethane, so that the soft segment of the polyurethane material can be increased, the mechanical strength of the shape memory polyurethane material is reduced, the ductility of the shape memory polyurethane material is improved, the cyclic tensile property of the polyurethane material is more excellent, and the shape memory effect of the polyurethane material is improved; the surface of the nano reinforced material contains a large number of active functional groups combined with polyurethane, and the nano reinforced material has a reinforcing effect on the mechanical property of the polyurethane material; the nano conductive material not only can further enhance the mechanical property of polyurethane, but also endows the polyurethane material with good conductive performance and enhances the flexible sensing performance of the polyurethane material; the organic antibacterial material enables the polyurethane material to have good antibacterial performance at the same time. According to the embodiment of the invention, through the modification and enhancement effects of the components on the polyurethane material, the polyurethane material has an excellent shape memory function, response performance to stimulation of water, pH and electricity, and good conductive performance and antibacterial performance, the stimulation response range of the shape memory polyurethane material is expanded, the polyurethane material has a multi-response shape memory function, the application requirements of a multifunctional flexible sensor are met, and the application range of the shape memory polyurethane material is expanded.
As a preferred embodiment, the acrylic crosslinking resin is carbomer 940. According to the embodiment of the invention, the acrylic cross-linked resin in the multi-response shape memory polyurethane material is selected from carbomer 940, the long chain of the carbomer 940 contains carboxyl combined with thermoplastic polyurethane, and the soft segment of the thermoplastic polyurethane is increased through the combination of the carbomer 940 and the thermoplastic polyurethane, so that the mechanical strength of the shape memory polyurethane is reduced, the ductility of the shape memory polyurethane is improved, the cyclic tensile property of the thermoplastic polyurethane material is more excellent, and the shape memory effect of the material is improved. The weight percentage content of the carbomer 940 is 0.5-1.0%, the carbomer 940 with the content has the best effect of improving the properties of the thermoplastic polyurethane, such as flexibility, shape memory and the like, and if the content of the carbomer 940 is too high, the mechanical strength of the thermoplastic polyurethane is too low; if the content of the carbomer 940 is too low, the improvement effect on the performance of the polyurethane is not obvious.
As a preferred embodiment, the nanoreinforcement is selected from: hydroxymethyl nanocellulose and/or hydroxyethyl nanocellulose. According to the embodiment of the invention, the hydroxymethyl nanocellulose and/or hydroxyethyl nanocellulose is selected as the nano reinforcing material in the multi-response shape memory polyurethane material, molecular chains of the hydroxymethyl nanocellulose and the hydroxyethyl nanocellulose contain a large amount of hydroxyl groups, and the hydroxyl groups have a good combination effect with the thermoplastic polyurethane through hydrogen bonds, so that a good physical and chemical crosslinking effect is achieved, and the mechanical property of the shape memory polyurethane is greatly improved. The mass percentage of the hydroxymethyl nanocellulose and/or the hydroxyethyl nanocellulose added in the embodiment of the invention is 0.1-1.0%, the nano reinforcing material with the content has the best improvement effect on the mechanical property of the shape memory polyurethane material, and if the content of the nano reinforcing material is too high, the polyurethane material has too high strength, poor ductility and is not easy to stretch; if the content of the nano reinforcing material is too low, the improvement on the mechanical property of the polyurethane material is not obvious.
