CN108559277A - A kind of bioabsorbable polymer material and preparation method thereof of carbon nanotube enhancing - Google Patents
A kind of bioabsorbable polymer material and preparation method thereof of carbon nanotube enhancing Download PDFInfo
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- CN108559277A CN108559277A CN201810458778.5A CN201810458778A CN108559277A CN 108559277 A CN108559277 A CN 108559277A CN 201810458778 A CN201810458778 A CN 201810458778A CN 108559277 A CN108559277 A CN 108559277A
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- carbon nanotube
- polymer material
- bioabsorbable polymer
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- nano cellulose
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L89/00—Compositions of proteins; Compositions of derivatives thereof
- C08L89/04—Products derived from waste materials, e.g. horn, hoof or hair
- C08L89/06—Products derived from waste materials, e.g. horn, hoof or hair derived from leather or skin, e.g. gelatin
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B32/00—Carbon; Compounds thereof
- C01B32/15—Nano-sized carbon materials
- C01B32/158—Carbon nanotubes
- C01B32/16—Preparation
- C01B32/162—Preparation characterised by catalysts
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B2202/00—Structure or properties of carbon nanotubes
- C01B2202/06—Multi-walled nanotubes
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B2202/00—Structure or properties of carbon nanotubes
- C01B2202/20—Nanotubes characterized by their properties
- C01B2202/34—Length
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B2202/00—Structure or properties of carbon nanotubes
- C01B2202/20—Nanotubes characterized by their properties
- C01B2202/36—Diameter
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- C—CHEMISTRY; METALLURGY
- 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
- C08K2201/00—Specific properties of additives
- C08K2201/011—Nanostructured additives
Abstract
The invention discloses a kind of bioabsorbable polymer materials and preparation method thereof of carbon nanotube enhancing.It is evenly dispersed in the bioabsorbable polymer material to have directional carbon nanotube array and nano cellulose crystal.While the bioabsorbable polymer material of the carbon nanotube enhancing of the present invention in bioabsorbable polymer material by disperseing directional carbon nanotube array, nano cellulose crystal is added.Nano cellulose crystal has distinctive colloid size, can form stable suspension in water for a long time, to improve its dispersibility in system and with the compatibility of matrix, there is low-density, high intensity and biodegradability；Reunion when to effectively prevent carbon nanotube to disperse in bioabsorbable polymer material enhances the combination between carbon nanotube and bioabsorbable polymer material, improves the storage stability of material.
Description
Technical field
The present invention relates to biomedical material technologies, and in particular to a kind of boiomacromolecule material of carbon nanotube enhancing
Material and preparation method thereof.
Background technology
There is carbon nanotube the network structure of hollow tubular, draw ratio to be up to 100~1000 quasi one-dimensional material.Due to carbon
There is nanotube good axial stability it to be made to show good non-deformability, have high intensity, toughness and bullet
Property modulus.
By preparing the bioabsorbable polymer material of carbon nanotube enhancing, bioabsorbable polymer material good biological phase can kept
While capacitive, its mechanical property and electric property are substantially improved, obtains the bio-medical material haveing excellent performance.
But simple addition carbon nanotube can cause carbon nanotube dispersibility bad, place will appear lamination for a long time,
The storage stability of material is influenced, therefore is greatly limited in the application.
Invention content
In order to solve the above technical problems, the present invention provides bioabsorbable polymer material and its preparation of a kind of carbon nanotube enhancing
Method.While by disperseing directional carbon nanotube array in bioabsorbable polymer material, nano cellulose crystal is added.Nanometer
Cellulose crystals have distinctive colloid size, stable suspension can be formed in water for a long time, to improve it in body
Dispersibility in system and the compatibility with matrix have low-density, high intensity and biodegradability；To effectively prevent carbon to receive
Reunion when mitron disperses in bioabsorbable polymer material enhances the combination between carbon nanotube and bioabsorbable polymer material,
Improve the storage stability of material.
To achieve the goals above, the present invention uses following technical scheme：
One aspect of the present invention provides a kind of bioabsorbable polymer material of carbon nanotube enhancing, in the bioabsorbable polymer material uniformly
It is dispersed with directional carbon nanotube array and nano cellulose crystal.
Preferably, the mass content of the carbon nanotube is 1%-10%；The mass content of the nano cellulose crystal is
1%-10%。
Another aspect of the present invention also provides the preparation method of the bioabsorbable polymer material of above-mentioned carbon nanotube enhancing, including with
Lower step：
S1, directional carbon nanotube array is prepared
Directional carbon nanotube array is prepared using chemical vapor deposition (CVD) technology.
