CN107313176B - 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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- CN107313176B CN107313176B CN201710454788.7A CN201710454788A CN107313176B CN 107313176 B CN107313176 B CN 107313176B CN 201710454788 A CN201710454788 A CN 201710454788A CN 107313176 B CN107313176 B CN 107313176B
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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 hollow iron oxide-Vingon electrostatic spinning hydrophobic fiber film preparation methods, first iron chloride is acidified with hydrochloric acid, then after addition water and alcohol mixeding liquid are dispersed, nano bamboo fiber is added, in the effect of ammonium hydroxide, form the nano bamboo fiber of surface enwrapping ferric oxide, it is added in nano silica and tetraethyl orthosilicate dispersion liquid after being sintered, it adds after ammonium hydroxide reacted, Hybrid Heating is carried out with Vingon lysate to react, electrostatic spinning after spinning solution is obtained after carrying out copolyreaction, after treatment both, present invention reduces the adhesions between ferric oxide particles, promote the dispersibility 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 fields, and in particular to a kind of hollow iron oxide-Vingon Static Spinning
The preparation method of silk hydrophobic fiber film.
Background technique
Polyvinylidene chloride resin is the high molecular material with high obstructing performance, its barrier property is common packaging materials
Tens times even hundred times.It also has self-extinguishment, oil resistivity and protects taste, and moisture-proof, fungicidal properties is also very excellent, especially
It is that it has low-temperature heat-sealing and heat-shrinkable, and is convenient for printing, therefore be one of the plastics that modern packaging industry is favored, extensively
For the packaging of food, drug, precision instrument and various military articles, it is known as " green " packaging material.In addition, with the resin
Manufactured latex has preferable anti-flammability and cohesiveness, thus is also widely used on building materials and fireproof coating.
Iron oxide has the features such as chemical stability is good, hardness is high, good weatherability, resourceful, cheap, nonhazardous,
Nano iron oxide large specific surface area, surface charge are high, have stronger adsorption capacity to pollutant, in catalyst, coating, magnetic note
Record material, fine ceramics and biomedical engineering etc. have a wide range of applications and development prospect, but just because of oxidation
Iron particle has high surface charge, therefore easily causes agglomeration.
In recent years, super hydrophobic surface is with its automatically cleaning and resistant to pollution characteristic by the concern of scientists.Pass through section
The research of scholars finds that super-hydrophobic phenomenon is related with the micro-nano dual structure and low surface energy coat on surface.Work as surface composition
After determination, roughness is the key factor for determining whether surface is super-hydrophobic.Up to the present, there are many methods that can 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, at low cost and is good at preparing large area super hydrophobic surface.
A kind of technology of the electrostatic spinning as effectively preparation nano material, has been widely used for the system of nano fibrous membrane
It is standby.By changing concentration, the viscosity, flow velocity of spinning solution, institute's making alive can obtain the regulatable nanofiber of diameter.Pass through
The advantages that porosity that the nano fibrous membrane that this method obtains has open-celled structure good, high, large specific surface area, these are excellent
Performance has a 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 feed separation, the fields such as sewage treatment.
Summary of the invention
The object of the invention is to remedy the disadvantages of known techniques, and it is quiet to provide a kind of hollow iron oxide-Vingon
The preparation method of Electrospun hydrophobic fiber film reduces the adhesion between ferric oxide particles, promotes the dispersibility between 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:
A kind of preparation method of hollow iron oxide-Vingon electrostatic spinning hydrophobic fiber film, which is characterized in that including
Following steps:
(1) 5-10 parts by weight iron chloride is added in suitable hydrochloric acid solution and is impregnated 20-50 minutes, appropriate parts by weight are added
After water adjusts pH5-7, the nano bamboo fiber of 50-60 parts by weight of ethanol and 1-5 parts by weight is added, water-bath is heated under nitrogen protection
It 50-90 DEG C, after the ammonium hydroxide of 5-8 parts by weight is added dropwise, reacts 3-5 hours, is sintered in tube furnace, obtains hollow iron oxide, for use；
(2) by 1-2 parts by weight nano silica powder and 0.1-0.3 parts by weight tetraethyl orthosilicate ultrasonic disperse in
In 50-80 parts by weight dimethyl acetamide, step (1) gains are added, after then addition 1-5 parts by weight ammonium hydroxide is uniformly dispersed,
It is stirred to react 4-8 hours at room temperature, for use；
(3) Vingon of 10-20 parts by weight is dissolved in appropriate dimethyl acetamide, 0.5-0.8 parts by weight is added
Polyethylene glycol after being uniformly dispersed, is mixed with step (2) gains, and then heating to 75-85 DEG C, to be stirred to react 12-16 small
When, spinning solution is obtained, for use；
(4) spinning solution obtained by step (3) is fitted into syringe, then the syringe needle installed on syringe is sprayed as spinning
Head, then syringe is mounted on portable hand-held electrostatic spinning machine and constitutes electrostatic spinning apparatus, distance is then adjusted, is opened quiet
The switch of electric spinning device after spinning parameter is arranged, carries out electrostatic spinning, after spinning, gains is placed in 80-150 DEG C
Carry out heat treatment 1-3 hours after cooled down at room temperature, both the hollow iron oxide-hydrophobic fibre of Vingon electrostatic spinning
Tie up film.
