CN108467517A - A kind of preparation method of high intensity water-responsive cellulose base composite material of shape memory - Google Patents
A kind of preparation method of high intensity water-responsive cellulose base composite material of shape memory Download PDFInfo
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- CN108467517A CN108467517A CN201810104965.3A CN201810104965A CN108467517A CN 108467517 A CN108467517 A CN 108467517A CN 201810104965 A CN201810104965 A CN 201810104965A CN 108467517 A CN108467517 A CN 108467517A
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- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J5/00—Manufacture of articles or shaped materials containing macromolecular substances
- C08J5/18—Manufacture of films or sheets
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- C08B15/00—Preparation of other cellulose derivatives or modified cellulose, e.g. complexes
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- C08J3/02—Making solutions, dispersions, lattices or gels by other methods than by solution, emulsion or suspension polymerisation techniques
- C08J3/03—Making solutions, dispersions, lattices or gels by other methods than by solution, emulsion or suspension polymerisation techniques in aqueous media
- C08J3/075—Macromolecular gels
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- C08J2301/00—Characterised by the use of cellulose, modified cellulose or cellulose derivatives
- C08J2301/02—Cellulose; Modified cellulose
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- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
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Abstract
The invention discloses a kind of preparation methods of high intensity water-responsive cellulose base composite material of shape memory.Dry sisal hemp nano-cellulose is weighed, alkalizes, soak in NaOH aqueous solutions.It is added with stirring absolute ethyl alcohol, monoxone is added in mixed solution, 2 ~ 3h is reacted at 70 DEG C.Centrifugation, is dried to obtain the crude product of monoxone g-sisal Fiber element.Crude product is mixed into high-speed stirred with deionized water and shears 1 ~ 2h, obtains the product of transparent g., jelly-like.It is diluted, is centrifuged at a high speed with deionized water, it is monoxone grafting sisal hemp nano-cellulose to take the solution on centrifuge tube top 80%.Monoxone is grafted sisal hemp nano-cellulose and graphene oxide is added in deionized water and is uniformly mixed, is filtered to obtain the aquagel membrane of cake shape with sand core filter.Then dry in air dry oven, obtain high intensity water-responsive cellulose base composite material of shape memory.The method of the present invention is easy to operate, and institute's prepared material has high water-responsive sensibility, invertibity.
Description
Technical field
The invention belongs to shape memory biology base technical field of function materials.More particularly to a kind of high intensity water-responsive fiber
The preparation method of plain base shape memory composite material.
Background technology
Shape-memory polymer (Shape Memory Polymers, SMPs) is most typical in intellectual material family
A member.It is primarily referred to as the polymer with certain original shape, by certain external influence, after deformation is fixed, then passes through light
Energy, electric energy, thermal energy, biological energy source, electrochemical conditions change(Acid-base value, chelatropic reaction and phase transition)Etc. external conditions stimulation again can be with
Restore the polymer of original-shape.Just because of there is this special performance, SMPs to be with a wide range of applications, it is small to daily
Food vessel apparatus in life, arrive greatly engineer application, space flight and aviation, bio-medical, intelligence weaving, sensing display part, oneself
The fields such as autocontrol system.It is especially played a very important role in biologic medical Material Field, present medical material has been reported
Road there is artificial muscle, artificial skin, drug to automatically engage in system, operation suture thread, holder, heart valve (Biomimetic membranes
Material), organizational project etc..With traditional marmem (Shape Memory Alloys, SMA) and shape memory ceramics
(Shape Memory Ceramics, SMC) both materials are compared, and SMPs has the following advantages:(1) it is higher elasticity and
Good reversibility;(2) structure designability is strong, adjustable, and recovery temperature can adjust chemically, controllable
Recovery behavior, it is easy to accomplish multiple response remember, multiple temperature region, Multiple Shape;(3) it prepares simply, raw material is extensive, and valence
Lattice are cheap;(4) processing and forming is easy, readily available complicated material;(5) bio-compatible performance is preferable, can natural degradation
Material;(6) density is low, etc..
Under normal conditions, applications of the thermotropic SMPs in biomedical or certain low temperature fields has larger limitation
Property, in biomedicine, excessive heat can generate tissue of biological cells certain damage.Water-responsive shape polymer can have
The deficiency for making up this respect of effect, compared with other shapes memory material, water-responsive shape polymer is led in biomedical applications
Domain has unique advantage.
Currently, the water-responsive memory polymer material major part that document is reported is prepared using petrochemical materials
, there are non-renewable, not biodegradable, and the shortcomings that poor biocompatibility.Therefore, it prepares with high intensity, water-responsive,
Biodegradable cellulose base shape-memory material is particularly important.The present invention is grafted sisal hemp nano-cellulose with monoxone
For basis material, graphene oxide is reinforced phase, by simply depressurizing suction method, is prepared a kind of with high intensity, water sound
Answer cellulose base composite material of shape memory.