As a preferred embodiment, the nano conductive material is selected from: at least one of carbon nano tube, graphene, carbon black and silver nano wire. According to the embodiment of the invention, the nano conductive material in the multi-response shape memory polyurethane material is selected from at least one of carbon nano tube, graphene, carbon black and silver nano wire, so that the shape memory polyurethane has good conductive performance, and the conductive materials with nano structures such as the carbon nano tube, the graphene, the carbon black and the silver nano wire are used as physical cross-linking points in the polyurethane and play a good synergistic enhancement role on the mechanical property of the shape memory polyurethane material together with the nano cellulose. The mass percentage of the nano conductive materials such as the carbon nano tube, the graphene, the carbon black and the silver nano wire is 0.2-1.0%, and the addition amount is reasonable, so that the conductivity of the polyurethane material is ensured, and the synergistic effect of the polyurethane material and the nano reinforcing material is realized. If the addition amount of the nano conductive material is too high, the nano conductive material is not beneficial to uniform dispersion in the polyurethane material, and the modification effect of each component on the polyurethane and the synergistic interaction effect among the components can be damaged, so that the mechanical property, the mechanical property and the like of the polyurethane material are influenced; if the addition amount of the nano conductive material is too low, the conductivity of the polyurethane material and the synergistic interaction effect of the nano conductive material and the nano reinforcing material are poor.
As a preferred embodiment, the organic antibacterial material is selected from: at least one of chloramphenicol, aloe vera gel, potassium sorbate, polyhexamethylene biguanide hydrochloride, povidone iodine, chlorhexidine gluconate, and benzalkonium chloride. The organic antibacterial material in the multiple-response shape memory polyurethane material provided by the embodiment of the invention is selected from the following materials: at least one of chloramphenicol, aloe vera gel, potassium sorbate, polyhexamethylene biguanide hydrochloride, povidone iodine, chlorhexidine gluconate, and benzalkonium chloride endows the shape memory polyurethane material with a good antibacterial effect, so that the shape memory polyurethane material provided by the embodiment of the invention has not only an excellent shape memory function and an excellent conductive property, but also a good antibacterial property, expands the stimulus response range of the polyurethane material, and has a better application prospect. The organic antibacterial material is added in an amount of 0.1-0.6% by mass, and the addition amount not only effectively ensures the antibacterial performance of the polyurethane material, but also does not affect other components of the polyurethane material and other performances.
As a preferred embodiment, the solvent is selected from: at least one of N, N-dimethylformamide, tetrahydrofuran, trichloromethane, dichloromethane and acetone. The solvent selected by the multi-response shape memory polyurethane material provided by the embodiment of the invention has good solubility to thermoplastic polyurethane and acrylic cross-linked resin, has good dispersion effect to nano reinforcing materials, nano conductive materials and antibacterial components, and is convenient for modification of polyurethane by each component and synergistic interaction between the components.
In some embodiments, the multi-responsive shape memory polyurethane comprises, based on 100% total mass of the multi-responsive shape memory polyurethane: 6.0-10.0% of thermoplastic polyurethane, 0.5-1.0% of carbomer 940, 0.1-1.0% of hydroxymethyl nanocellulose and/or hydroxyethyl nanocellulose, 0.2-1.0% of at least one of carbon nanotubes, graphene, carbon black and silver nanowires, 0.1-0.6% of at least one of chloramphenicol, aloe vera gel, potassium sorbate, polyhexamethylene biguanide hydrochloride, povidone iodine, chlorhexidine gluconate and benzalkonium chloride, and a solvent.
The multi-response shape memory polyurethane provided by the embodiment of the invention can be prepared by the following method.
The embodiment of the invention also provides a preparation method of the multiple-response shape memory polyurethane material, which comprises the following steps:
s10, obtaining a nano conductive material and a solvent, and dispersing the nano conductive material in the solvent to obtain a dispersion liquid of the nano conductive material;
s20, obtaining thermoplastic polyurethane, acrylic crosslinked resin and a nano reinforcing material, and dispersing the thermoplastic polyurethane, the acrylic crosslinked resin and the nano reinforcing material in the solvent to obtain a mixed solution;
s30, adding the dispersion liquid of the nano conductive material into the mixed liquid, and stirring to obtain a conductive shape memory polyurethane dispersion liquid;
s40, obtaining an organic antibacterial material, adding the organic antibacterial material into the conductive shape memory polyurethane dispersion liquid, and performing dispersion treatment to obtain the multi-response shape memory polyurethane material with antibacterial property.
