CN107313176A - A kind of preparation method of hollow iron oxide Vingon electrostatic spinning hydrophobic fiber film - Google Patents
A kind of preparation method of hollow iron oxide Vingon electrostatic spinning hydrophobic fiber film Download PDFInfo
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- CN107313176A CN107313176A CN201710454788.7A CN201710454788A CN107313176A CN 107313176 A CN107313176 A CN 107313176A CN 201710454788 A CN201710454788 A CN 201710454788A CN 107313176 A CN107313176 A CN 107313176A
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- vingon
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- electrostatic spinning
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Classifications
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- D—TEXTILES; PAPER
- D04—BRAIDING; LACE-MAKING; KNITTING; TRIMMINGS; NON-WOVEN FABRICS
- D04H—MAKING TEXTILE FABRICS, e.g. FROM FIBRES OR FILAMENTARY MATERIAL; FABRICS MADE BY SUCH PROCESSES OR APPARATUS, e.g. FELTS, NON-WOVEN FABRICS; COTTON-WOOL; WADDING ; NON-WOVEN FABRICS FROM STAPLE FIBRES, FILAMENTS OR YARNS, BONDED WITH AT LEAST ONE WEB-LIKE MATERIAL DURING THEIR CONSOLIDATION
- D04H1/00—Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres
- D04H1/70—Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres characterised by the method of forming fleeces or layers, e.g. reorientation of fibres
- D04H1/72—Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres characterised by the method of forming fleeces or layers, e.g. reorientation of fibres the fibres being randomly arranged
- D04H1/728—Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres characterised by the method of forming fleeces or layers, e.g. reorientation of fibres the fibres being randomly arranged by electro-spinning
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G49/00—Compounds of iron
- C01G49/02—Oxides; Hydroxides
- C01G49/06—Ferric oxide (Fe2O3)
-
- 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
- D01D1/06—Feeding liquid to the spinning head
- D01D1/09—Control of pressure, temperature or feeding rate
-
- 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
- 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
- D01D5/0092—Electro-spinning characterised by the electro-spinning apparatus characterised by the electrical field, e.g. combined with a magnetic fields, using biased or alternating fields
-
- 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
- D04—BRAIDING; LACE-MAKING; KNITTING; TRIMMINGS; NON-WOVEN FABRICS
- D04H—MAKING TEXTILE FABRICS, e.g. FROM FIBRES OR FILAMENTARY MATERIAL; FABRICS MADE BY SUCH PROCESSES OR APPARATUS, e.g. FELTS, NON-WOVEN FABRICS; COTTON-WOOL; WADDING ; NON-WOVEN FABRICS FROM STAPLE FIBRES, FILAMENTS OR YARNS, BONDED WITH AT LEAST ONE WEB-LIKE MATERIAL DURING THEIR CONSOLIDATION
- D04H1/00—Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres
- D04H1/40—Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres from fleeces or layers composed of fibres without existing or potential cohesive properties
- D04H1/42—Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres from fleeces or layers composed of fibres without existing or potential cohesive properties characterised by the use of certain kinds of fibres insofar as this use has no preponderant influence on the consolidation of the fleece
- D04H1/4282—Addition polymers
Abstract
The invention discloses a kind of preparation method of hollow iron oxide Vingon electrostatic spinning hydrophobic fiber film, first iron chloride is acidified with hydrochloric acid, then water is added to carry out after disperseing with alcohol mixeding liquid, add nano bamboo fiber, in the effect of ammoniacal liquor, form the nano bamboo fiber of surface enwrapping ferric oxide, added after being sintered in nano silicon and tetraethyl orthosilicate dispersion liquid, add after ammoniacal liquor reacted, Hybrid Heating reaction is carried out with Vingon lysate, carry out obtaining electrostatic spinning after spinning solution after copolyreaction, both obtain after treatment, present invention reduces the adhesion between ferric oxide particles, lift the dispersiveness between ferric oxide particles, the material of preparation has excellent hydrophobicity, the performances such as self-cleaning property, method is simple, it is easy to operate, and raw material is cheap and easy to get.