Invention content
The object of the present invention is to provide a kind of preparation methods of high intensity water-responsive cellulose base composite material of shape memory.
The specific steps are:
(1) the sisal hemp nano-cellulose for weighing 10 ~ 14g dryings, is put into the NaOH aqueous solutions of a concentration of 10wt% of 50 ~ 70mL
It alkalizes, soak 4 ~ 6min, the sisal hemp nano-cellulose soaked is transferred in three-necked flask, 300 ~ 350mL absolute ethyl alcohols are added
Make solvent and mechanical agitation 30min, 3 ~ 7g monoxones are then added, is warming up to 2 ~ 3h of reaction under 70 DEG C of mechanical agitations, reaction knot
Shu Houyong distilled water is centrifuged repeatedly washing and is in neutrality to pH value, is dried to obtain the crude product of monoxone g-sisal Fiber element, will
Crude product is mixed with the deionized water of 100 ~ 200mL, by mixed liquor homogenizer 1 ~ 2h of high speed shear, obtains transparent jelly
The product of shape is added the dilution of 100 ~ 200mL deionized waters, then centrifuges 30 ~ 40min with the rotating speed of 6000 r/min, take
The solution on centrifuge tube top 80% is monoxone grafting sisal hemp nano-cellulose.
(2) graphene oxide is prepared using modified Hummers methods(Abbreviation GO).
(3) graphene oxide made from monoxone grafting sisal hemp nano-cellulose made from step (1) and step (2) is pressed
It is 95 ~ 99.7 according to the ratio between mass percent:It is added in deionized water and is uniformly mixed after 0.3 ~ 5 weighing, obtained mixed dispersion liquid, two
The sum of mass percent of person is 100%, and the water removed in mixed dispersion liquid is then filtered with sand core filter, obtains cake shape
Aquagel membrane, dry 48h at 35 DEG C, allows moisture slowly to vapor away completely in air dry oven, you can high intensity water is made
Respond cellulose base composite material of shape memory.
Compared with the prior art, the present invention has the following advantages:
(1) preparation method is simple, easy to utilize.
(2) there is high water-responsive sensibility, invertibity.The materials such as shape memory elastic body, bio-medical can be used as
It uses.
Specific implementation mode
In order to enable those skilled in the art to be further understood that the feature and technology contents of the present invention, below with embodiment
It is described further, but protection domain is not limited by this.
Embodiment 1:
(1) the sisal hemp nano-cellulose for weighing 12g dryings is put into the NaOH aqueous solutions of a concentration of 10wt% of 60mL and alkalizes, soaks
The sisal hemp nano-cellulose soaked is transferred in three-necked flask by wet 5min, and addition 325mL absolute ethyl alcohols make solvent and machinery stirs
30min is mixed, 5g monoxones are then added, is warming up under 70 DEG C of mechanical agitations and reacts 2.5h, after reaction repeatedly with distilled water
Centrifuge washing to pH value is in neutrality, and is dried to obtain the crude product of monoxone g-sisal Fiber element, by going for crude product and 150mL
Ionized water mixes, and by mixed liquor homogenizer high speed shear 1.5h, obtains the product of transparent g., jelly-like, and 150mL is added and goes
Ionized water dilutes, and then centrifuges 35min with the rotating speed of 6000 r/min, it is chloroethene to take the solution on centrifuge tube top 80%
Acid grafting sisal hemp nano-cellulose.
(2) graphene oxide is prepared using modified Hummers methods.
(3) by oxygen made from monoxone grafting sisal hemp nano-cellulose made from 99.7g steps (1) and 0.3g steps (2)
Stirring in 160mL deionized waters is added in graphite alkene, ultrasonic disperse makes it be uniformly mixed, and mixed dispersion liquid is made, then uses sand
Core filter(Using polytetrafluoroethylene film as filter membrane)The water removed in mixed dispersion liquid is filtered, the hydrogel of cake shape is obtained
Film, then stripping removes polytetrafluoroethylene film in water, so as not to it is damaged;It is smooth that Nanometer composite hydrogel is finally moved on into surface
On sheet glass, dry 48h at 35 DEG C, allows moisture slowly to vapor away completely in air dry oven, you can high intensity water is made and rings
Answer cellulose base composite material of shape memory.
The mechanical property and shape of high intensity water-responsive cellulose base composite material of shape memory made from the present embodiment are remembered
It is as follows to recall the performance test results:
(1) mechanical property:Tensile strength reaches 139.7MPa, stretch modulus 5.77GPa, elongation at break 13%.
