CN106245138A - A kind of preparation method of high recovery stress shape memory complex fiber material - Google Patents
A kind of preparation method of high recovery stress shape memory complex fiber material Download PDFInfo
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- CN106245138A CN106245138A CN201610594639.6A CN201610594639A CN106245138A CN 106245138 A CN106245138 A CN 106245138A CN 201610594639 A CN201610594639 A CN 201610594639A CN 106245138 A CN106245138 A CN 106245138A
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- shape memory
- high recovery
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- recovery stress
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- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01F—CHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
- D01F6/00—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof
- D01F6/44—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof from mixtures of polymers obtained by reactions only involving carbon-to-carbon unsaturated bonds as major constituent with other polymers or low-molecular-weight compounds
- D01F6/50—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof from mixtures of polymers obtained by reactions only involving carbon-to-carbon unsaturated bonds as major constituent with other polymers or low-molecular-weight compounds of polyalcohols, polyacetals or polyketals
-
- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01D—MECHANICAL METHODS OR APPARATUS IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS
- D01D1/00—Treatment of filament-forming or like material
- D01D1/02—Preparation of spinning solutions
-
- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01D—MECHANICAL METHODS OR APPARATUS IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS
- D01D5/00—Formation of filaments, threads, or the like
- D01D5/06—Wet spinning methods
-
- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01F—CHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
- D01F1/00—General methods for the manufacture of artificial filaments or the like
- D01F1/02—Addition of substances to the spinning solution or to the melt
- D01F1/10—Other agents for modifying properties
-
- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01F—CHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
- D01F6/00—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof
- D01F6/28—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof from copolymers obtained by reactions only involving carbon-to-carbon unsaturated bonds
- D01F6/34—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof from copolymers obtained by reactions only involving carbon-to-carbon unsaturated bonds comprising unsaturated alcohols, acetals or ketals as the major constituent
Abstract
The invention provides the preparation method of a kind of high recovery stress composite material of shape memory, use liquid phase flow method, utilize fluid layer to make CNT be orientated in the solution;It is then injected in the coagulating bath rotated, makes CNT again be orientated;And utilize the poor solvent of polymer, make polymer flocculation the state of orientation of fixed carbon nanotube, preparation has the composite material of shape memory of high recovery stress, the present invention uses wet spinning to prepare material, wet spinning technology is ripe, production technology of the present invention need not transform existing equipment in a large number, pollution-free, it is easy to industrialized production.
Description
Technical field
The present invention relates to performance function field of compound material, be specifically related to a kind of high recovery stress shape memory composite wood
The preparation method of material.
Background technology
Shape-memory polymer as the intellectual material of a kind of stimuli responsive type, be widely used in micro electronmechanical, hold
The various aspects such as row device, self-healing, biologic medical, space flight, thus increasingly paid close attention to by people.This kind of material is at specific ring
Shape can be changed (such as hot, optical, electrical, magnetic etc.) under the conditions of border;Shape after change is referred to as temporary shapes.When again material being executed
When adding generation deformation during condition, material recovers again original shape.So, claim it to have " memory " function.
When replying deformation due to shape-memory polymer, it is generally in glass transition or melting transition.This makes its time
Combined stress is usual the lowest (mechanical property of macromolecular material), only zero point several MPas to tens MPas.Therefore, for material exists
There is high recovery stress, it is necessary to use other materials to strengthen during deformation.
CNT is the novel enhanced material being widely used in various field, particularly high-performance composite materials field.
CNT can regard the hollow pipe curled into by single or multiple lift Graphene as.Have stronger intermolecular each other
Interact.When CNT is directly blended with polymeric material, polymeric matrix interaction force between CNT
More weak, material still can not produce high recovery stress;And when content of carbon nanotubes is higher, materials processing difficulty.But, carbon nanometer
When pipe content is higher, CNT can limit the warm-up movement of macromolecular chain, and this restriction effect can make the vitrification of polymer turn
Temperature is to elevated temperature excursions [1];Meanwhile, when the CNT degree of orientation is higher, the intermolecular interaction of CNT can strengthen.
Quotation explanation [1] Berriot, J., et al., Gradient of glass transition
temperature in filled elastomers. Europhysics Letters, 2003. 64(1): p. 50-56。
Summary of the invention
The invention provides the preparation method of a kind of high recovery stress composite material of shape memory, use liquid phase flow method,
Fluid layer is utilized to make CNT be orientated in the solution;It is then injected in the coagulating bath rotated, makes CNT again be orientated;And
Utilize the poor solvent of polymer, make polymer flocculation the state of orientation of fixed carbon nanotube, preparation have high recovery stress
Composite material of shape memory.This technique is simple, pollution-free, it is easy to industrialized production.