The preparation method of the multiple response shape memory polyurethane material provided by the embodiment of the invention comprises the steps of dispersing a nano conductive material in a solvent to form a dispersion liquid of the conductive material, and then dispersing the thermoplastic polyurethane, the acrylic cross-linked resin and the nano reinforcing material in the solvent to form a mixed solution; and stirring and mixing the dispersion liquid of the nano conductive material and the mixed liquid, adding the organic antibacterial material, and uniformly dispersing to obtain the multi-response shape memory polyurethane material. The preparation method adopted by the embodiment can avoid the agglomeration phenomenon of the nano material to the maximum extent by the mixing and dissolving sequence of the components, achieves the effects of full dissolution and dispersion, enables the components of the materials to exert the optimal effect, has simple preparation process flow and low cost, and can realize industrial production.
Specifically, in step S10, a nano conductive material and a solvent are obtained, and the nano conductive material is dispersed in the solvent to obtain a dispersion liquid of the nano conductive material. As a preferred embodiment, the step of dispersing the nano conductive material in the solvent includes: and adding the nano conductive material into the solvent, and performing ultrasonic dispersion for 30-60 minutes. According to the embodiment of the invention, through ultrasonic dispersion treatment, the nano conductive material is dispersed in the solvent in advance to form the dispersion liquid of the nano conductive material, so that the nano conductive material can be better dispersed in the shape memory polyurethane material, a uniform organic whole can be formed, and the agglomeration phenomenon of the nano material can be avoided.
Specifically, in step S20, thermoplastic polyurethane, acrylic crosslinked resin, and a nano reinforcing material are obtained, and the thermoplastic polyurethane, the acrylic crosslinked resin, and the nano reinforcing material are dispersed in the solvent to obtain a mixed solution. In a preferred embodiment, the thermoplastic polyurethane, the acrylic crosslinked resin and the nano reinforcing material are added into the solvent at a temperature of 75-90 ℃, and stirred at a speed of 200-600 r/min for 1-2 hours to obtain a mixed solution. According to the embodiment of the invention, the thermoplastic polyurethane, the acrylic crosslinked resin and the nano reinforcing material are dispersed in the solvent by stirring at a rotating speed of 200-600 r/min for 1-2 hours, so that raw material components are fully dissolved and dispersed, and full contact reaction among the components is facilitated.
Specifically, in step S30, the dispersion of the nano conductive material is added to the mixed solution and stirred to obtain a conductive shape memory polyurethane dispersion. As a preferred embodiment, the step of the stirring process includes: and adding the dispersion liquid of the nano conductive material into the mixed liquid at the temperature of 75-90 ℃, and stirring at the speed of 200-600 r/min for 2-3 hours. According to the embodiment of the invention, the dispersed mixed solution of the nano conductive material, the thermoplastic polyurethane, the acrylic cross-linked resin and the nano reinforcing material is stirred for 2-3 hours at the rotating speed of 200-600 r/min, so that the nano conductive material and the mixed solution are fully and uniformly mixed, the problems of uneven dispersion of raw material components, agglomeration and the like caused by the fact that all raw material products are simultaneously added into a solvent for dispersion can be effectively solved, all raw material components are fully dissolved and dispersed, the interaction among all components is facilitated, and the stability of the performance of the shape memory polyurethane material is ensured.
Specifically, in step S40, an organic antibacterial material is obtained, and the organic antibacterial material is added to the conductive shape memory polyurethane dispersion liquid and subjected to dispersion treatment to obtain an antibacterial multi-response shape memory polyurethane material. As a preferred embodiment, the step of the dispersion treatment includes: adding the organic antibacterial material into the conductive shape memory polyurethane dispersion liquid at the temperature of 75-90 ℃, and stirring at the speed of 200-600 r/min for 0.5-1 hour. According to the embodiment of the invention, the organic antibacterial material is added into the dispersed conductive shape memory polyurethane dispersion liquid, the mixture is stirred for 0.5-1 hour under the condition that the rotating speed is 200-600 r/min, and the organic antibacterial material is further uniformly dispersed in the conductive shape memory polyurethane dispersion liquid to obtain the multi-response shape memory polyurethane material, and all raw materials are dissolved and dispersed into a uniform organic unified whole, so that the optimal action among all raw material components is favorably exerted.