(2) shape-memory properties:Sample is folded under the conditions of 60 DEG C and forms U-shaped temporary shapes, constant external force, cooling
To 0 DEG C, the temporary shape of fixed sample.Shape fixed rate is up to 95% or more.It immerses again in 25 DEG C of deionized waters after 27s, shape
Response rate is 95%.
Embodiment 2:
(1) the sisal hemp nano-cellulose for weighing 12g dryings is put into the NaOH aqueous solutions of a concentration of 10wt% of 60mL and alkalizes, soaks
The sisal hemp nano-cellulose soaked is transferred in three-necked flask by wet 5min, and addition 325mL absolute ethyl alcohols make solvent and machinery stirs
30min is mixed, 5g monoxones are then added, is warming up under 70 DEG C of mechanical agitations and reacts 2.5h, after reaction repeatedly with distilled water
Centrifuge washing to pH value is in neutrality, and is dried to obtain the crude product of monoxone g-sisal Fiber element, by going for crude product and 150mL
Ionized water mixes, and by mixed liquor homogenizer high speed shear 1.5h, obtains the product of transparent g., jelly-like, and 150mL is added and goes
Ionized water dilutes, and then centrifuges 35min with the rotating speed of 6000 r/min, it is chloroethene to take the solution on centrifuge tube top 80%
Acid grafting sisal hemp nano-cellulose.
(2) graphene oxide is prepared using modified Hummers methods.
(3) by oxygen made from monoxone grafting sisal hemp nano-cellulose made from 99.5g steps (1) and 0.5g steps (2)
Stirring in 160mL deionized waters is added in graphite alkene, ultrasonic disperse makes it be uniformly mixed, and mixed dispersion liquid is made, then uses sand
Core filter(Using polytetrafluoroethylene film as filter membrane)The water removed in mixed dispersion liquid is filtered, the hydrogel of cake shape is obtained
Film, then stripping removes polytetrafluoroethylene film in water, so as not to it is damaged;It is smooth that Nanometer composite hydrogel is finally moved on into surface
On sheet glass, dry 48h at 35 DEG C, allows moisture slowly to vapor away completely in air dry oven, you can high intensity water is made and rings
Answer cellulose base composite material of shape memory.
The mechanical property and shape of high intensity water-responsive cellulose base composite material of shape memory made from the present embodiment are remembered
It is as follows to recall the performance test results:
(1) mechanical property:Tensile strength is up to 183.4MPa, stretch modulus 8.54GPa, elongation at break 14%.
(2) shape-memory properties:Sample is folded under the conditions of 60 DEG C and forms U-shaped temporary shapes, constant external force, cooling
To 0 DEG C, the temporary shape of fixed sample.Shape fixed rate is up to 95% or more.It immerses again in 25 DEG C of deionized waters after 14s, shape
Response rate is 95%.
Embodiment 3:
(1) the sisal hemp nano-cellulose for weighing 12g dryings is put into the NaOH aqueous solutions of a concentration of 10wt% of 60mL and alkalizes, soaks
The sisal hemp nano-cellulose soaked is transferred in three-necked flask by wet 5min, and addition 325mL absolute ethyl alcohols make solvent and machinery stirs
30min is mixed, 5g monoxones are then added, is warming up under 70 DEG C of mechanical agitations and reacts 2.5h, after reaction repeatedly with distilled water
Centrifuge washing to pH value is in neutrality, and is dried to obtain the crude product of monoxone g-sisal Fiber element, by going for crude product and 150mL
Ionized water mixes, and by mixed liquor homogenizer high speed shear 1.5h, obtains the product of transparent g., jelly-like, and 150mL is added and goes
Ionized water dilutes, and then centrifuges 35min with the rotating speed of 6000 r/min, it is chloroethene to take the solution on centrifuge tube top 80%
Acid grafting sisal hemp nano-cellulose.
(2) graphene oxide is prepared using modified Hummers methods.
(3) by monoxone grafting sisal hemp nano-cellulose made from 98g steps (1) and 2g steps (2) oxidation stone obtained
Stirring in 170mL deionized waters is added in black alkene, ultrasonic disperse makes it be uniformly mixed, and mixed dispersion liquid is made, then with sand core mistake
Filter(Using polytetrafluoroethylene film as filter membrane)The water removed in mixed dispersion liquid is filtered, obtains the aquagel membrane of cake shape, so
Stripping removes polytetrafluoroethylene film in water afterwards, so as not to it is damaged;Nanometer composite hydrogel is finally moved on into the smooth glass in surface
On piece, dry 48h at 35 DEG C, allows moisture slowly to vapor away completely, you can it is fine that high intensity water-responsive is made in air dry oven
The plain base shape memory composite material of dimension.