In order to solve above-mentioned technical problem, the present invention adopts the following technical scheme that
The preparation method of a kind of high recovery stress shape memory complex fiber material, comprises the following steps:
(1) matrix material, reinforcing material are taken;Described matrix material is water soluble polymer material, includes but not limited to polyethylene
Alcohol;Described reinforcing material be can dispersed tubulose in the solution, rod-like nano material, include but not limited to that single wall carbon is received
Mitron, multi-walled carbon nano-tubes;
(2) matrix material is dissolved formation dilute polymer;
(3) reinforcing material is prepared as stable carbon nano-tube solution;
(4) carbon nano-tube solution is mixed with dilute polymer, form spinning solution;
(5) utilize Micro-metering Pumps with the speed of 1ml/min~10ml/min by spinning solution along the conduit stream of 0.5m~1.5m
Dynamic, utilize the shear stress between fluid layer to make CNT be orientated in the solution;
(6) again by spinning solution through spinning head inject rotate coagulating bath in, carry out spinning, reinforcing material rotate produce from
Under mental and physical efforts, secondary orientation, obtains having high recovery stress shape memory composite fibre after flocculation.
Further, in step (2), matrix material is dissolved in deionized water or organic solvent forms dilute polymer.
Further, step (3), specifically, add in deionized water by reinforcing material and surfactant, stirs, then surpasses
Sound disperses, and obtains stable homodisperse carbon nano-tube solution.
Further, the poor solvent that coagulating bath is polyvinyl alcohol in step (6), including dehydrated alcohol, acetone.
Further, the preparation method of a kind of high recovery stress shape memory complex fiber material, it is characterised in that include
Following steps:
(1) weighing polyvinyl alcohol, is dissolved in deionized water, heating for dissolving, makes the polyvinyl alcohol that mass fraction is 5%~15%
Solution;
(2) CNT that mass ratio is 1:1~1:5 is mixed with sodium lauryl sulphate, after ultrasonic disperse 0.5h~3h, system
The most scattered carbon nano-tube solution;
(3) carbon nano-tube solution being mixed with poly-vinyl alcohol solution, after ultrasonic disperse 0.5h~3h, making content of carbon nanotubes is
0~the spinning solution of 20%;
(4) utilize Micro-metering Pumps, with the speed that injection volume is 0.5~10mL/min, spinning solution is flowed through 0.5m~1.5m and lead
Pipe is orientated;Again by spinning solution in spinning head injects the coagulating bath rotated, carry out spinning;Had after polyvinyl alcohol flocculates
There is high recovery stress shape memory composite fibre.
In preparation process, the centrifugal force of the shear stress and rotation that are utilized respectively flowing liquid layer makes CNT carry out two
Secondary orientation, utilizes the poor solvent of polymer in coagulating bath to make fiber quick solidification molding, prepares and have height-oriented answering
Condensating fiber.
The method have the advantages that
(1) present invention uses aligned carbon nanotube fiber, substantially increases polymeric matrix at high temperature (higher than glass transition
Temperature) mechanics ability, and when generally polymeric material is in glass transition, the mechanical property of material has under the order of magnitude
Fall.
(2) when the matrix material that the present invention uses is polyvinyl alcohol, owing to polyvinyl alcohol is a kind of biodegradable height
Molecular material, does not results in " white " and pollutes thus welding.
(3) present invention uses wet spinning to prepare material, and wet spinning technology is ripe, and it is right that production technology of the present invention need not
Existing equipment is transformed in a large number, and production process is simple, it is easy to industrialized production.
Accompanying drawing explanation
The invention will be further described with detailed description of the invention below in conjunction with the accompanying drawings:
Fig. 1 be composite fibre of the present invention prepare schematic diagram;
Fig. 2 is the recovery stress figure of composite fibre of the present invention;
Fig. 3 is the scanning electron microscope (SEM) photograph of composite fibre oblique section of the present invention.
Detailed description of the invention
The invention will be further described below in conjunction with the accompanying drawings:
Embodiment 1:
As Figure 1-3, the preparation method of a kind of high recovery stress shape memory complex fiber material, comprise the following steps:
(1) weighing 4g polyvinyl alcohol, be dissolved in 46g water, heating for dissolving, making mass fraction is 8% poly-vinyl alcohol solution;
(2) weigh CNT and the mixing of 48.4 g deionized waters of 0.6g, after adding 1 g sodium lauryl sulphate, stir 1
Min, after ultrasonic disperse 30 min, forms homodisperse carbon nano-tube solution;
(3) carbon nano-tube solution is mixed with poly-vinyl alcohol solution 1:1 by volume, after ultrasonic disperse 30 min, make spinning
Stock solution;
(4) utilizing Micro-metering Pumps, spinning solution is flowed through 1.5m conduit orientation by the speed with injection volume as 2mL/min;Again will
Spinning solution through spinning head inject rotate coagulating bath in, carbon nanotubes mass fraction is the composite fibre of 13.4%.
