CN109306070A - A kind of preparation method with nanoparticle orientated polymer fiber foam material - Google Patents
A kind of preparation method with nanoparticle orientated polymer fiber foam material Download PDFInfo
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- CN109306070A CN109306070A CN201810917368.2A CN201810917368A CN109306070A CN 109306070 A CN109306070 A CN 109306070A CN 201810917368 A CN201810917368 A CN 201810917368A CN 109306070 A CN109306070 A CN 109306070A
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J9/00—Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof
- C08J9/04—Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof using blowing gases generated by a previously added blowing agent
- C08J9/12—Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof using blowing gases generated by a previously added blowing agent by a physical blowing agent
- C08J9/122—Hydrogen, oxygen, CO2, nitrogen or noble gases
-
- 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
- D01F6/44—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
-
- 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
- D01F6/88—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof from mixtures of polycondensation products as major constituent with other polymers or low-molecular-weight compounds
- D01F6/94—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof from mixtures of polycondensation products as major constituent with other polymers or low-molecular-weight compounds of other polycondensation products
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2203/00—Foams characterized by the expanding agent
- C08J2203/06—CO2, N2 or noble gases
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2325/00—Characterised by the use of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by an aromatic carbocyclic ring; Derivatives of such polymers
- C08J2325/02—Homopolymers or copolymers of hydrocarbons
- C08J2325/04—Homopolymers or copolymers of styrene
- C08J2325/06—Polystyrene
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2375/00—Characterised by the use of polyureas or polyurethanes; Derivatives of such polymers
- C08J2375/04—Polyurethanes
Abstract
The invention belongs to foam material fields, specifically disclose a kind of preparation method with nanoparticle orientated polymer fiber foam material, specifically include: 1) using thermoplastic polymer as matrix, solution blending composite nano inoganic particle obtains the composite material of nanoparticle and polymer;2) obtained composite material is injected in 180~200 DEG C of capillary rheometer barrel, it is squeezed out with the shear rate of 20~40mm/min, the melt of extrusion is drawn with the draw-down rate of 0.1~50m/min again, obtains the composite polymer fibers of nanoparticle different orientation;3) obtained polymer fiber is foamed, obtains the different polymer fiber foamed material in aperture.The present invention is controlled by the cell morphology to polymer fiber foamed material, so that the electromagnetic shielding performance of material and electric property generate variation, is assigned the unique performance of material, is provided new approaches for the material of new function.
Description
Technical field
The invention belongs to foamed material technical fields, and in particular to one kind has nanoparticle orientated polymer fiber foam
The preparation method of material.
Background technique
Polymer foaming fibrous material with nanoparticle orientation is inhaled due to its unique performance and special structure
The attention of Yin Liao academia and industry.Due to there is the nanoparticle of orientation texture, different orientations in a polymer matrix
Degree can generate different size of aperture, so that the physical mechanical property of material is changed, including its power electricity behavior, electromagnetic screen
Cover behavior.The light-weighted polymer fiber with nanoparticle orientation is widely used in the fields such as sensor, electromagnetic shielding.
Currently, preparing the control method of micropore foamed polymer cell morphology mainly include the following types: 1) control foaming is pressed
Strong: this method mainly will affect the solubility of supercritical fluid in the polymer using the rising of saturation pressure, and solubility is got over
Greatly, nucleating point is more, to control cell diameter.2) control blowing temperature: this method is control blowing temperature in polymer
On glass transition temperature, as temperature increases, viscosity decline, so that bubble growth rate be made to increase to control abscess shape
State.3) polymer blending modification method: two kinds of incompatible polymers are used, nucleation can be generated when dispersed phase is dispersed in continuous phase
The effect of agent, to control cell morphology.4) the additional field of force controls waveforms method: in foaming process, the additional field of force is introduced, thus
Control cell morphology.
