CN108752813A - A kind of poly-dopamine/ionic liquid/plant fibre blending film and preparation method thereof - Google Patents
A kind of poly-dopamine/ionic liquid/plant fibre blending film and preparation method thereof Download PDFInfo
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Abstract
The invention discloses a kind of poly-dopamine/ionic liquid/plant fibre blending films and preparation method thereof, belong to polymer modification field.It first prepares the plant fiber of poly-dopamine powder and certain mesh number, then by poly-dopamine powder, Kynoar admixture of powder in the ionic liquid dissolved with plant fiber, the poly-dopamine/ionic liquid/plant fibre blending film is obtained using immersion precipitation phase inversion process.Material of the present invention is environmentally protective, simple for process, easily operated, low for equipment requirements, is easy to industrializing implementation, and gained poly-dopamine/ionic liquid/plant fibre blending film has good hydrophilic and mechanical performance, and permeability of the membrane can be greatly improved.
Description
Technical field
The invention belongs to polymer modification fields, and in particular to a kind of poly-dopamine/ionic liquid/plant fibre blending film
And preparation method thereof.
Background technology
Kynoar（PVDF）There are many hydrophilic modification method of film, and physical modification is that one of which is critically important
Method.Physical modification is broadly divided into two classes at present：One kind is that inorganic hydrophilic particle is blended with PVDF, and another kind of is will have
Machine hydrophilic macromers are blended with PVDF.Wherein organic hydrophilicity macromolecular and PVDF blending and modifyings is with obvious effects, and modifying agent is not easy
Effusion, obtains extensive concern.And plant fiber contains abundant hydrophilic hydroxy group group, derives from a wealth of sources, and is easy to get cheap, for
The modification of pvdf membrane holds out broad prospects.But plant fiber is due to itself hydrogen bond action, and solubility property is poor and the compatibility of PVDF
It is weak.Pollution is easily caused with solvent method dissolving cellulose, and ionic liquid can open that plant fiber is intermolecular and intramolecular hydrogen bond, it is right
The solubility property of fiber is good, and ionic liquid is not volatile, and pollution is small, easily repeats to recycle, be taken seriously increasingly.
On the other hand, it is a kind of effective method to increase the compatibility between macromolecular and PVDF using bulking agent.Research
It was found that containing abundant hydroxyl group in poly-dopamine structure, hydrogen bond can occur with plant fiber and react, and poly-dopamine sheet
The macromolecular structure of body and the Adhesion property strong to solid so that it can have strong interaction with Kynoar, utilize
Hydrogen bond reaction between poly-dopamine molecule, can increase the interaction of plant fiber and PVDF macromoleculars, to increase indirectly
Add the compatibility of the two.In addition there are no pollution to the environment for poly-dopamine.
Based on this, the method comprises the steps of firstly, preparing the plant fibers of poly-dopamine and certain mesh number, then by poly-dopamine/poly- inclined
Vinyl fluoride solution blending passes through immersion precipitation inversion of phases in the ionic liquid dissolved with plant fiber, by obtained uniform casting solution
Poly-dopamine/ionic liquid/plant fibre blending film is made.This is a kind of very simple method of modifying, without expensive instrument
Device not only increases the utilization rate to discarding natural resources, and there are no pollution to the environment.
Invention content
The purpose of the present invention is to provide a kind of poly-dopamine/ionic liquid/plant fibre blending film and preparation method thereof,
Its is simple for process, easily operated, low for equipment requirements, is easy to industrializing implementation, and gained poly-dopamine/ionic liquid/plant is fine
Tieing up blend film has good hydrophilic and mechanical performance, and is not injured to human body.
To achieve the above object, the present invention adopts the following technical scheme that：
A kind of poly-dopamine/ionic liquid/plant fibre blending film, is the plant for first preparing poly-dopamine powder and certain mesh number
Then poly-dopamine powder, Kynoar admixture of powder are utilized leaching by fibres in the ionic liquid dissolved with plant fiber
It does not precipitate phase inversion and obtains the poly-dopamine/ionic liquid/plant fibre blending film.
The plant fiber includes monkey grass, bamboo fibre, flaxen fiber, cotton fiber etc..
The ionic liquid includes 1- hexyl -3- methylimidazole villaumites, 1- octyl -3- methylimidazole villaumites, 1- hydroxyl second
Any one in base -3- methyl imidazolium tetrafluoroborates.
