CN107699974A - A kind of preparation method of modified oxidized iron Vingon electrospun material - Google Patents
A kind of preparation method of modified oxidized iron Vingon electrospun material Download PDFInfo
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- CN107699974A CN107699974A CN201710820493.7A CN201710820493A CN107699974A CN 107699974 A CN107699974 A CN 107699974A CN 201710820493 A CN201710820493 A CN 201710820493A CN 107699974 A CN107699974 A CN 107699974A
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- Prior art keywords
- vingon
- weight
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- parts
- modified oxidized
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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
- D01F6/48—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 polymers of halogenated hydrocarbons
-
- 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
- D01D5/0007—Electro-spinning
- D01D5/0015—Electro-spinning characterised by the initial state of the material
- D01D5/003—Electro-spinning characterised by the initial state of the material the material being a polymer solution or dispersion
-
- 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
- D01D5/0007—Electro-spinning
- D01D5/0061—Electro-spinning characterised by the electro-spinning apparatus
- D01D5/0069—Electro-spinning characterised by the electro-spinning apparatus characterised by the spinning section, e.g. capillary tube, protrusion or pin
-
- 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
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- Engineering & Computer Science (AREA)
- Textile Engineering (AREA)
- Chemical & Material Sciences (AREA)
- Mechanical Engineering (AREA)
- Chemical Kinetics & Catalysis (AREA)
- General Chemical & Material Sciences (AREA)
- Dispersion Chemistry (AREA)
- Manufacturing & Machinery (AREA)
- Artificial Filaments (AREA)
- Spinning Methods And Devices For Manufacturing Artificial Fibers (AREA)
Abstract
The invention discloses a kind of preparation method of modified oxidized iron Vingon electrospun material, first iron oxide particles are acidified with hydrochloric acid, water is then dispersed in be reacted with tetraethyl orthosilicate is added dropwise in the mixed liquor of ethanol and ammoniacal liquor, then keep reaction condition to add PEI to continue to react with 18 carbon fatty acids, added after treatment after end in Vingon lysate after obtaining spinning solution after progress copolyreaction and carry out electrostatic spinning, to both having been obtained after product processing, material prepared by the present invention has excellent hydrophobicity, the performances such as self-cleaning property, magnetic particle is uniformly dispersed, resulting materials stable performance, high mechanical strength.
Description
Technical field
The invention belongs to electrostatic spinning technique field, and in particular to a kind of modified oxidized iron-Vingon electrostatic spinning
The preparation method of material.
Background technology
In the last few years, super hydrophobic surface enjoyed the concern of scientists with its automatically cleaning and resistant to pollution characteristic.Typically handle
Contact angle is more than 150 ° and the surface of solids of the roll angle less than 10 ° regards super hydrophobic surface as.Super-hydrophobic phenomenon is in nature
Ubiquitous in boundary, Sometimes When It Rains, raindrop can arbitrarily roll in lotus leaf surface and take away the pollutant on its surface, this spy
Property causes the very big interest of researcher, because it can save the cost of substantial amounts of labour and cleaning service.Pass through section
The research of scholars finds that super-hydrophobic phenomenon is relevant with the micro-nano dual structure and low surface energy coat on surface.Work as surface composition
After it is determined that, roughness is that an important factor for whether surface is super-hydrophobic determined.Up to the present, many methods manufacture coarse
Surface, such as template-based extrusion method, etching method, electrochemical deposition method, electrical spinning method and chemical vapour deposition technique.In these methods
In, electrical spinning method has the advantages of easy to operate, cost is low and is good at preparing large area super hydrophobic surface.
Electrostatic spinning has been widely used for the system of nano fibrous membrane as a kind of technology for effectively preparing nano material
It is standby.By changing the concentration, viscosity, flow velocity of spinning solution, institute's making alive can obtain the regulatable nanofiber of diameter.Pass through
The advantages that nano fibrous membrane that this method obtains has good, the high porosity of open-celled structure, and specific surface area is big, these are excellent
Performance has good application prospect in fields such as environmental improvement, chemical petroleum, medicine foods.Electrospun nano-fibers film is outstanding
It provides efficient filter medium in fields such as feed separation, sewage disposals.