The polymeric foamable material of the available different cell morphology of above-mentioned several method, but its all there is lack
Point.Control foaming pressure requires the air-tightness and maximum pressure ability to bear of equipment very high.Blowing temperature is controlled to polymerization
Object is more demanding, and higher temperature can be such that polymer viscosity declines rapidly, makes cell collapse.Polymer blending modification method early period
The technique of polymer blend is more complex.The modes process such as the additional field of force of additional field of force control waveforms method or radiation it is complicated and
It is not easy to realize in Basic Laboratory.
(the polymer composites foaming research Zhejiang [D] with nanoparticle orientation: Zhejiang industry is big by Song Lin et al.
Learn, 2016.) solution blending is utilized and the compound fibre of polymer with different-diameter has been made in Minitype twin-screw extrusion machine
Dimension, but since it is artificial spinning, hauling speed is too low and uncontrollable, the orientation dispersion of nanoparticle in a polymer matrix
Property is poor.
Therefore, seek a kind of simple process, method low for equipment requirements prepares the polymerization with different cell morphologies
Object porous material becomes more urgent.
Summary of the invention
It is an object of the invention to have different nanoparticle degree of orientations by controlling different hauling speed preparations
The method of polymer fiber foamed material, to obtain the controllable foamed material of pore size.
A kind of preparation method with nanoparticle orientated polymer fiber foam material, includes the following steps:
(1) using thermoplastic polymer as matrix, solution blending composite nano inoganic particle obtains nanoparticle and polymer
Composite material;
(2) composite material obtained step (1) injects in 180~200 DEG C of capillary rheometer barrel, with 20~
The shear rate of 40mm/min squeezes out, and obtains melt;The melt of extrusion is drawn with the draw-down rate of 0.1~50m/min again, is obtained
Different composite polymer fibers are orientated to nanoparticle;
(3) polymer fiber that step (2) obtains is foamed, obtains the different polymer fiber foaming material in aperture
Material.
It with the increase of melt spinning draw-down rate, will increase along the power in machine direction, thus in polymer melting
The power that nanoparticulate fillers are applied under process is bigger, and nanoparticle is presented in the polymer along on polymer fiber direction
Arrangement.
When adding nanoparticle in the polymer, nucleation in the polymer is not just spontaneous, due to polymerization
In object caused by additive, additive can reduce the energy barrier of cell nucleation, but this depends on the type and table of additive
The nucleating point of face form, heterogeneous nucleation can preferentially select in the cone-shaped groove on additive surface.
When orientation dispersion is presented in nanoparticle, whether nanoparticle end to end, or on its surface, all
It is possible that will appear multiple heterogeneous nucleation points;But when its mixed and disorderly random dispersion, it is possible to multiple nanoparticles can be made to bridge
Together, so that the quantity of heterogeneous nucleation point declines, the decline of abscess quantity in polymer is eventually led to.
Thermoplastic polymer described in step (1) is any one in polyurethane, polylactic acid, polypropylene or polystyrene
Kind.
Inorganic nano-particle described in step (1) is any in carbon nanotube, graphene or SiC nano fiber
One kind, the carbon nanotube are multi-walled carbon nanotube or single-walled carbon nanotube, and the graphene is single-layer graphene, double-layer graphite
Alkene, few layer graphene or multi-layer graphene.
In step (1), the mass ratio of the inorganic nano-particle and thermoplastic polymer is 0.1~3:100, preferably
0.5~3:100.
If the additive amount of nanoparticle is excessive, the viscosity that will lead to polymeric system becomes larger, thus during the spinning process
Can be easily broken, and additive amount is too many, can make a big impact to the dispersion of nanoparticle;And additive amount is very few, then will lead to out-phase
Nucleating effect is unobvious, seriously limits the application of obtained foamed material.
In step (1), the specific steps of the solution blending are as follows: in a solvent by thermoplastic polymer dissolution, carry out
Magnetic agitation obtains polymer solution;It again disperses nanoparticle in solvent, 30~60min of ultrasound, cell pulverization ultrasound 10
Obtained nanoparticle mixed liquor is added in the polymer solution~20min, and 30~40min of magnetic agitation obtains nanometer
The composite material of particle and polymer.