The embodiment of the invention also provides a flexible sensor, wherein the multi-response shape memory polyurethane material or the multi-response shape memory polyurethane material prepared by the method is obtained, the multi-response shape memory polyurethane material is poured into a mold, and is cured for 40-60 hours at the temperature of 75-90 ℃ to obtain a conductive polyurethane film, and the flexible sensor is prepared by a hot pressing process.
According to the flexible sensor provided by the embodiment of the invention, the multi-response shape memory polyurethane material is used as a raw material, curing and molding are carried out in a mold under the conditions that the temperature is 75-90 ℃ and the curing time is 40-60 hours, so as to obtain a conductive polyurethane film, and the flexible sensor with a certain thickness is prepared through a hot pressing process. Because the flexible sensor provided by the embodiment of the invention adopts the multi-response shape memory polyurethane material which not only has an excellent shape memory function, but also has good conductivity, antibacterial property and stability, the prepared flexible sensor also has the excellent shape memory function, good conductivity, antibacterial property, excellent sensitivity and flexibility, and can realize a deformation sensing function.
The embodiment of the invention also provides a conductive textile, wherein the multiple-response shape memory polyurethane material or the multiple-response shape memory polyurethane material prepared by the method is obtained, and the multiple-response shape memory polyurethane material is prepared into shape memory polyurethane fibers by adopting a wet spinning process; the conductive textile contains the shape memory polyurethane fiber.
The conductive textile provided by the embodiment of the invention adopts the shape memory polyurethane fiber made of the multi-response shape memory polyurethane material, and the adopted multi-response shape memory polyurethane material not only has an excellent shape memory function, but also has good conductivity, antibacterial performance and stability, so that the shape memory polyurethane fiber made of the material also has the excellent characteristics. Furthermore, the textile made of the fiber also has excellent shape memory function, good conductivity, antibacterial property, stability, excellent sensitivity and flexibility, and can realize deformation sensing function.
In order to make the above implementation details and operations of the present invention clearly understood by those skilled in the art and to make the advanced performance of the multiple response shape memory polyurethane material of the present invention obviously apparent, the above technical solution is illustrated by the following examples.
Example 1
A multiple response shape memory polyurethane material comprises the following preparation steps:
s11, adding 0.27g of Carbon Nanotubes (CNTs) into 20mL of N, N-Dimethylformamide (DMF), and performing ultrasonic dispersion for 30min to obtain a dispersion liquid of the CNTs;
s21, adding 4.0g of TPU, 0.5g of carbomer-940 and 0.225g of hydroxyethyl nanocellulose (CNC) into 25mL of DMF, and magnetically stirring at 75 ℃ at a speed of 200r/min for 2 hours to completely dissolve the TPU and the carbomer-940 and uniformly disperse the CNC to obtain a mixed solution of the TPU, the carbomer-940 and the CNC;
s31, slowly adding the dispersion liquid of the CNTs into a mixed liquid of TPU, carbomer-940 and CNC, and continuously magnetically stirring at the speed of 200r/min for 3.0h at the temperature of 75 ℃ to ensure that the CNTs are uniformly dispersed in the shape memory polyurethane system to obtain a conductive shape memory polyurethane dispersion liquid;
s41, adding 0.2g of chloramphenicol into the conductive shape memory polyurethane dispersion liquid, and continuously magnetically stirring at the speed of 200r/min for 0.5-1 h at the temperature of 75 ℃ to obtain the multi-response shape memory polyurethane material.