Description
Technical field
The invention belongs to tunica fibrosa processing technology field, and in particular to a kind of hollow iron oxide-Vingon Static Spinning
The preparation method of silk hydrophobic fiber film.
Background technology
Polyvinylidene chloride resin is the high polymer material with high obstructing performance, and its barrier property is common packaging materials
Tens times even hundred times.It also has self-extinguishment, oil resistivity and protects taste, and moistureproof, fungicidal properties is also very excellent, especially
It is that it has low-temperature heat-sealing and heat-shrinkable, and is easy to printing, therefore be one of plastics that modern packaging industry is favored, extensively
For the packaging of food, medicine, precision instrument and various military articles for use, " green " packaging material is described as.In addition, using the resin
The latex being made has preferable anti-flammability and cohesiveness, thus is also widely used on building materials and fireproof coating.
Iron oxide tool chemical stability is good, hardness is high, good weatherability, aboundresources, cheap, nonhazardous the features such as,
Nano-sized iron oxide specific surface area is big, surface charge is high, has stronger adsorption capacity to pollutant, in catalyst, coating, magnetic note
Have a wide range of applications and DEVELOPMENT PROSPECT in terms of record material, fine ceramics and biomedical engineering, but just because of oxidation
Iron particle has high surface charge, therefore easily causes agglomeration.
In the last few years, super hydrophobic surface enjoyed the concern of scientists with its automatically cleaning and resistant to pollution characteristic.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
It is determined that after, roughness is the key factor for determining whether surface is super-hydrophobic.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 that 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 effective technology for 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 nano fibrous membrane that this method is obtained has open-celled structure good, high porosity, the advantages of specific surface area is big, and 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 is in feed separation, and the field such as sewage disposal provides efficient filter medium.
The content of the invention
The object of the invention is exactly that there is provided a kind of hollow iron oxide-Vingon is quiet in order to make up the defect of prior art
The preparation method of Electrospun hydrophobic fiber film, reduces the dispersiveness between the adhesion between ferric oxide particles, lifting ferric oxide particles,
The material of preparation has the performances such as excellent hydrophobicity, self-cleaning property, and method is simple, easy to operate, and raw material is cheap and easy to get.
The present invention is achieved by the following technical solutions：
The preparation method of a kind of hollow iron oxide-Vingon electrostatic spinning hydrophobic fiber film, it is characterised in that including following
Step：
（1）5-10 parts by weight iron chloride is added in appropriate hydrochloric acid solution and soaked 20-50 minutes, added appropriate parts by weight water and adjust
Save after pH5-7, add the nano bamboo fiber of 50-60 parts by weight of ethanol and 1-5 parts by weight, the lower heating water bath 50-90 of nitrogen protection
DEG C, after the ammoniacal liquor that 5-8 parts by weight are added dropwise, react 3-5 hours, be sintered in tube furnace, obtain hollow iron oxide, it is stand-by；
（2）By 1-2 parts by weight nano silica powder and 0.1-0.3 parts by weight tetraethyl orthosilicate ultrasonic disperses in 50-80
In weight dimethyl acetamide, step is added（1）Gains, after then addition 1-5 parts by weight ammoniacal liquor is uniformly dispersed, are stirred at room temperature
Reaction 4-8 hours is mixed, it is stand-by；
（3）The Vingon of 10-20 parts by weight is dissolved in appropriate dimethyl acetamide, the poly- second of 0.5-0.8 parts by weight is added
Glycol, after being uniformly dispersed, with step（2）Gains are mixed, and then heat to 75-85 DEG C of stirring reaction 12-16 hours, are obtained
Spinning solution, it is stand-by；
（4）By step（3）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 constitutes electrostatic spinning apparatus, distance is then adjusted, electrostatic is opened
The switch of device for spinning, is set after spinning parameter, carries out electrostatic spinning, after spinning terminates, gains is placed in into 80-150 DEG C and entered
Row heat treatment 1-3 hours after cooled down at room temperature, both the hollow iron oxide-Vingon electrostatic spinning hydrophobic fiber
Film.