Preferably, draw-down rate described in step (2) is 2~45m/min, when draw-down rate is too low, can make big
The polymer melt of amount is gathered at the mouth mold of capillary rheometer, and aggregation can then be fallen too much, seriously affects spinning effect;And
When draw-down rate is excessively high, since the melt strength of polymer has certain limitation, polymer fiber can be made to be broken, cannot spun
Silk.
Foaming method described in step (3) are as follows: polymer fiber is put into autoclave, is purged by foaming agent gas
Injection has the foaming agent of pressure in autoclave afterwards, control pressure in 5~30Mpa, at 60~300 DEG C sealing saturation 1~
For 24 hours, rapid pressure release to atmospheric pressure and being put into ice-water bath is cooled to room temperature, and obtains the polymer fiber foamed material.
The foaming agent is carbon dioxide, nitrogen, butane, freon or hydrogeneous chlorine freon.
Compared with prior art, the beneficial effects of the present invention are:
(1) the method for the present invention preparation process is simple, low for equipment requirements;
(2) the method for the present invention hauling speed different by control, can make nanoparticle obtain different degrees of orientation,
The lightweight fibre-forming polymer foamed material of different pore size is made, and then is made with good power electrical property and electromagnetic shielding
The foamed material of performance;
(3) present invention is controlled by the cell morphology to polymer fiber foamed material, so that the electromagnetic screen of material
It covers performance and electric property generates variation, assign the unique performance of material, the preparation for new function material provides new approaches.
Detailed description of the invention
Fig. 1 is the TEM figure of the polymer fiber foamed material obtained under different hauling speeds in embodiment 1;
Fig. 2 is the SEM figure of the polymer fiber foamed material obtained under different hauling speeds in embodiment 1.
Specific embodiment
The invention is further illustrated by the examples, but the present invention is not limited by following embodiment.
Embodiment 1
(1) 30g polyurethane is dissolved by heating in 200mLDMF, magnetic agitation 30min obtains polyurethane solutions;Separately take
150mg carbon nanotube, is dispersed in 100mLDMF, first ultrasound 30min, reuses cell disruptor ultrasound 10min, will
To uniform carbon nanotubes dispersion liquid be added polyurethane solutions in, magnetic agitation 30min, be sufficiently mixed uniformly after obtain mixing it is molten
Liquid, then mixed solution is added in 1000mL methanol while stirring, polyurethane and carbon nano tube compound material is finally precipitated;
(2) after removing solvent, then obtained composite material is added in capillary rheometer, in 180 DEG C of items
Composite material is sufficiently melted under part, is squeezed out with the rate of 40mm/min, then with 1.4m/min, 6.8m/min, 12.2m/min,
The rate of 25.1m/min is distracted into fiber, obtains the polyurethane fiber of different orientation;
(3) fibrous material of obtained different orientation is put into autoclave, in autoclave after being purged by carbon dioxide
Middle injection has the carbon dioxide of pressure, and control pressure is in 13.8Mpa, and sealing saturation is after 12 hours at 100 DEG C, rapid pressure release
It is cooled to room temperature to atmospheric pressure and being put into ice-water bath, takes out sample and obtain the polymerization of different orientation degree, different cell diameters
Object foamed material.
In embodiment 1, the TEM of the polymeric foamable material obtained under the hauling speed of 1.4m/min, 25.1m/min schemes
As shown in Figure 1, as shown in Figure 1, since method for making sample is perpendicular to the direction of fiber, under the hauling speed of 1.4m/min, carbon
Pipe orientation is unobvious, and transverse and longitudinal arrangement is more unordered, however in the case where height draws 25.1m/min rate, carbon pipe can only all be presented one
End is in TEM figure, and therefore, with the increase of hauling speed, degree of orientation can increase therewith.
In embodiment 1, what is obtained under the hauling speed of 1.4m/min, 6.8m/min, 12.2m/min, 25.1m/min is poly-
The SEM figure of object foamed material is closed as shown in Fig. 2, as shown in Figure 2, cell diameter variation is respectively 2.22 ± 1.24,2.15 ±
0.90,2.05 ± 1.13,1.07 ± 0.42, therefore, with the increase of degree of orientation, cell diameter is gradually become smaller, nucleation efficiencies
It gets higher.