100oUnder C after deformation, the maximum recovery stress of this fiber is 166.5MPa.
Embodiment 2:
As Figure 1-3, the preparation method of a kind of high recovery stress shape memory complex fiber material, comprise the following steps:
(1) weigh the polyvinyl alcohol of 3g, be dissolved in the deionized water of 37.5g, heating for dissolving, obtain mass fraction be 8% poly-
Glycohol solution;
(2) weigh CNT and the mixing of 24 g deionized waters of 0.3g, add 0.6 g sodium lauryl sulphate, ultrasonic disperse
After 30 min, form homodisperse carbon nano-tube solution;
(3) carbon nano-tube solution being mixed with poly-vinyl alcohol solution 1:2 by volume, ultrasonic disperse is after 30 minutes,
To spinning solution;
(4) with Micro-metering Pumps by spinning solution with injection flow as 2ml/min, along leading the conduit of 1.5m;Again by spinning solution
In spinning head injects the coagulating bath rotated, carry out spinning;Obtaining carbon nanotubes mass fraction after polyvinyl alcohol flocculates is
The composite fibre of 7.2%.
100oUnder C after deformation, the maximum recovery stress of this fiber is more than 123MPa.
Embodiment 3:
As Figure 1-3, the preparation method of a kind of high recovery stress shape memory complex fiber material, comprise the following steps:
(1) weigh the polyvinyl alcohol of 5g, be dissolved in the deionized water of 62.5g, heating for dissolving, obtain mass fraction be 8% poly-
Glycohol solution;
(2) CNT and the mixing of 24 g deionized waters of 0.16g are weighed, after adding 0.32 g sodium lauryl sulphate (SDS)
Stir 1 min, after ultrasonic disperse 30 min, form homodisperse carbon nano-tube solution;
(3) carbon nano-tube solution being mixed with poly-vinyl alcohol solution 1:2 by volume, ultrasonic disperse is after 30 minutes,
To spinning solution;
(4) will utilize Micro-metering Pumps, spinning solution is flowed through 1.5m conduit orientation by the speed with injection volume as 2mL/min;Again
By spinning solution in spinning head injects the coagulating bath (dehydrated alcohol) rotated, after polyvinyl alcohol flocculates, obtain carbon nanotubes
Mass fraction is the composite fibre of 4%.
100oUnder C after deformation, the maximum recovery stress about 87MPa of this fiber.
Embodiment 4:
The not preparation method of the vinal of carbon nanotubes, comprises the following steps:
(1) weighing the polyvinyl alcohol of 2g, be dissolved in the deionized water of 23g, heating for dissolving two is little, and obtaining mass fraction is 8%
Poly-vinyl alcohol solution;
(2) preparation of polymer fiber
It is 2 mL/mins by poly-vinyl alcohol solution with injection flow with Micro-metering Pumps, along leading the conduit of 1.5m, by mixed solution
In spinning head injects the coagulating bath (dehydrated alcohol) rotated, after polyvinyl alcohol flocculates, the poly-second of not carbon containing nanometer
Enol fiber.
100oUnder C after deformation, the maximum recovery stress of this fiber is only 32.9MPa.
Claims (5)
1. the preparation method of one kind high recovery stress shape memory complex fiber material, it is characterised in that comprise the following steps:
(1) matrix material, reinforcing material are taken;Described matrix material is water soluble polymer material, includes but not limited to polyethylene
Alcohol;Described reinforcing material be can dispersed tubulose in the solution, rod-like nano material, include but not limited to that single wall carbon is received
Mitron, multi-walled carbon nano-tubes;
(2) matrix material is dissolved formation dilute polymer;
(3) reinforcing material is prepared as stable carbon nano-tube solution;
(4) carbon nano-tube solution is mixed with dilute polymer, form spinning solution;
(5) utilize Micro-metering Pumps with the speed of 1ml/min~10ml/min by spinning solution along the conduit stream of 0.5m~1.5m
Dynamic, utilize the shear stress between fluid layer to make CNT be orientated in the solution;
(6) again by spinning solution through spinning head inject rotate coagulating bath in, carry out spinning, reinforcing material rotate produce from
Under mental and physical efforts, secondary orientation, obtains having high recovery stress shape memory composite fibre after flocculation.
The preparation method of a kind of high recovery stress shape memory complex fiber material the most according to claim 1, its feature
Being, in step (2), matrix material is dissolved in deionized water or organic solvent forms dilute polymer.