The preparation method of the poly-dopamine/ionic liquid/plant fibre blending film includes the following steps：
1）The preparation of poly-dopamine powder
The dopamine hydrochloride solution of 2-10 mg/L is added in the Tris solution of 10mM, Tris solution is used in combination to be settled to
200-400 mL are centrifuged after 24 h are stirred at room temperature, and are filtered, and are washed, and are lyophilized, and vacuum drying obtains poly-dopamine powder；
2）Dissolved with the preparation of the ionic liquid of plant fiber
Pulp plate is cut into 1 × 1 cm2Fritter, be put into secondary water, stirring at normal temperature cleans 0.5h, then filtering and impurity removing exists
Dry 24 h, place into blender and crush in 60 DEG C of thermostatic drying chambers, until crossing 400 mesh sieve, obtain plant fiber；Gained is planted again
Fibres are added in the flask equipped with ionic liquid, and 60-65 DEG C of stirring 4-6 h obtains the ionic liquid dissolved with plant fiber；
3）The preparation of poly-dopamine/ionic liquid/plant fibre blending film
Kynoar powder, pore former polyvinylpyrrolidone and solvent dimethylformamide are mixed, 70-75 DEG C of stirring is equal
After even, 20 DEG C are cooled to hereinafter, a certain amount of poly-dopamine powder and the ionic liquid dissolved with plant fiber, deaeration, room temperature is added
Knifing dries, and obtains poly-dopamine/ionic liquid/plant fibre blending film.
Step 2）In ionic liquid and plant fiber used mass ratio be 60:1-10:1.
Step 3）The mass ratio of middle plant fiber and poly-dopamine powder is 4:1-4:3；Kynoar powder with it is poly- more
The mass ratio of bar amine powder is 20:1-10:1；The mass ratio of Kynoar powder and polyvinylpyrrolidone is 2:1-1.5:
1；Total dosage of Kynoar powder and polyvinylpyrrolidone is the 10%-20% of dimethylformamide quality.
Compared with prior art, the present invention innovatively drops low-fiber size using ionic liquid dissolving plant fiber,
And increases the compatibility of plant fiber and Kynoar with poly-dopamine, ionic liquid/plant fiber modified polyvinilidene is made
Fluoride blending film, which has good hydrophilic, antifouling property and excellent mechanical performance, and its is simple for process,
It is easily operated, it is low for equipment requirements, it is easy to industrializing implementation, ionic liquid is repeatable to be utilized, and can increase the profit of natural resources
With rate.
Description of the drawings
Fig. 1 is the scanning electron microscope (SEM) photograph for the plant fiber film not prepared with poly-dopamine, ionic liquid blending and modifying；
Fig. 2 is the scanning electron microscope (SEM) photograph of poly-dopamine/ionic liquid/plant fibre blending film prepared by embodiment 1；
Fig. 3 is the scanning electron microscope (SEM) photograph of poly-dopamine/ionic liquid/plant fibre blending film prepared by embodiment 2；
Fig. 4 is the scanning electron microscope (SEM) photograph of poly-dopamine/ionic liquid/plant fibre blending film prepared by embodiment 3.
Specific implementation mode
In order to make content of the present invention easily facilitate understanding, With reference to embodiment to of the present invention
Technical solution is described further, but the present invention is not limited only to this.
Embodiment 1
1）The preparation of poly-dopamine powder：The dopamine hydrochloride solution of 2 mg/L is added in the Tris solution of 10mM, and
200 mL are settled to Tris solution, are centrifuged after 24 h are stirred at room temperature, are filtered, are washed, are lyophilized, vacuum drying obtains poly-dopamine
Powder；
2）Dissolved with the preparation of the ionic liquid of plant fiber：Pulp plate is cut into 1 × 1 cm2Fritter, be put into secondary water, often
Warm stirring and washing 0.5h, filtering and impurity removing, then dry 24 h in 60 DEG C of thermostatic drying chambers, place into blender and crush, until
400 mesh sieve is crossed, plant fiber is obtained；Plant fiber obtained by 0.2 g is added to equipped with 4 g ionic liquid 1- hexyl -3- methyl again
In the flask of imidazoles villaumite, 60 DEG C of 4 h of stirring obtain the ionic liquid dissolved with plant fiber；
3）The preparation of poly-dopamine/ionic liquid/plant fibre blending film：By 0.85 g Kynoar powder, 0.5 g pore-formings
Agent polyvinylpyrrolidone and the mixing of 13.5 g dimethylformamides, 70-75 DEG C stirs evenly postcooling to 20 DEG C hereinafter, being added
0.05 g poly-dopamines powder and 3g are dried dissolved with the ionic liquid of plant fiber, deaeration, room temperature knifing, obtain poly-dopamine/from
Sub- liquid/plant fibre blending film, scanning electron microscope (SEM) photograph are shown in Fig. 1.