Example 2
A multiple response shape memory polyurethane material comprises the following preparation steps:
s12, adding 0.27g of graphene into 20mL of N, N-Dimethylformamide (DMF), and performing ultrasonic dispersion for 30min to obtain a graphene dispersion liquid;
s22, adding 4.0g of TPU, 0.5g of carbomer-940 and 0.225g of hydroxyethyl nanocellulose (CNC) into 25mL of DMF, and magnetically stirring at 75 ℃ at a speed of 200r/min for 2 hours to completely dissolve the TPU and the carbomer-940 and uniformly disperse the CNC to obtain a mixed solution of the TPU, the carbomer-940 and the CNC;
s32, slowly adding the dispersion liquid of the graphene into a mixed liquid of TPU, carbomer-940 and CNC, and continuously magnetically stirring at the speed of 200r/min for 3.0 hours at the temperature of 75 ℃ to ensure that the graphene is uniformly dispersed in the shape memory polyurethane system to obtain a conductive shape memory polyurethane dispersion liquid;
s42, adding 0.2g of chloramphenicol into the conductive shape memory polyurethane dispersion liquid, and continuously magnetically stirring at the speed of 200r/min for 0.5-1 h at the temperature of 75 ℃ to obtain the multi-response shape memory polyurethane material.
A flexible sensor is prepared by pouring the multi-response shape memory polyurethane material into a mould, curing at 75 ℃ for 48h, and taking out the product from the mould to obtain the flexible sensor with antibacterial property and multi-response shape memory polyurethane.
A conductive textile is prepared by using the multi-response shape memory polyurethane material to prepare shape memory polyurethane fibers by a wet spinning process, and the fibers are used for manufacturing the conductive textile.
Example 3
A multiple response shape memory polyurethane material comprises the following preparation steps:
s11, adding 0.27g of carbon black into 20mL of N, N-Dimethylformamide (DMF), and performing ultrasonic dispersion for 30min to obtain a carbon black dispersion liquid;
s23, adding 4.0g of TPU, 0.5g of carbomer-940 and 0.225g of hydroxyethyl nanocellulose (CNC) into 25mL of DMF, and magnetically stirring at 75 ℃ at a speed of 200r/min for 2 hours to completely dissolve the TPU and the carbomer-940 and uniformly disperse the CNC to obtain a mixed solution of the TPU, the carbomer-940 and the CNC;
s33, slowly adding the dispersion liquid of the carbon black into the mixed liquid of the TPU, the carbomer-940 and the CNC, and continuously magnetically stirring for 3.0 hours at the speed of 200r/min at the temperature of 75 ℃ to ensure that the carbon black is uniformly dispersed in the shape memory polyurethane system to obtain the conductive shape memory polyurethane dispersion liquid;
s43, adding 0.2g of chloramphenicol into the conductive shape memory polyurethane dispersion liquid, and continuously magnetically stirring at the speed of 200r/min for 0.5-1 h at the temperature of 75 ℃ to obtain the multi-response shape memory polyurethane material.
A flexible sensor is prepared by pouring the multi-response shape memory polyurethane material into a mould, curing at 75 ℃ for 48h, and taking out the product from the mould to obtain the flexible sensor with antibacterial property and multi-response shape memory polyurethane.
A conductive textile is prepared by using the multi-response shape memory polyurethane material to prepare shape memory polyurethane fibers by a wet spinning process, and the fibers are used for manufacturing the conductive textile.