Wang Shuai exists《Method of electrostatic spinning prepares feature super hydrophobic material》With tridecafluoro-n-octyltriethoxysilane in one text
(POTS) magnetic Fe of modification3O4@SiO2Nano-particle and Kynoar (PVDF) are raw material, with the method system of electrostatic spinning
For a series of composite film materials, and the relevant natures such as its hydrophobicity and stretch-resistance are investigated, but magnetic particle
Disperse in Kynoar uneven.
The content of the invention
The defects of the object of the invention is exactly to make up prior art, there is provided a kind of modified oxidized iron-Vingon is quiet
The preparation method of electrospinning wire material, by changing reactant feed and preparation method, the material of preparation has excellent this method
The performances such as hydrophobicity, self-cleaning property, magnetic particle are uniformly dispersed.
The present invention is achieved by the following technical solutions：
A kind of preparation method of modified oxidized iron-Vingon electrospun material, comprises the following steps：
（1）5-10 parts by weight iron oxide is added 20-50 minutes are soaked in appropriate hydrochloric acid solution, take out cleaning, add 15-25
Parts by weight water, the ammoniacal liquor of 50-60 parts by weight of ethanol and 1-5 parts by weight, after ultrasonic disperse is uniform, it is former that 0.1-0.3 parts by weight are added dropwise
Tetraethyl orthosilicate, it is stirred at room temperature 4-8 hours under nitrogen protection and adds 15-20 weight account polyethylenes imines and 5-8 parts by weight 18-
Carbon fatty acid, after stirring 5-10 hours, filtered, after clear water washs 2-3 times, electric drying oven with forced convection is dried, and must be changed
Property iron oxide, it is stand-by after grinding；
（2）The Vingon of 10-20 parts by weight is dissolved into 100-200 parts by weight dimethyl acetamides and adds 0.5-0.8
Weight account polyethylene alcohol, add step（1）Gains are stirred, and are then heated to 75-85 DEG C of reaction 12-16 hour, must be spun
Silk solution, it is stand-by；
（3）By step（2）Gained spinning solution is fitted into syringe, then installs syringe needle on syringe as spinning nozzle,
Syringe is arranged on portable hand-held electrostatic spinning machine again and forms electrostatic spinning apparatus, then adjusts distance, opens electrostatic
The switch of device for spinning, after spinning parameter is set, electrostatic spinning is carried out, after spinning terminates, gains is placed in 80-150 DEG C and entered
Row heat treatment 1-3 hours after cooled down at room temperature, both the modified oxidized iron-Vingon electrospun material.
Described step（1）It is middle that to take out cleaning be to be separated from solution product with magnet.
Described step（2）In be stirred as using magnetic agitation progress fast after first slow.
Described step（3）Distance in middle adjustment distance between electrostatic spinning apparatus and receiver is 7-10 centimetres.
Described step（3）It is middle to set spinning parameter to push away post speed 0.01-0.5ml/min, environment temperature for spinning solution
For 25-45 DEG C, voltage 15-20kv, syringe needle internal diameter is 0.6-0.9mm, and syringe volume is 2-4ml, and spinneret revolves around axle
The rotating speed turned is 0.001-100rpm, and the rotary rpm of roller receiver is 10-5000rpm, and the temperature of liquid bath is 30-90 DEG C.