After testing, the contact angle of PVDF originals film and water without blending and modifying reaches 105 °, and the present embodiment poly-dopamine/from
The contact angle of sub- liquid/plant fibre blending film and water drops to 45 °, and contact angle declines rapidly with time of contact, until 20
There was only 7 ° when the second.With universal testing machine measure not with poly-dopamine, the plant fiber film of ionic liquid blending and modifying and poly-
The mechanical performance of dopamine/ionic liquid/plant fibre blending film, as a result, it has been found that the springform of modified plant fibre blending film
Amount improves 22%, and tensile strength improves 27%（The elasticity modulus of unmodified plant fiber film is 459.85 MPa, and tension is strong
Degree is 23.81 MPa）.
Embodiment 2
1）The preparation of poly-dopamine powder：The dopamine hydrochloride solution of 2 mg/L is added in the Tris solution of 10mM, and
200 mL are settled to Tris solution, are centrifuged after 24 h are stirred at room temperature, are filtered, are washed, are lyophilized, vacuum drying obtains poly-dopamine
Powder；
2）Dissolved with the preparation of the ionic liquid of plant fiber：Pulp plate is cut into 1 × 1 cm2Fritter, be put into secondary water, often
Warm stirring and washing 0.5h, filtering and impurity removing, then dry 24 h in 60 DEG C of thermostatic drying chambers, place into blender and crush, until
400 mesh sieve is crossed, plant fiber is obtained；Plant fiber obtained by 0.4 g is added to equipped with 4 g ionic liquid 1- hexyl -3- methyl again
In the flask of imidazoles villaumite, 60 DEG C of 4 h of stirring obtain the ionic liquid dissolved with plant fiber；
3）The preparation of poly-dopamine/ionic liquid/plant fibre blending film：By 1.7 g Kynoar powder, 1 g pore formers
Polyvinylpyrrolidone and the mixing of 13.5 g dimethylformamides, 70-75 DEG C stirs evenly postcooling to 20 DEG C hereinafter, being added
0.1 g poly-dopamines powder and 3g are dried dissolved with the ionic liquid of plant fiber, deaeration, room temperature knifing, obtain poly-dopamine/from
Sub- liquid/plant fibre blending film, scanning electron microscope (SEM) photograph are shown in Fig. 2.
After testing, the contact angle of PVDF originals film and water without blending and modifying reaches 105 °, and the present embodiment poly-dopamine/from
The contact angle of sub- liquid/plant fibre blending film and water drops to 40 °, and contact angle declines rapidly with time of contact, until 15
There was only 7 ° when the second.With universal testing machine measure not with poly-dopamine, the plant fiber film of ionic liquid blending and modifying and poly-
The mechanical performance of dopamine/ionic liquid/plant fibre blending film, as a result, it has been found that the springform of modified plant fibre blending film
Amount improves 25%, and tensile strength improves 28%（The elasticity modulus of unmodified plant fiber film is 459.85 MPa, and tension is strong
Degree is 23.81 MPa）.
Embodiment 3
1）The preparation of poly-dopamine powder：The dopamine hydrochloride solution of 2 mg/L is added in the Tris solution of 10mM, and
200 mL are settled to Tris solution, are centrifuged after 24 h are stirred at room temperature, are filtered, are washed, are lyophilized, vacuum drying obtains poly-dopamine
Powder；
2）Dissolved with the preparation of the ionic liquid of plant fiber：Pulp plate is cut into 1 × 1 cm2Fritter, be put into secondary water, often
Warm stirring and washing 0.5h, filtering and impurity removing, then dry 24 h in 60 DEG C of thermostatic drying chambers, place into blender and crush, until
400 mesh sieve is crossed, plant fiber is obtained；Plant fiber obtained by 0.2 g is added to equipped with 7 g ionic liquid 1- hexyl -3- methyl again
In the flask of imidazoles villaumite, 60 DEG C of 4 h of stirring obtain the ionic liquid dissolved with plant fiber；
3）The preparation of poly-dopamine/ionic liquid/plant fibre blending film：1.7g Kynoar powder, 1 g pore formers are gathered
Vinylpyrrolidone and the mixing of 14 g dimethylformamides, 70-75 DEG C stirs evenly postcooling to 20 DEG C hereinafter, 0.1 g is added
Poly-dopamine powder and 4g are dried dissolved with the ionic liquid of plant fiber, deaeration, room temperature knifing, obtain poly-dopamine/ionic liquid
Body/plant fibre blending film, scanning electron microscope (SEM) photograph are shown in Fig. 3.