The mechanical property and shape of high intensity water-responsive cellulose base composite material of shape memory made from the present embodiment are remembered
It is as follows to recall the performance test results:
(1) mechanical property:Tensile strength is up to 167.5MPa, stretch modulus 8.17GPa, elongation at break 9%.
(2) shape-memory properties:Sample is folded under the conditions of 60 DEG C and forms U-shaped temporary shapes, constant external force, cooling
To 0 DEG C, the temporary shape of fixed sample.Shape fixed rate is up to 95% or more.It immerses again in 25 DEG C of deionized waters after 22s, shape
Response rate is 95%.
Claims (1)
1. a kind of preparation method of high intensity water-responsive cellulose base composite material of shape memory, it is characterised in that specific steps
For:
(1) the sisal hemp nano-cellulose for weighing 10 ~ 14g dryings, is put into the NaOH aqueous solutions of a concentration of 10wt% of 50 ~ 70mL
It alkalizes, soak 4 ~ 6min, the sisal hemp nano-cellulose soaked is transferred in three-necked flask, 300 ~ 350mL absolute ethyl alcohols are added
Make solvent and mechanical agitation 30min, 3 ~ 7g monoxones are then added, is warming up to 2 ~ 3h of reaction under 70 DEG C of mechanical agitations, reaction knot
Shu Houyong distilled water is centrifuged repeatedly washing and is in neutrality to pH value, is dried to obtain the crude product of monoxone g-sisal Fiber element, will
Crude product is mixed with the deionized water of 100 ~ 200mL, by mixed liquor homogenizer 1 ~ 2h of high speed shear, obtains transparent jelly
The product of shape is added the dilution of 100 ~ 200mL deionized waters, then centrifuges 30 ~ 40min with the rotating speed of 6000 r/min, take
The solution on centrifuge tube top 80% is monoxone grafting sisal hemp nano-cellulose;
(2) graphene oxide is prepared using modified Hummers methods;
(3) by graphene oxide made from monoxone grafting sisal hemp nano-cellulose made from step (1) and step (2) according to matter
It is 95 ~ 99.7 to measure the ratio between percentage:It is added in deionized water and is uniformly mixed after 0.3 ~ 5 weighing, mixed dispersion liquid is made, the two
The sum of mass percent is 100%, and the water removed in mixed dispersion liquid is then filtered with sand core filter, obtains the water of cake shape
Gel mould, dry 48h at 35 DEG C, allows moisture slowly to vapor away completely, you can high intensity water-responsive is made in air dry oven
Cellulose base composite material of shape memory.
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Cited By (3)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN110408080A (en) * | 2019-08-13 | 2019-11-05 | 沈阳航空航天大学 | Graphene oxide and its composite nano fiber element conductive flexible film and its preparation method |
CN110760092A (en) * | 2019-09-27 | 2020-02-07 | 中国科学院青岛生物能源与过程研究所 | Water-driven shape memory high-strength moisture-sensitive cellulose membrane and preparation method thereof |
CN111925553A (en) * | 2020-07-30 | 2020-11-13 | 西安工程大学 | Preparation method of badminton head |
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CN106832428A (en) * | 2017-01-10 | 2017-06-13 | 西安交通大学 | A kind of rapid water response shape memory composite material and preparation method thereof |
CN106947133A (en) * | 2017-02-10 | 2017-07-14 | 北京化工大学 | A kind of water-responsive elastomer functional composite material and preparation method thereof |
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CN105602213A (en) * | 2015-12-29 | 2016-05-25 | 哈尔滨工业大学 | Preparation of shape memory micro-nano composite material and application of shape memory micro-nano composite material in 4D (four-dimensional) printing |
CN106832428A (en) * | 2017-01-10 | 2017-06-13 | 西安交通大学 | A kind of rapid water response shape memory composite material and preparation method thereof |
CN106947133A (en) * | 2017-02-10 | 2017-07-14 | 北京化工大学 | A kind of water-responsive elastomer functional composite material and preparation method thereof |
Non-Patent Citations (1)
Title |
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Cited By (3)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN110408080A (en) * | 2019-08-13 | 2019-11-05 | 沈阳航空航天大学 | Graphene oxide and its composite nano fiber element conductive flexible film and its preparation method |
CN110760092A (en) * | 2019-09-27 | 2020-02-07 | 中国科学院青岛生物能源与过程研究所 | Water-driven shape memory high-strength moisture-sensitive cellulose membrane and preparation method thereof |
CN111925553A (en) * | 2020-07-30 | 2020-11-13 | 西安工程大学 | Preparation method of badminton head |
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