Example 4
A multiple response shape memory polyurethane material comprises the following preparation steps:
s14, adding 0.27g of Carbon Nanotubes (CNTs) into 20mL of N, N-Dimethylformamide (DMF), and performing ultrasonic dispersion for 30min to obtain a dispersion liquid of the CNTs;
s24, adding 4.0g of TPU, 0.5g of carbomer-940 and 0.225g of hydroxyethyl nanocellulose (CNC) into 25mL of DMF, and magnetically stirring at 75 ℃ at a speed of 200r/min for 2 hours to completely dissolve the TPU and the carbomer-940 and uniformly disperse the CNC to obtain a mixed solution of the TPU, the carbomer-940 and the CNC;
s34, slowly adding the dispersion liquid of the CNTs into a mixed liquid of TPU, carbomer-940 and CNC, and continuously magnetically stirring at the speed of 200r/min for 3.0h at the temperature of 75 ℃ to ensure that the CNTs are uniformly dispersed in the shape memory polyurethane system to obtain a conductive shape memory polyurethane dispersion liquid;
s44, adding 0.2g of polyhexamethylene biguanide hydrochloride into the conductive shape memory polyurethane dispersion, and continuously magnetically stirring at the speed of 200r/min for 0.5-1 h at the temperature of 75 ℃ to obtain the multi-response shape memory polyurethane material.
A flexible sensor is prepared by pouring the multi-response shape memory polyurethane material into a mould, curing at 75 ℃ for 48h, and taking out the product from the mould to obtain the flexible sensor with antibacterial property and multi-response shape memory polyurethane.
A conductive textile is prepared by using the multi-response shape memory polyurethane material to prepare shape memory polyurethane fibers by a wet spinning process, and the fibers are used for manufacturing the conductive textile.
Example 5
A multiple response shape memory polyurethane material comprises the following preparation steps:
s15, adding 0.27g of graphene into 20mL of N, N-Dimethylformamide (DMF), and performing ultrasonic dispersion for 30min to obtain a graphene dispersion liquid;
s25, adding 4.0g of TPU, 0.5g of carbomer-940 and 0.225g of hydroxyethyl nanocellulose (CNC) into 25mL of DMF, and magnetically stirring at 75 ℃ at a speed of 200r/min for 2 hours to completely dissolve the TPU and the carbomer-940 and uniformly disperse the CNC to obtain a mixed solution of the TPU, the carbomer-940 and the CNC;
s35, slowly adding the graphene dispersion liquid into a mixed liquid of TPU, carbomer-940 and CNC, and continuously magnetically stirring at the speed of 200r/min for 3.0 hours at the temperature of 75 ℃ to uniformly disperse the graphene in the shape memory polyurethane system to obtain a conductive shape memory polyurethane dispersion liquid;
s45, adding 0.2g of polyhexamethylene biguanide hydrochloride into the conductive shape memory polyurethane dispersion, and continuously magnetically stirring at the speed of 200r/min for 0.5-1 h at the temperature of 75 ℃ to obtain the multi-response shape memory polyurethane material.
A flexible sensor is prepared by pouring the multi-response shape memory polyurethane material into a mould, curing at 75 ℃ for 48h, and taking out the product from the mould to obtain the flexible sensor with antibacterial property and multi-response shape memory polyurethane.
A conductive textile is prepared by using the multi-response shape memory polyurethane material to prepare shape memory polyurethane fibers by a wet spinning process, and the fibers are used for manufacturing the conductive textile.
Example 6
A multiple response shape memory polyurethane material comprises the following preparation steps:
s16, adding 0.27g of carbon black into 20mL of N, N-Dimethylformamide (DMF), and performing ultrasonic dispersion for 30min to obtain a carbon black dispersion liquid;
s26, adding 4.0g of TPU, 0.5g of carbomer-940 and 0.225g of hydroxyethyl nanocellulose (CNC) into 25mL of DMF, and magnetically stirring at 75 ℃ at a speed of 200r/min for 2 hours to completely dissolve the TPU and the carbomer-940 and uniformly disperse the CNC to obtain a mixed solution of the TPU, the carbomer-940 and the CNC;
s36, slowly adding the dispersion liquid of the carbon black into the mixed liquid of the TPU, the carbomer-940 and the CNC, and continuously magnetically stirring for 3.0 hours at the speed of 200r/min at the temperature of 75 ℃ to ensure that the carbon black is uniformly dispersed in the shape memory polyurethane system to obtain the conductive shape memory polyurethane dispersion liquid;
s46, adding 0.2g of polyhexamethylene biguanide hydrochloride into the conductive shape memory polyurethane dispersion, and continuously magnetically stirring at the speed of 200r/min for 0.5-1 h at the temperature of 75 ℃ to obtain the multi-response shape memory polyurethane material.