Specifically, using resistance stove heat, use quartz glass tube as reactor.It is received using quartz glass plate as orientation carbon
The growth substrate of mitron, is equipped on quartz boat, is placed among reative cell.Carbon source, catalyst and carrier gas (hydrogen and argon gas)
It is introduced from one end of quartz ampoule, tail gas is discharged from the other end.Carbon source is carbon monoxide or hydrocarbon such as methane, ethane, second
Alkene, propylene etc. control the flow of carbon source with mass flowmenter control valve.If needing in advance to apply catalyst using loaded catalyst
Onto substrate；If using floating catalyst, need a spraying system (such as delicate flow pump) by the catalyst injection of gasification
Into carbon source air-flow.The growing method for being generally oriented carbon nanotube is first to use argon gas or other inert gas purge reactors to anti-
It answers device to reach reaction temperature, gas is then switched into carbon source, cut gas after directional carbon nanotube array is grown
It gains inert gas and is cooled to room temperature, take out sample.The carbon nanotube prepared in this way is generally multi-wall carbon nano-tube
It manages (5~100nm of external diametrical extent), the growth length of carbon nanotube depends on the supply of carbon source or even growth length can reach
6mm。
S2, preparation are dispersed with the polymeric sol of nano cellulose crystal
High molecular polymer and nano cellulose crystal are added in deionized water, being configured to high molecular polymer mass fraction is
20~40% aqueous solution stirs in 50~95 DEG C of waters bath with thermostatic control to solid polymer uniform dissolution；Finally, it will be uniformly dissolved
Polymeric sol stand cooling at room temperature, until bubble drains.
The high molecular polymer is the avirulent high molecular polymer for being suitable for biomedicine field, poly- selected from shell
One or more mixtures in sugar, gelatin, hyaluronic acid, sodium alginate.
S3, polymeric sol is penetrated into carbon nanotube precast body
Directional carbon nanotube array made from S1 is dispersed in plane mould, then to slowly penetrate into mold macromolecule molten
Glue makes polymeric sol enveloped carbon nanometer tube precast body, obtains mixture.
S4, freeze-thaw method prepare the bioabsorbable polymer material of carbon nanotube enhancing
Freeze-thaw circulation processing is carried out to the mixture that S3 is obtained.Specifically, cryogenic temperature -25~-15 DEG C, cooling time 5
It~12 hours, then thaws 5~12 hours at room temperature, such freeze-thaw circulation 3~8 times obtains carbon nanotube enhancing
Bioabsorbable polymer material.
Beneficial effects of the present invention
The bioabsorbable polymer material of carbon nanotube enhancing provided by the invention in bioabsorbable polymer material by disperseing orientation carbon
While nano-tube array, nano cellulose crystal is added.Nano cellulose crystal has distinctive colloid size, when can be long
Between form stable suspension in water, to improve its dispersibility in system and with the compatibility of matrix, have low close
Degree, high intensity and biodegradability；Reunion when to effectively prevent carbon nanotube to disperse in bioabsorbable polymer material increases
Strong combination between carbon nanotube and bioabsorbable polymer material, improves the storage stability of material.
Specific implementation mode
The present invention is specifically described below by embodiment, it is necessary to which indicated herein is that the present embodiment is served only for pair
The present invention is further described, and should not be understood as limiting the scope of the invention, and the person skilled in the art in the field can
To make some nonessential modifications and adaptations according to the content invented above.In the absence of conflict, the reality in the present invention
The feature applied in example and embodiment can be combined with each other.
Embodiment 1
S1, by 5g ferrocene powder, be dissolved in 50mL toluene.Stand 24 hours after mixing.Quartz glass plate is equipped on
On quartz boat, slowly it is pushed into the middle part of chemical vapor deposition unit reative cell, with the both ends of fluid sealant closed quartz tube.It is passed through argon
Gas, flow 100mL/min, heating reative cell is to 900 DEG C.Adjustment argon flow amount is 2000mL/min, and is passed through 400mL/min
Hydrogen.Mobile quartz ampoule, position of the adjustment capillary apertures relative to burner hearth, makes the registration of thermocouple be maintained at 250~300
DEG C, ensure that reaction solution can be in misty sprays into.Delicate flow pump is opened, ferrocene/toluene reactant solution is made to pass through capillary
Pipe is sprayed into misty in reative cell, and solution feed speed is 0.4mL/min.Reaction finishes, and stopping is passed through hydrogen, turns argon gas down
Flow makes reative cell be cooled to room temperature in argon gas atmosphere to 100mL/min, takes out sample, obtains orientation multi-walled carbon nanotube
Array.
S2, gelatin solid particle, nano cellulose crystal are mixed with deionized water, be made mass fraction be 20% it is bright
Glue solution, the wherein quality of nano cellulose crystal are the 5% of gelatin solid particle, and stirring is to admittedly in 95 DEG C of waters bath with thermostatic control
Body polymer uniform dissolves；Finally, the gelatin colloidal sol being uniformly dissolved is stood into cooling at room temperature, until bubble drains.