After testing, the contact angle of PVDF originals film and water without blending and modifying reaches 105 °, and the present embodiment poly-dopamine/from
The contact angle of sub- liquid/plant fibre blending film and water drops to 38 °, and contact angle declines rapidly with time of contact, until 10
There was only 5 ° when the second.With universal testing machine measure not with poly-dopamine, the plant fiber film of ionic liquid blending and modifying and poly-
The mechanical performance of dopamine/ionic liquid/plant fibre blending film, as a result, it has been found that the springform of modified plant fibre blending film
Amount improves 27%, and tensile strength improves 29%（The elasticity modulus of unmodified plant fiber film is 459.85 MPa, and tension is strong
Degree is 23.81 MPa）.
Embodiment 4
1）The preparation of poly-dopamine powder：The dopamine hydrochloride solution of 2 mg/L is added in the Tris solution of 10mM, and
200 mL are settled to Tris solution, are centrifuged after 24 h are stirred at room temperature, are filtered, are washed, are lyophilized, vacuum drying obtains poly-dopamine
Powder；
2）Dissolved with the preparation of the ionic liquid of plant fiber：Pulp plate is cut into 1 × 1 cm2Fritter, be put into secondary water, often
Warm stirring and washing 0.5h, filtering and impurity removing, then dry 24 h in 60 DEG C of thermostatic drying chambers, place into blender and crush, until
400 mesh sieve is crossed, plant fiber is obtained；Plant fiber obtained by 0.2 g is added to equipped with 7 g ionic liquid 1- octyl -3- methyl again
In the flask of imidazoles villaumite, 60 DEG C of 4 h of stirring obtain the ionic liquid dissolved with plant fiber；
3）The preparation of poly-dopamine/ionic liquid/plant fibre blending film：By 1.65 g Kynoar powder, 1.0 g pore-formings
Agent polyvinylpyrrolidone and 13.25 g dimethylformamides mixing, 70-75 DEG C stir evenly postcooling to 20 DEG C hereinafter, plus
Enter 0.15 g poly-dopamines powder and 6g dissolved with the ionic liquid of plant fiber, deaeration, room temperature knifing dries, obtain poly-dopamine/
Ionic liquid/plant fibre blending film.
After testing, the contact angle of PVDF originals film and water without blending and modifying reaches 105 °, and the present embodiment poly-dopamine/from
The contact angle of sub- liquid/plant fibre blending film and water drops to 35 °, and contact angle declines rapidly with time of contact, until 8 seconds
When there was only 5 °.With universal testing machine measure not with poly-dopamine, the plant fiber film of ionic liquid blending and modifying and poly- more
The mechanical performance of bar amine/ionic liquid/plant fibre blending film, as a result, it has been found that the elasticity modulus of modified plant fibre blending film
25% is improved, tensile strength improves 27%（The elasticity modulus of unmodified plant fiber film is 459.85 MPa, tensile strength
For 23.81 MPa）.
Embodiment 5
1）The preparation of poly-dopamine powder：The dopamine hydrochloride solution of 2 mg/L is added in the Tris solution of 10mM, and
200 mL are settled to Tris solution, are centrifuged after 24 h are stirred at room temperature, are filtered, are washed, are lyophilized, vacuum drying obtains poly-dopamine
Powder；
2）Dissolved with the preparation of the ionic liquid of plant fiber：Pulp plate is cut into 1 × 1 cm2Fritter, be put into secondary water, often
Warm stirring and washing 0.5h, filtering and impurity removing, then dry 24 h in 60 DEG C of thermostatic drying chambers, place into blender and crush, until
400 mesh sieve is crossed, plant fiber is obtained；Plant fiber obtained by 0.2 g is added to equipped with 8 g ionic liquid 1- octyl -3- methyl again
In the flask of imidazoles villaumite, 60 DEG C of 4 h of stirring obtain the ionic liquid dissolved with plant fiber；
3）The preparation of poly-dopamine/ionic liquid/plant fibre blending film：By 1.65 g Kynoar powder, 1.0 g pore-formings
Agent polyvinylpyrrolidone and the mixing of 15 g dimethylformamides, 70-75 DEG C stirs evenly postcooling to 20 DEG C hereinafter, being added
0.15 g poly-dopamines powder and 7g are dried dissolved with the ionic liquid of plant fiber, deaeration, room temperature knifing, obtain poly-dopamine/from
Sub- liquid/plant fibre blending film.