Described step（1）In be sintered to and be warming up to 800 DEG C from 25 DEG C, heating rate is 1-2.5 DEG C/min, is incubated 2-
4 hours, sintered in air, then cool to normal temperature with the furnace.
Described step（4）Distance in middle adjustment distance between electrostatic spinning apparatus and receiver is 7-10 centimetres.
Described step（3）Middle to set spinning parameter to push away post speed 0.01-0.5ml/min for spinning solution, environment temperature is
25-45 DEG C, voltage is 15-20kv, and syringe needle internal diameter is 0.6-0.9mm, syringe volume is 2-4ml, and spinneret is pivoted
Rotating speed be 0.001-100rpm, 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 chloride is first acidified by the present invention with hydrochloric acid, is then added water and is carried out with alcohol mixeding liquid after disperseing, adds nanometer
Bamboo fibre, in the effect of ammoniacal liquor, forms the nano bamboo fiber of surface enwrapping ferric oxide, nano silicon is added after being sintered
With in tetraethyl orthosilicate dispersion liquid, adding after ammoniacal liquor reacted, Hybrid Heating is carried out with Vingon lysate anti-
Should, carry out carrying out electrostatic spinning after obtaining spinning solution after copolyreaction, to both having obtained after product processing, the iron chloride after acidifying adds ammonia
After water, using electrostatic adsorption, it is enclosed in around nano bamboo fiber, hollow iron oxide is formed after oversintering so that oxygen
The Space adjustment changed in iron obtains bigger, is conducive to tetraethyl orthosilicate to be coated with nano silicon by sol-gel
Silicon dioxide layer is formed, hydrophobic effect and adsorptivity is greatly improved, the adhesion between ferric oxide particles can be reduced, added
Vingon is carried out after copolymerized grafting, and iron oxide particles form good scattered, stable metal ion in Vingon
With improving adsorptivity, present invention reduces the adhesion between ferric oxide particles, the dispersiveness between ferric oxide particles, the material of preparation are lifted
Material has the performances such as excellent hydrophobicity, self-cleaning property, and method is simple, easy to operate, and raw material is cheap and easy to get.
Embodiment
A kind of preparation method of hollow iron oxide-Vingon electrostatic spinning hydrophobic fiber film, it is characterised in that including
Following steps：
（1）8 parts by weight iron chloride are added in appropriate hydrochloric acid solution and soaked 35 minutes, add appropriate parts by weight water regulation pH5-
After 7, the nano bamboo fiber of 55 parts by weight of ethanol and 3 parts by weight is added, 6 parts by weight are added dropwise in lower 65 DEG C of the heating water bath of nitrogen protection
Ammoniacal liquor after, react 4 hours, be sintered in tube furnace, obtain hollow iron oxide, it is stand-by；
（2）By 1.5 parts by weight nano silica powders and 0.2 parts by weight tetraethyl orthosilicate ultrasonic disperse in 55 weight diformazans
In yl acetamide, step is added（1）Gains, are then added after 3 parts by weight ammoniacal liquor are uniformly dispersed, stirring reaction 6 is small at room temperature
When, it is stand-by；
（3）The Vingon of 15 parts by weight is dissolved in appropriate dimethyl acetamide, 0.7 parts by weight polyethylene glycol is added, point
After dissipating uniformly, with step（2）Gains are mixed, and then heat to 80 DEG C of stirring reactions 14 hours, are obtained spinning solution, are treated
With；
（4）By step（3）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 constitutes electrostatic spinning apparatus, distance is then adjusted, electrostatic is opened
The switch of device for spinning, is set after spinning parameter, carries out electrostatic spinning, after spinning terminates, and gains are placed in into 100 DEG C carries out heat
Processing 2 hours after cooled down at room temperature, both the hollow iron oxide-Vingon electrostatic spinning hydrophobic fiber film.