S3, weigh a certain amount of orientation array of multi-walled carbon nanotubes and be dispersed in plane mould, by gelatin colloidal sol by
Mold side is allowed to uniformly coat directional carbon nanotube array, the matter of carbon nanotube and polymeric sol along being slowly injected into mold
It is 1/99 to measure percentage.
S4, mold is put into -25 DEG C of environment and freezes 10 hours, then thawed 4 hours, so recycle cold at room temperature
Freeze and thaw 5 times, obtains the bioabsorbable polymer material of carbon nanotube enhancing.
Embodiment 2
S1, by 5g ferrocene powder, be dissolved in 50mL toluene.Stand 24 hours after mixing.Quartz glass plate is equipped on
On quartz boat, slowly it is pushed into the middle part of chemical vapor deposition unit reative cell, with the both ends of fluid sealant closed quartz tube.It is passed through argon
Gas, flow 100mL/min, heating reative cell is to 900 DEG C.Adjustment argon flow amount is 2000mL/min, and is passed through 400mL/min
Hydrogen.Mobile quartz ampoule, position of the adjustment capillary apertures relative to burner hearth, makes the registration of thermocouple be maintained at 250~300
DEG C, ensure that reaction solution can be in misty sprays into.Delicate flow pump is opened, ferrocene/toluene reactant solution is made to pass through capillary
Pipe is sprayed into misty in reative cell, and solution feed speed is 0.4mL/min.Reaction finishes, and stopping is passed through hydrogen, turns argon gas down
Flow makes reative cell be cooled to room temperature in argon gas atmosphere to 100mL/min, takes out sample, obtains orientation multi-walled carbon nanotube
Array.
S2, gelatin solid particle, nano cellulose crystal are mixed with deionized water, be made mass fraction be 30% it is bright
Glue solution, the wherein quality of nano cellulose crystal are the 33% of gelatin solid particle, and stirring is to admittedly in 60 DEG C of waters bath with thermostatic control
Body polymer uniform dissolves；Finally, the gelatin colloidal sol being uniformly dissolved is stood into cooling at room temperature, until bubble drains.
S3, weigh a certain amount of orientation array of multi-walled carbon nanotubes and be dispersed in plane mould, by gelatin colloidal sol by
Mold side is allowed to uniformly coat directional carbon nanotube array, the matter of carbon nanotube and polymeric sol along being slowly injected into mold
It is 5/95 to measure percentage.
S4, mold is put into -15 DEG C of environment and freezes 12 hours, then thawed 4 hours, so recycle cold at room temperature
Freeze and thaw 8 times, obtains the bioabsorbable polymer material of carbon nanotube enhancing.
Embodiment 3
S1, by 5g ferrocene powder, be dissolved in 50mL toluene.Stand 24 hours after mixing.Quartz glass plate is equipped on
On quartz boat, slowly it is pushed into the middle part of chemical vapor deposition unit reative cell, with the both ends of fluid sealant closed quartz tube.It is passed through argon
Gas, flow 100mL/min, heating reative cell is to 900 DEG C.Adjustment argon flow amount is 2000mL/min, and is passed through 400mL/min
Hydrogen.Mobile quartz ampoule, position of the adjustment capillary apertures relative to burner hearth, makes the registration of thermocouple be maintained at 250~300
DEG C, ensure that reaction solution can be in misty sprays into.Delicate flow pump is opened, ferrocene/toluene reactant solution is made to pass through capillary
Pipe is sprayed into misty in reative cell, and solution feed speed is 0.4mL/min.Reaction finishes, and stopping is passed through hydrogen, turns argon gas down
Flow makes reative cell be cooled to room temperature in argon gas atmosphere to 100mL/min, takes out sample, obtains orientation multi-walled carbon nanotube
Array.
S2, gelatin solid particle, nano cellulose crystal are mixed with deionized water, be made mass fraction be 40% it is bright
Glue solution, the wherein quality of nano cellulose crystal be gelatin solid particle 12.5%, stirred in 50 DEG C of waters bath with thermostatic control to
Solid polymer uniform dissolution；Finally, the gelatin colloidal sol being uniformly dissolved is stood into cooling at room temperature, until bubble drains.
S3, weigh a certain amount of orientation array of multi-walled carbon nanotubes and be dispersed in plane mould, by gelatin colloidal sol by
Mold side is allowed to uniformly coat directional carbon nanotube array, the matter of carbon nanotube and polymeric sol along being slowly injected into mold
It is 10/90 to measure percentage.
S4, mold is put into -20 DEG C of environment and freezes 8 hours, then thawed 8 hours, so recycle cold at room temperature
Freeze and thaw 3 times, obtains the bioabsorbable polymer material of carbon nanotube enhancing.