The preparation method of a kind of high recovery stress shape memory complex fiber material the most according to claim 1, its feature
Being, step (3), specifically, add in deionized water by reinforcing material and surfactant, stirs, then ultrasonic disperse, obtains
Stable homodisperse carbon nano-tube solution.
The preparation method of a kind of high recovery stress shape memory complex fiber material the most according to claim 1, its feature
Being, the poor solvent that coagulating bath is polyvinyl alcohol in step (6), including dehydrated alcohol, acetone.
The preparation method of a kind of high recovery stress shape memory complex fiber material the most according to claim 1, its feature
It is, comprises the following steps:
(1) weighing polyvinyl alcohol, is dissolved in deionized water, heating for dissolving, makes the polyvinyl alcohol that mass fraction is 5%~15%
Solution;
(2) CNT that mass ratio is 1:1~1:5 is mixed with sodium lauryl sulphate, after ultrasonic disperse 0.5h~3h, system
The most scattered carbon nano-tube solution;
(3) carbon nano-tube solution being mixed with poly-vinyl alcohol solution, after ultrasonic disperse 0.5h~3h, making content of carbon nanotubes is
0~the spinning solution of 20%;
(4) utilize Micro-metering Pumps, with the speed that injection volume is 0.5~10mL/min, spinning solution is flowed through 0.5m~1.5m and lead
Pipe is orientated;Again by spinning solution in spinning head injects the coagulating bath rotated, carry out spinning;Had after polyvinyl alcohol flocculates
There is high recovery stress shape memory composite fibre.
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Cited By (7)
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CN108103766A (en) * | 2017-12-29 | 2018-06-01 | 成都新柯力化工科技有限公司 | A kind of molybdenum disulfide composite fibre photochemical catalyst and preparation method for sewage disposal |
CN109576822A (en) * | 2018-11-29 | 2019-04-05 | 中国科学院金属研究所 | A method of preparing single-walled carbon nanotube fiber and its composite fibre |
CN111575867A (en) * | 2020-05-26 | 2020-08-25 | 苏州海天运动器材有限公司 | Novel elastic net material for trampoline |
CN112160037A (en) * | 2020-10-16 | 2021-01-01 | 武汉智达纺织科技有限公司 | Preparation method of oxidized carbon nanotube modified polyvinyl alcohol shape memory fiber |
CN112410927A (en) * | 2020-11-19 | 2021-02-26 | 南开大学 | Stretchable carbon nanotube/organic composite thermoelectric fiber and preparation method and application thereof |
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CN108103766A (en) * | 2017-12-29 | 2018-06-01 | 成都新柯力化工科技有限公司 | A kind of molybdenum disulfide composite fibre photochemical catalyst and preparation method for sewage disposal |
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CN109576822A (en) * | 2018-11-29 | 2019-04-05 | 中国科学院金属研究所 | A method of preparing single-walled carbon nanotube fiber and its composite fibre |
CN111575867A (en) * | 2020-05-26 | 2020-08-25 | 苏州海天运动器材有限公司 | Novel elastic net material for trampoline |
CN112160037A (en) * | 2020-10-16 | 2021-01-01 | 武汉智达纺织科技有限公司 | Preparation method of oxidized carbon nanotube modified polyvinyl alcohol shape memory fiber |
CN112160037B (en) * | 2020-10-16 | 2024-03-12 | 聚源材料科技(遵义)有限公司 | Preparation method of oxidized carbon nanotube modified polyvinyl alcohol shape memory fiber |
CN112410927A (en) * | 2020-11-19 | 2021-02-26 | 南开大学 | Stretchable carbon nanotube/organic composite thermoelectric fiber and preparation method and application thereof |
CN112410927B (en) * | 2020-11-19 | 2022-06-14 | 南开大学 | Stretchable carbon nanotube/organic composite thermoelectric fiber and preparation method and application thereof |
CN113235182A (en) * | 2021-04-09 | 2021-08-10 | 大连理工大学 | Preparation method of high-flexibility carbon nanotube fiber |
CN113235182B (en) * | 2021-04-09 | 2022-04-15 | 大连理工大学 | Preparation method of high-flexibility carbon nanotube fiber |
CN114381812A (en) * | 2022-01-24 | 2022-04-22 | 中国科学院苏州纳米技术与纳米仿生研究所 | Spinning nozzle, nano material assembly and preparation method thereof |
CN114381812B (en) * | 2022-01-24 | 2023-07-21 | 中国科学院苏州纳米技术与纳米仿生研究所 | Spinning nozzle, nano material assembly and preparation method of nano material assembly |
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