Embodiment 2
(1) 30g polyurethane is dissolved by heating in 200mLDMF, magnetic agitation 40min obtains polyurethane solutions;Separately take
180mg graphene, is dispersed in 100mLDMF, and first ultrasound 40min, reuses cell disruptor ultrasound 10min, will obtain
Uniform graphene dispersing solution be added polyurethane solutions in, magnetic agitation 40min, be sufficiently mixed uniformly after obtain mixed solution,
Mixed solution is added in 1000mL methanol while stirring again, the composite material of polyurethane and graphene is finally precipitated;
(2) after removing solvent, obtained composite material is added in capillary rheometer, in 190 DEG C of conditions
It is lower sufficiently to melt composite material, squeezed out with the rate of 40mm/min, then with 1.4m/min, 6.8m/min, 12.2m/min,
The rate of 25.1m/min is distracted into fiber, obtains the polyurethane fiber of different orientation;
(3) fibrous material of obtained different orientation is put into autoclave, in autoclave after being purged by carbon dioxide
Middle injection has the carbon dioxide of pressure, and control pressure is in 15Mpa, at 90 DEG C after sealing saturation 12h, rapid pressure release to atmosphere
It presses and is put into ice-water bath and be cooled to room temperature, take out sample and obtain the polyalcohol stephanoporate of different orientation degree, different cell diameters
Material.
Embodiment 3
(1) 30g polyurethane and 120mg graphene are placed in 180 DEG C of Minitype twin-screw extrusion machine, vacuum mixing
10min, it is ensured that its after mixing, pelletizing obtain graphene filling polyurethane pellet;
(2) obtained pellet is added in capillary rheometer, sufficiently melts composite material under the conditions of 185 DEG C,
Polyurethane composition is squeezed out with the rate of 20mm/min, then with 2.5m/min, 5.0m/min, 10m/min, 20m/min, 30m/
The rate of min is distracted into fiber, the available polyurethane fiber being orientated in various degree;
(3) fibrous material of obtained different orientation is put into autoclave, in autoclave after being purged by carbon dioxide
Middle injection has the carbon dioxide of pressure, and control pressure is in 10Mpa, and at 120 DEG C after sealing saturation 12h, rapid pressure release is to big
Air pressure and being put into ice-water bath is cooled to room temperature, and taking out sample, to obtain different orientation degree, the polymer of different cell diameters more
Porous materials.
Embodiment 4
(1) 30g polystyrene is dissolved by heating in 200mLDMF, magnetic agitation 30min obtains polystyrene solution;
150mg carbon nanotube separately is taken, is dispersed in 100mLDMF, first ultrasound 30min, reuses cell disruptor ultrasound 10min,
Obtain the uniform dispersion of carbon nanotube;Carbon nano tube dispersion liquid is added in polystyrene solution, magnetic agitation 30min,
The mixed solution of polystyrene Yu carbon pipe is obtained after being sufficiently mixed uniformly, then mixed solution is added to 1000mL first while stirring
In alcohol, the composite material of polystyrene and carbon pipe is finally precipitated;
(2) after removing solvent, then obtained composite material is added in capillary rheometer, in 180 DEG C of items
Composite material is sufficiently melted under part, with the rate extruded polystyrene compound of 40mm/min, then with 8m/min, 16m/min,
The rate of 32m/min, 48m/min are distracted into fiber, obtain the styroflex of different carbon pipe orientations;
(3) fibrous material of obtained different orientation is put into autoclave, in autoclave after being purged by carbon dioxide
Middle injection has the carbon dioxide of pressure, and control pressure is in 20Mpa, at 85 DEG C after sealing saturation 12h, rapid pressure release to atmosphere
It presses and is put into ice-water bath and be cooled to room temperature, take out sample and obtain the polyalcohol stephanoporate of different orientation degree, different cell diameters
Material.