Described step（1）In be sintered to and be warming up to 800 DEG C from 25 DEG C, heating rate is 1.5 DEG C/min, and insulation 3 is small
When, sinter in air, then cool to normal temperature with the furnace.
Described step（4）Distance in middle adjustment distance between electrostatic spinning apparatus and receiver is 9 centimetres.
Described step（3）Middle to set spinning parameter to push away post speed 0.01-0.5ml/min for spinning solution, environment temperature is
25-45 DEG C, voltage is 15-20kv, and syringe needle internal diameter is 0.6-0.9mm, syringe volume is 2-4ml, and spinneret is pivoted
Rotating speed be 0.001-100rpm, the rotary rpm of roller receiver is 10-5000rpm, and the temperature of liquid bath is 30-90 DEG C.
Claims (4)
1. a kind of preparation method of hollow iron oxide-Vingon electrostatic spinning hydrophobic fiber film, it is characterised in that including with
Lower step：
（1）5-10 parts by weight iron chloride is added in appropriate hydrochloric acid solution and soaked 20-50 minutes, added appropriate parts by weight water and adjust
Save after pH5-7, add the nano bamboo fiber of 50-60 parts by weight of ethanol and 1-5 parts by weight, the lower heating water bath 50-90 of nitrogen protection
DEG C, after the ammoniacal liquor that 5-8 parts by weight are added dropwise, react 3-5 hours, be sintered in tube furnace, obtain hollow iron oxide, it is stand-by；
（2）By 1-2 parts by weight nano silica powder and 0.1-0.3 parts by weight tetraethyl orthosilicate ultrasonic disperses in 50-80
In weight dimethyl acetamide, step is added（1）Gains, after then addition 1-5 parts by weight ammoniacal liquor is uniformly dispersed, are stirred at room temperature
Reaction 4-8 hours is mixed, it is stand-by；
（3）The Vingon of 10-20 parts by weight is dissolved in appropriate dimethyl acetamide, the poly- second of 0.5-0.8 parts by weight is added
Glycol, after being uniformly dispersed, with step（2）Gains are mixed, and then heat to 75-85 DEG C of stirring reaction 12-16 hours, are obtained
Spinning solution, it is stand-by；
（4）By step（3）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 constitutes electrostatic spinning apparatus, distance is then adjusted, electrostatic is opened
The switch of device for spinning, is set after spinning parameter, carries out electrostatic spinning, after spinning terminates, gains is placed in into 80-150 DEG C and entered
Row heat treatment 1-3 hours after cooled down at room temperature, both the hollow iron oxide-Vingon electrostatic spinning hydrophobic fiber
Film.
2. according to a kind of preparation method of hollow iron oxide of claim 1-Vingon electrostatic spinning hydrophobic fiber film, it is special
Levy and be, described step（1）In be sintered to and be warming up to 800 DEG C from 25 DEG C, heating rate is 1-2.5 DEG C/min, is incubated 2-4
Hour, sintered in air, then cool to normal temperature with the furnace.
3. according to a kind of preparation method of hollow iron oxide of claim 1-Vingon electrostatic spinning hydrophobic fiber film, it is special
Levy and be, described step（4）Distance in middle adjustment distance between electrostatic spinning apparatus and receiver is 7-10 centimetres.