It is an advantage of the invention that：
Iron oxide particles are first acidified by the present invention with hydrochloric acid, are then dispersed in water with being added dropwise in the mixed liquor of ethanol and ammoniacal liquor
Tetraethyl orthosilicate is reacted, and is then kept reaction condition to add PEI and is continued to react with 18- carbon fatty acids,
Added after treatment after end in Vingon lysate after obtaining spinning solution after progress copolyreaction and carry out electrostatic spinning, it is right
After product processing both, for the iron oxide particles after acidifying in the presence of ammoniacal liquor, tetraethyl orthosilicate passes through sol-gel process
Iron oxide particles surface is coated on, the silicon dioxide layer that layer of surface contains hydroxyl is formed, adds PEI and 18- carbon
Aliphatic acid carries out surface modification, PEI and 18- carbon fatty acids, can effectively improve the water-resistance of finished surface, carry
High leakage resistance energy；When being reacted with Vingon, PEI can be copolymerized with it so that modified oxidized abrasive grit
Son is good in Vingon to be disperseed, and modified oxidized iron particle is incorporated into Vingon using the method for electrostatic spinning
In, modified oxidized iron particle mixes with " beading " type Vingon, constructs double scales structure, adds composite wood
Expect the roughness on surface；Material prepared by the present invention has the performances such as excellent hydrophobicity, self-cleaning property, and magnetic particle disperses equal
It is even, resulting materials stable performance, high mechanical strength.
Embodiment
A kind of preparation method of modified oxidized iron-Vingon electrospun material, comprises the following steps：
（1）8 parts by weight iron oxide are added in appropriate hydrochloric acid solution and soaked 30 minutes, take out cleaning, add 20 parts by weight water,
The ammoniacal liquor of 55 parts by weight of ethanol and 3 parts by weight, after ultrasonic disperse is uniform, 0.2 parts by weight tetraethyl orthosilicate, nitrogen protection is added dropwise
Under be stirred at room temperature and add within 6 hours 17 weight account polyethylene imines and 6 parts by weight 18- carbon fatty acids, after stirring 8 hours, carry out
Filter, after clear water washs 3 times, electric drying oven with forced convection is dried, and obtains modified oxidized iron, stand-by after grinding；
（2）The Vingon of 15 parts by weight is dissolved into 150 parts by weight dimethyl acetamides and adds 0.7 weight account polyethylene
Alcohol, add step（1）Gains are stirred, and are then heated to 80 DEG C and are reacted 14 hours, obtain spinning solution, stand-by；
（3）By step（2）Gained spinning solution is fitted into syringe, then installs syringe needle on syringe as spinning nozzle,
Syringe is arranged on portable hand-held electrostatic spinning machine again and forms electrostatic spinning apparatus, then adjusts distance, opens electrostatic
The switch of device for spinning, after spinning parameter is set, electrostatic spinning is carried out, after spinning terminates, gains are placed in 100 DEG C and carry out heat
Processing 2 hours after cooled down at room temperature, both the modified oxidized iron-Vingon electrospun material.
Described step（1）It is middle that to take out cleaning be to be separated from solution product with magnet.
Described step（2）In be stirred as using magnetic agitation progress fast after first slow.
Described step（3）Distance in middle adjustment distance between electrostatic spinning apparatus and receiver is 9 centimetres.
Described step（3）It is middle to set spinning parameter to push away post speed 0.01-0.5ml/min, environment temperature for spinning solution
For 25-45 DEG C, voltage 15-20kv, syringe needle internal diameter is 0.6-0.9mm, and syringe volume is 2-4ml, and spinneret revolves around axle
The rotating speed turned is 0.001-100rpm, and the rotary rpm of roller receiver is 10-5000rpm, and the temperature of liquid bath is 30-90 DEG C.