A flexible sensor is prepared by pouring the multi-response shape memory polyurethane material into a mould, curing at 75 ℃ for 48h, and taking out the product from the mould to obtain the flexible sensor with antibacterial property and multi-response shape memory polyurethane.
A conductive textile is prepared by using the multi-response shape memory polyurethane material to prepare shape memory polyurethane fibers by a wet spinning process, and the fibers are used for manufacturing the conductive textile.
Furthermore, in order to verify the advancement of the flexible sensor made of the multi-response shape memory polyurethane material in the embodiment of the invention, tests on the aspects of mechanical property, conductivity, antibacterial property, sensing property and the like are performed in the embodiment of the invention.
Test example 1
The invention carries out comparative test analysis on the mechanical property of the film prepared by the multi-response shape memory polyurethane material in the embodiment 1.
Comparative example 1 with Thermoplastic Polyurethane (TPU) added only; a flexible sensor was prepared under the same conditions as in example 1, with addition of TPU and hydroxyethyl nanocellulose nanoreinforcement as comparative example 2.
The flexible sensors prepared in example 1, comparative example 1 and comparative example 2 were used to test mechanical properties with a sample tape having a clamping pitch of 50mm, a width of 10mm and a thickness of 0.15mm, respectively. As shown in fig. 1, the flexible sensor of example 1 of the present invention has the best strain and stress, and the mechanical strength of polyurethane is significantly improved with the addition of nanocellulose (CNC), the elongation at break is increased from 583.61% to 909.87%, and the mechanical properties are still significantly improved with the addition of Carbon Nanotubes (CNT).
In addition, the sensor sample strip prepared in the embodiment 1 of the invention has the advantages of 50mm in length, 10mm in width and 0.15mm in thickness, the resistance of the sensor sample strip is 45.6k omega, the conductivity of the sensor sample strip is 0.142S/m, and the excellent conductivity is displayed.
Test example 2
The sensing performance of the film prepared from the multi-response shape memory polyurethane material in the example 1 is tested and analyzed, and the sensor sample strip with the length of 50mm, the width of 10mm and the thickness of 0.15mm is prepared in the example 1, and is subjected to 5-cycle tensile test, and the resistance change of the sample strip is tested at the same time. As shown in fig. 2, the spline resistance shows a linear increase with increasing length; as the splines recover, their resistance decreases, exhibiting flexible sensing performance.
Test example 3
The antibacterial function of the multiple-response shape memory polyurethane material prepared by taking TPU, carbomer 940, hydroxyethyl nanocellulose and benzalkonium chloride as raw materials is tested and analyzed, TPU, carbomer 940 and a hydroxyethyl nanocellulose nano reinforcing material are added as a comparative example 3, and the test result is shown in the attached drawing 3.
Test example 4
The shape recovery of the film prepared from the shape memory polyurethane material with multiple responses in example 1 is tested, the sensor with the length of 50mm, the width of 10mm and the thickness of 0.15mm is a sample bar, the sample bar is placed in water for soaking, then is folded in half, is fixed in shape at 85 ℃, is placed in deionized water, and is recovered in shape within 3min, so that a good shape memory effect is shown, as shown in fig. 4.
The above description is only for the purpose of illustrating the preferred embodiments of the present invention and is not to be construed as limiting the invention, and any modifications, equivalents and improvements made within the spirit and principle of the present invention are intended to be included within the scope of the present invention.
Claims (10)
1. The multiple-response shape memory polyurethane material is characterized by comprising the following components in percentage by mass based on 100% of the total mass of the multiple-response shape memory polyurethane:
2. the multiple-response shape memory polyurethane material of claim 1, wherein the acrylic cross-linking resin is carbomer 940.