4. according to a kind of preparation method of hollow iron oxide of claim 1-Vingon electrostatic spinning hydrophobic fiber film, it is special
Levy and be, described step（3）Middle to set spinning parameter to push away post speed 0.01-0.5ml/min for spinning solution, environment temperature is
25-45 DEG C, voltage is 15-20kv, and syringe needle internal diameter is 0.6-0.9mm, syringe volume is 2-4ml, and spinneret is pivoted
Rotating speed be 0.001-100rpm, the rotary rpm of roller receiver is 10-5000rpm, and the temperature of liquid bath is 30-90 DEG C.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201710454788.7A CN107313176B (en) | 2017-06-16 | 2017-06-16 | A kind of preparation method of hollow iron oxide-Vingon electrostatic spinning hydrophobic fiber film |
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| CN201710454788.7A CN107313176B (en) | 2017-06-16 | 2017-06-16 | A kind of preparation method of hollow iron oxide-Vingon electrostatic spinning hydrophobic fiber film |
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| CN107313176A true CN107313176A (en) | 2017-11-03 |
| CN107313176B CN107313176B (en) | 2019-03-26 |
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Citations (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2002020132A2 (en) * | 2000-09-05 | 2002-03-14 | Donaldson Company, Inc. | Filtration arrangement utilizing pleated construction and method |
| CN1475339A (en) * | 2002-08-15 | 2004-02-18 | 孙建宁 | Fire retarding antistatic polyvinyl chloride composite pipe material and its preparation method |
| CN102218871A (en) * | 2011-04-14 | 2011-10-19 | 万向电动汽车有限公司 | Preparation method of modified diaphragm for lithium-ion secondary battery as well as product and preparation device thereof |
| US20130017748A1 (en) * | 2011-07-15 | 2013-01-17 | Samsung Electro-Mechanics Co., Ltd. | Porous sheet and method for manufacturing the same |
| CN103924384A (en) * | 2014-03-21 | 2014-07-16 | 石河子大学 | Preparation method of constant-hydrophilic graft-modified chlorinated polymer micro/nano fiber film |
| CN104313796A (en) * | 2014-09-09 | 2015-01-28 | 天津工业大学 | Manufacturing method for fibrous membrane for oil-water separation |
| CN106192081A (en) * | 2016-06-30 | 2016-12-07 | 天津工业大学 | A kind of preparation method of Graphene skeletal porous nanofiber |
| CN106345314A (en) * | 2016-09-23 | 2017-01-25 | 江苏大学 | Porous ferric oxide-titanium oxide-activated carbon complex fiber membrane and preparation method |
-
2017
- 2017-06-16 CN CN201710454788.7A patent/CN107313176B/en active Active
Patent Citations (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2002020132A2 (en) * | 2000-09-05 | 2002-03-14 | Donaldson Company, Inc. | Filtration arrangement utilizing pleated construction and method |
| CN1475339A (en) * | 2002-08-15 | 2004-02-18 | 孙建宁 | Fire retarding antistatic polyvinyl chloride composite pipe material and its preparation method |
| CN102218871A (en) * | 2011-04-14 | 2011-10-19 | 万向电动汽车有限公司 | Preparation method of modified diaphragm for lithium-ion secondary battery as well as product and preparation device thereof |
| US20130017748A1 (en) * | 2011-07-15 | 2013-01-17 | Samsung Electro-Mechanics Co., Ltd. | Porous sheet and method for manufacturing the same |
| CN103924384A (en) * | 2014-03-21 | 2014-07-16 | 石河子大学 | Preparation method of constant-hydrophilic graft-modified chlorinated polymer micro/nano fiber film |
| CN104313796A (en) * | 2014-09-09 | 2015-01-28 | 天津工业大学 | Manufacturing method for fibrous membrane for oil-water separation |
| CN106192081A (en) * | 2016-06-30 | 2016-12-07 | 天津工业大学 | A kind of preparation method of Graphene skeletal porous nanofiber |
| CN106345314A (en) * | 2016-09-23 | 2017-01-25 | 江苏大学 | Porous ferric oxide-titanium oxide-activated carbon complex fiber membrane and preparation method |
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|---|---|
| CN107313176B (en) | 2019-03-26 |
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Effective date of registration: 20200601 Address after: 300202 room 329, no.423, South Jiefang Road, Hexi District, Tianjin Patentee after: TIANJIN FENGSHUO SHENGMAO TECHNOLOGY Co.,Ltd. Address before: Gu Qiao Zhen Tong Ying community natural village of Fengtai County in Anhui province Huainan city 232100 Patentee before: FENGTAI JINGXING BIOLOGICAL TECHNOLOGY Co.,Ltd. |
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