Claims (5)
1. the preparation method of a kind of modified oxidized iron-Vingon electrospun material, it is characterised in that including following step
Suddenly：
（1）5-10 parts by weight iron oxide is added 20-50 minutes are soaked in appropriate hydrochloric acid solution, take out cleaning, add 15-25
Parts by weight water, the ammoniacal liquor of 50-60 parts by weight of ethanol and 1-5 parts by weight, after ultrasonic disperse is uniform, it is former that 0.1-0.3 parts by weight are added dropwise
Tetraethyl orthosilicate, it is stirred at room temperature 4-8 hours under nitrogen protection and adds 15-20 weight account polyethylenes imines and 5-8 parts by weight 18-
Carbon fatty acid, after stirring 5-10 hours, filtered, after clear water washs 2-3 times, electric drying oven with forced convection is dried, and must be changed
Property iron oxide, it is stand-by after grinding；
（2）The Vingon of 10-20 parts by weight is dissolved into 100-200 parts by weight dimethyl acetamides and adds 0.5-0.8
Weight account polyethylene alcohol, add step（1）Gains are stirred, and are then heated to 75-85 DEG C of reaction 12-16 hour, must be spun
Silk solution, it is stand-by；
（3）By step（2）Gained spinning solution is fitted into syringe, then installs syringe needle on syringe as spinning nozzle,
Syringe is arranged on portable hand-held electrostatic spinning machine again and forms electrostatic spinning apparatus, then adjusts distance, opens electrostatic
The switch of device for spinning, after spinning parameter is set, electrostatic spinning is carried out, after spinning terminates, gains is placed in 80-150 DEG C and entered
Row heat treatment 1-3 hours after cooled down at room temperature, both the modified oxidized iron-Vingon electrospun material.
2. according to a kind of preparation method of modified oxidized iron of claim 1-Vingon electrospun material, its feature exists
In described step（1）It is middle that to take out cleaning be to be separated from solution product with magnet.
3. according to a kind of preparation method of modified oxidized iron of claim 1-Vingon electrospun material, its feature exists
In described step（2）In be stirred as using magnetic agitation progress fast after first slow.
4. according to a kind of preparation method of modified oxidized iron of claim 1-Vingon electrospun material, its feature exists
In described step（3）Distance in middle adjustment distance between electrostatic spinning apparatus and receiver is 7-10 centimetres.
5. according to a kind of preparation method of modified oxidized iron of claim 1-Vingon electrospun material, its feature exists
In described step（3）It is middle to set spinning parameter to push away post speed 0.01-0.5ml/min, environment temperature 25-45 for spinning solution
DEG C, voltage 15-20kv, syringe needle internal diameter is 0.6-0.9mm, and syringe volume is 2-4ml, the rotating speed being pivoted of spinneret
For 0.001-100rpm, the rotary rpm of roller receiver is 10-5000rpm, and the temperature of liquid bath is 30-90 DEG C.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201710820493.7A CN107699974A (en) | 2017-09-13 | 2017-09-13 | A kind of preparation method of modified oxidized iron Vingon electrospun material |
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| Application Number | Priority Date | Filing Date | Title |
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| CN201710820493.7A CN107699974A (en) | 2017-09-13 | 2017-09-13 | A kind of preparation method of modified oxidized iron Vingon electrospun material |
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| CN107699974A true CN107699974A (en) | 2018-02-16 |
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| CN201710820493.7A Pending CN107699974A (en) | 2017-09-13 | 2017-09-13 | A kind of preparation method of modified oxidized iron Vingon electrospun material |
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Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1850356A (en) * | 2005-04-22 | 2006-10-25 | 中国科学院化学研究所 | Super-hydrophotic magnetic carbon film, its preparing method and use |
| CN1880526A (en) * | 2005-06-13 | 2006-12-20 | 中国科学院化学研究所 | Ultra-hydrophobic conductive macromolecular nano fiber and method for preparing same and use thereof |
-
2017
- 2017-09-13 CN CN201710820493.7A patent/CN107699974A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1850356A (en) * | 2005-04-22 | 2006-10-25 | 中国科学院化学研究所 | Super-hydrophotic magnetic carbon film, its preparing method and use |
| CN1880526A (en) * | 2005-06-13 | 2006-12-20 | 中国科学院化学研究所 | Ultra-hydrophobic conductive macromolecular nano fiber and method for preparing same and use thereof |
Non-Patent Citations (1)
| Title |
|---|
| 王帅: "静电纺丝法制备功能性超疏水材料", 《中国博士学位论文全文数据库 工程科技I辑》 * |
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Application publication date: 20180216 |