3. The multiple-response shape memory polyurethane material of claim 1 or 2, wherein the nanoreinforcement material is selected from the group consisting of: hydroxymethyl nanocellulose and/or hydroxyethyl nanocellulose.
4. The multiple-response shape memory polyurethane material of claim 3, wherein the nano-conductive material is selected from the group consisting of: at least one of carbon nano tube, graphene, carbon black and silver nano wire.
5. The multiple response shape memory polyurethane material of claim 1, 2 or 4, wherein the organic antimicrobial material is selected from the group consisting of: at least one of chloramphenicol, aloe vera gel, potassium sorbate, polyhexamethylene biguanide hydrochloride, povidone iodine, chlorhexidine gluconate, and benzalkonium chloride; and/or the presence of a gas in the gas,
the solvent is selected from: at least one of N, N-dimethylformamide, tetrahydrofuran, trichloromethane, dichloromethane and acetone.
6. A preparation method of a multiple-response shape memory polyurethane material is characterized by comprising the following steps:
obtaining a nano conductive material and a solvent, and dispersing the nano conductive material in the solvent to obtain a dispersion liquid of the nano conductive material;
obtaining thermoplastic polyurethane, acrylic crosslinked resin and a nano reinforcing material, and dispersing the thermoplastic polyurethane, the acrylic crosslinked resin and the nano reinforcing material in the solvent to obtain a mixed solution;
adding the dispersion liquid of the nano conductive material into the mixed liquid, and stirring to obtain a conductive shape memory polyurethane dispersion liquid;
and (3) obtaining an organic antibacterial material, adding the organic antibacterial material into the conductive shape memory polyurethane dispersion liquid, and performing dispersion treatment to obtain the multi-response shape memory polyurethane material with antibacterial performance.
7. The method of preparing the multiple response shape memory polyurethane material of claim 6, wherein the step of dispersing the nano conductive material in the solvent comprises: adding the nano conductive material into the solvent, and performing ultrasonic dispersion for 30-60 minutes; and/or the presence of a gas in the gas,
the step of dispersing the thermoplastic polyurethane, the acrylic crosslinked resin, and the nanoreinforcement material in the solvent includes: and adding the thermoplastic polyurethane, the acrylic crosslinked resin and the nano reinforcing material into the solvent at the temperature of 75-90 ℃, and stirring at the speed of 200-600 r/min for 1-2 hours.
8. The method for preparing a multiple response shape memory polyurethane material according to claim 5, wherein the stirring treatment step comprises: adding the dispersion liquid of the nano conductive material into the mixed liquid at the temperature of 75-90 ℃, and stirring at the speed of 200-600 r/min for 2-3 hours; and/or the presence of a gas in the gas,
the step of dispersion treatment comprises: adding the organic antibacterial material into the conductive shape memory polyurethane dispersion liquid at the temperature of 75-90 ℃, and stirring at the speed of 200-600 r/min for 0.5-1 hour.
9. A flexible sensor, characterized by: the method comprises the steps of obtaining the multi-response shape memory polyurethane material according to any one of claims 1 to 5 or the multi-response shape memory polyurethane material prepared by the method according to any one of claims 6 to 8, pouring the multi-response shape memory polyurethane material into a mold, curing for 40 to 60 hours at the temperature of 75 to 90 ℃ to obtain a conductive polyurethane film, and preparing the flexible sensor through a hot pressing process.
10. An electroconductive textile characterized by: obtaining the multiple-response shape memory polyurethane material as defined in any one of claims 1 to 5 or the multiple-response shape memory polyurethane material prepared by the method as defined in any one of claims 6 to 8, and using a wet spinning process to prepare the multiple-response shape memory polyurethane material into shape memory polyurethane fibers; the conductive textile contains the shape memory polyurethane fiber.
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