Embodiment 5
(1) 30g polystyrene and 240mg SiC nano fiber are placed in 200 DEG C of torque rheologies, in high shear speed
10min is sufficiently mixed under rate, pelletizing obtains the polystyrene pellets of silicon carbide filling;
(2) obtained pellet is added in capillary rheometer, sufficiently melts composite material under the conditions of 200 DEG C,
With the rate extruded polystyrene compound of 30mm/min, then with 5m/min, 10m/min, 15m/min, 20m/min, 25m/min
Rate be distracted into styroflex, obtain the styroflex of different silicon carbide orientation;
(3) fibrous material of obtained different orientation is put into autoclave, in autoclave after being purged by carbon dioxide
Middle injection has the carbon dioxide of pressure, and control pressure is in 13.8Mpa, and at 125 DEG C after sealing saturation 12h, rapid pressure release is extremely
Atmospheric pressure and being put into ice-water bath is cooled to room temperature, and is taken out sample and is obtained the polymer of different orientation degree, different cell diameters
Porous material.
Claims (8)
1. a kind of preparation method with nanoparticle orientated polymer fiber foam material, includes the following steps:
(1) using thermoplastic polymer as matrix, solution blending composite nano inoganic particle obtains answering for nanoparticle and polymer
Condensation material;
(2) in the capillary rheometer barrel of 180~200 DEG C of the composite material injection obtained step (1), with 20~40mm/
The shear rate of min squeezes out, and obtains melt;The melt of extrusion is drawn with the draw-down rate of 0.1~50m/min again, is received
Rice corpuscles is orientated different composite polymer fibers;
(3) polymer fiber that step (2) obtains is foamed, obtains the different polymer fiber foamed material in aperture.
2. having the preparation method of nanoparticle orientated polymer fiber foam material as described in claim 1, feature exists
In in step (1), the thermoplastic polymer is any one in polyurethane, polylactic acid, polypropylene or polystyrene.
3. having the preparation method of nanoparticle orientated polymer fiber foam material as described in claim 1, feature exists
In in step (1), the inorganic nano-particle is any one in carbon nanotube, graphene or SiC nano fiber.
4. having the preparation method of nanoparticle orientated polymer fiber foam material as described in claim 1, feature exists
In in step (1), the mass ratio of the inorganic nano-particle and thermoplastic polymer is 0.1~3:100.
5. having the preparation method of nanoparticle orientated polymer fiber foam material as described in claim 1, feature exists
In, in step (1), the specific steps of the solution blending are as follows: in a solvent by thermoplastic polymer dissolution, carry out magnetic force and stir
It mixes, obtains polymer solution;It again disperses nanoparticle in solvent, 30~60min of ultrasound, cell pulverization ultrasound 10~
Obtained nanoparticle mixed liquor is added in the polymer solution 20min, and 30~40min of magnetic agitation obtains nanoparticle
The composite material of son and polymer.
6. having the preparation method of nanoparticle orientated polymer fiber foam material as described in claim 1, feature exists
In in step (2), the draw-down rate is 2~45m/min.
7. having the preparation method of nanoparticle orientated polymer fiber foam material as described in claim 1, feature exists
In, in step (3), the foaming method are as follows: polymer fiber is put into autoclave, after being purged by foaming agent gas
Injection has the foaming agent of pressure in autoclave, and control pressure is in 5~30Mpa, the sealing saturation 1~for 24 hours at 60~300 DEG C,
Rapid pressure release to atmospheric pressure and being put into ice-water bath is cooled to room temperature, and obtains the polymer fiber foamed material.
8. having the preparation method of nanoparticle orientated polymer fiber foam material as claimed in claim 7, feature exists
In the foaming agent is carbon dioxide, nitrogen, butane, freon or hydrogeneous chlorine freon.
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CN110791079A (en) * | 2019-10-18 | 2020-02-14 | 蔡娟 | Co3O4-composite electromagnetic shielding material of carbon nano tube modified polyurethane |
CN113733507A (en) * | 2021-07-20 | 2021-12-03 | 浙江理工大学 | Preparation method of high-dispersion silicon dioxide nanorod orientation reinforced chemical fiber |
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