Embodiment 4
S1, by 5g ferrocene powder, be dissolved in 50mL toluene.Stand 24 hours after mixing.Quartz glass plate is equipped on
On quartz boat, slowly it is pushed into the middle part of chemical vapor deposition unit reative cell, with the both ends of fluid sealant closed quartz tube.It is passed through argon
Gas, flow 100mL/min, heating reative cell is to 900 DEG C.Adjustment argon flow amount is 2000mL/min, and is passed through 400mL/min
Hydrogen.Mobile quartz ampoule, position of the adjustment capillary apertures relative to burner hearth, makes the registration of thermocouple be maintained at 250~300
DEG C, ensure that reaction solution can be in misty sprays into.Delicate flow pump is opened, ferrocene/toluene reactant solution is made to pass through capillary
Pipe is sprayed into misty in reative cell, and solution feed speed is 0.4mL/min.Reaction finishes, and stopping is passed through hydrogen, turns argon gas down
Flow makes reative cell be cooled to room temperature in argon gas atmosphere to 100mL/min, takes out sample, obtains orientation multi-walled carbon nanotube
Array.
S2, gelatin solid particle, nano cellulose crystal are mixed with deionized water, be made mass fraction be 20% it is bright
Glue solution, the wherein quality of nano cellulose crystal are the 15% of gelatin solid particle, and stirring is to admittedly in 50 DEG C of waters bath with thermostatic control
Body polymer uniform dissolves；Finally, the gelatin colloidal sol being uniformly dissolved is stood into cooling at room temperature, until bubble drains.
S3, weigh a certain amount of orientation array of multi-walled carbon nanotubes and be dispersed in plane mould, by gelatin colloidal sol by
Mold side is allowed to uniformly coat directional carbon nanotube array, the matter of carbon nanotube and polymeric sol along being slowly injected into mold
It is 5/95 to measure percentage.
S4, mold is put into -22 DEG C of environment and freezes 5 hours, then thawed 5 hours, so recycle cold at room temperature
Freeze and thaw 5 times, obtains the bioabsorbable polymer material of carbon nanotube enhancing.
Obviously, described embodiments are only a part of the embodiments of the present invention, instead of all the embodiments.Based on this
Embodiment in invention, every other reality obtained by those of ordinary skill in the art without making creative efforts
Example is applied, the scope of the present invention is belonged to.
Claims (5)
1. a kind of bioabsorbable polymer material of carbon nanotube enhancing, which is characterized in that uniformly divide in the bioabsorbable polymer material
Dissipating has directional carbon nanotube array and nano cellulose crystal.
2. the bioabsorbable polymer material of carbon nanotube enhancing according to claim 1, which is characterized in that the carbon nanotube
Mass content be 1%-10%；The mass content of the nano cellulose crystal is 1%-10%.
3. a kind of preparation method of the bioabsorbable polymer material of carbon nanotube enhancing as claimed in claim 1 or 2, feature exist
In including the following steps：
S1, directional carbon nanotube array is prepared
Directional carbon nanotube array is prepared using chemical vapor deposition (CVD) technology；
S2, preparation are dispersed with the polymeric sol of nano cellulose crystal
High molecular polymer and nano cellulose crystal are added in deionized water, being configured to high molecular polymer mass fraction is
20~40% aqueous solution stirs in 50~95 DEG C of waters bath with thermostatic control to solid polymer uniform dissolution；Finally, it will be uniformly dissolved
Polymeric sol stand cooling at room temperature, until bubble drains；
S3, polymeric sol is penetrated into carbon nanotube precast body
Directional carbon nanotube array made from S1 is dispersed in plane mould, then to slowly penetrate into mold macromolecule molten
Glue makes polymeric sol enveloped carbon nanometer tube precast body, obtains mixture；
S4, freeze-thaw method prepare the bioabsorbable polymer material of carbon nanotube enhancing
Freeze-thaw circulation processing is carried out to the mixture that S3 is obtained, obtains the bioabsorbable polymer material of carbon nanotube enhancing.
4. preparation method according to claim 1, which is characterized in that the high molecular polymer is selected from chitosan, bright
One or more mixtures in glue, hyaluronic acid, sodium alginate.
5. preparation method according to claim 1, which is characterized in that S4 is specially：Cryogenic temperature -25~-15 DEG C, freezing
Then 5~12 hours time thawed 5~12 hours at room temperature, such freeze-thaw circulation 3~8 times, obtained carbon nanotube increasing
Strong bioabsorbable polymer material.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN111607848A (en) * | 2020-05-29 | 2020-09-01 | 哈尔滨工程大学 | Method for chemically crosslinking and modifying carbon nanotube fibers |
| CN112603593A (en) * | 2020-12-14 | 2021-04-06 | 上海大学 | Self-anastomotic artificial blood vessel stent and preparation method thereof |
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