After testing, the contact angle of PVDF originals film and water without blending and modifying reaches 105 °, and the present embodiment poly-dopamine/from
The contact angle of sub- liquid/plant fibre blending film and water drops to 38 °, and contact angle declines rapidly with time of contact, until 20
There was only 10 ° when the second.With universal testing machine measure not with poly-dopamine, the plant fiber film of ionic liquid blending and modifying and poly-
The mechanical performance of dopamine/ionic liquid/plant fibre blending film, as a result, it has been found that the springform of modified plant fibre blending film
Amount improves 32%, and tensile strength improves 34%（The elasticity modulus of unmodified plant fiber film is 459.85 MPa, and tension is strong
Degree is 23.81 MPa）.
The foregoing is merely presently preferred embodiments of the present invention, all equivalent changes done according to scope of the present invention patent with
Modification should all belong to the covering scope of the present invention.
Claims (6)
1. a kind of poly-dopamine/ionic liquid/plant fibre blending film, it is characterised in that：First prepare poly-dopamine powder and one
The plant fiber of mesh number is determined, then by poly-dopamine powder, Kynoar admixture of powder in the ionic liquid dissolved with plant fiber
In body, the poly-dopamine/ionic liquid/plant fibre blending film is obtained using immersion precipitation phase inversion process.
2. poly-dopamine/ionic liquid/plant fibre blending film according to claim 1, it is characterised in that：The plant
Fiber includes monkey grass, bamboo fibre, flaxen fiber, cotton fiber.
3. poly-dopamine/ionic liquid/plant fibre blending film according to claim 1, it is characterised in that：It is described from
Sub- liquid includes 1- hexyl -3- methylimidazole villaumites, 1- octyl -3- methylimidazole villaumites, 1- ethoxy -3- methylimidazole tetrafluoros
Any one in borate.
4. a kind of preparation method of poly-dopamine/ionic liquid/plant fibre blending film as described in claim 1, feature
It is：Include the following steps：
1）The preparation of poly-dopamine powder
The dopamine hydrochloride solution of 2-10 mg/L is added in the Tris solution of 10mM, Tris solution is used in combination to be settled to
200-400 mL are centrifuged after 24 h are stirred at room temperature, and are filtered, and are washed, and are lyophilized, and vacuum drying obtains poly-dopamine powder；
2）Dissolved with the preparation of the ionic liquid of plant fiber
Pulp plate is cut into 1 × 1 cm2Fritter, be put into secondary water, stirring at normal temperature clean 0.5h, filtering and impurity removing, then 60
Dry 24 h, place into blender and crush in DEG C thermostatic drying chamber, until crossing 400 mesh sieve, obtain plant fiber；Again by gained plant
Fiber is added in ionic liquid, and 60-65 DEG C of stirring 4-6 h obtains the ionic liquid dissolved with plant fiber；
3）The preparation of poly-dopamine/ionic liquid/plant fibre blending film
Kynoar powder, pore former polyvinylpyrrolidone and solvent dimethylformamide are mixed, 70-75 DEG C of stirring is equal
After even, 20 DEG C are cooled to hereinafter, a certain amount of poly-dopamine powder and the ionic liquid dissolved with plant fiber, deaeration, room temperature is added
Knifing dries, and obtains poly-dopamine/ionic liquid/plant fibre blending film.
5. the preparation method of poly-dopamine/ionic liquid/plant fibre blending film according to claim 4, feature exist
In：Step 2）In ionic liquid and plant fiber used mass ratio be 60:1-10:1.
6. the preparation method of poly-dopamine/ionic liquid/plant fibre blending film according to claim 4, feature exist
In：Step 3）The mass ratio of middle plant fiber and poly-dopamine powder is 4:1-4:3；
The mass ratio of Kynoar powder and poly-dopamine powder is 20:1-10:1；
The mass ratio of Kynoar powder and polyvinylpyrrolidone is 2:1-1.5:1；
Total dosage of Kynoar powder and polyvinylpyrrolidone is the 10%-20% of dimethylformamide quality.
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| CN114904495A (en) * | 2022-04-29 | 2022-08-16 | 东南大学 | Adsorption film for adsorbing and removing mycotoxin in liquid, adsorption method and application thereof |
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| 张大钊: "离子液体中改性植物纤维制备功能化复合膜的研究", 《江苏科技大学专业硕士学位论文 中国优秀硕士论文全文数据库工程科技I辑》 * |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114904495A (en) * | 2022-04-29 | 2022-08-16 | 东南大学 | Adsorption film for adsorbing and removing mycotoxin in liquid, adsorption method and application thereof |
| CN114904495B (en) * | 2022-04-29 | 2024-02-20 | 东南大学 | Adsorption film for removing mycotoxin in liquid by adsorption, adsorption method and application thereof |
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