It is sintered in the step (1) and is being warming up to 800 DEG C from 25 DEG C, heating rate is 1-2.5 DEG C/min, keeps the temperature 2-
It 4 hours, is sintered in air, then cools to room temperature with the furnace.
In the step (4) in adjustment distance electrostatic spinning apparatus between receiver at a distance from be 7-10 centimetres.
Setting spinning parameter pushes away column speed 0.01-0.5ml/min for spinning solution in the step (3), and environment temperature is
25-45 DEG C, voltage 15-20kv, syringe needle internal diameter is 0.6-0.9mm, and syringe volume is 2-4ml, and spinneret is pivoted
Revolving 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.
The invention has the advantages that
Iron chloride is first acidified with hydrochloric acid by the present invention, after then addition water and alcohol mixeding liquid are dispersed, is added
Nano bamboo fiber forms the nano bamboo fiber of surface enwrapping ferric oxide, nano-silica is added after being sintered in the effect of ammonium hydroxide
It in SiClx and tetraethyl orthosilicate dispersion liquid, adds after ammonium hydroxide reacted, mix with Vingon lysate and add
Thermal response carries out electrostatic spinning after obtaining spinning solution after progress copolyreaction, and to both having obtained after product processing, the iron chloride after acidification adds
It after entering ammonium hydroxide, using electrostatic adsorption, is enclosed in around nano bamboo fiber, forms hollow iron oxide after oversintering, make
Space adjustment in iron oxide obtains bigger, be conducive to tetraethyl orthosilicate and nano silica and pass through sol-gel progress
Cladding forms silicon dioxide layer, greatly improves hydrophobic effect and adsorptivity, can reduce the adhesion between ferric oxide particles, then
After Vingon progress copolymerized grafting is added, iron oxide particles form good dispersion, stable metal in Vingon
Ion and raising adsorptivity, present invention reduces the adhesions between ferric oxide particles, promote the dispersibility between ferric oxide particles, preparation
Material there are the performances such as excellent hydrophobicity, self-cleaning property, method is simple, easy to operate, and raw material is cheap and easy to get.
Specific embodiment
A kind of preparation method of hollow iron oxide-Vingon electrostatic spinning hydrophobic fiber film, which is characterized in that including
Following steps:
(1) 8 parts by weight iron chloride are added in suitable hydrochloric acid solution and are impregnated 35 minutes, appropriate parts by weight water is added and adjusts
After pH5-7, the nano bamboo fiber of 55 parts by weight of ethanol and 3 parts by weight is added, water-bath is heated to 65 DEG C under nitrogen protection, is added dropwise 6
After the ammonium hydroxide of parts by weight, reacts 4 hours, be sintered in tube furnace, obtain hollow iron oxide, for use；
(2) by 1.5 parts by weight nano silica powders and 0.2 parts by weight tetraethyl orthosilicate ultrasonic disperse in 55 weight
In part dimethyl acetamide, step (1) gains are added, are then added after 3 parts by weight ammonium hydroxide are uniformly dispersed, stirring is anti-at room temperature
Answer 6 hours, for use；
(3) Vingon of 15 parts by weight is dissolved in appropriate dimethyl acetamide, the poly- second two of 0.7 parts by weight is added
Alcohol after being uniformly dispersed, is mixed with step (2) gains, then heats to 80 DEG C and be stirred to react 14 hours, it is molten to obtain spinning
Liquid, for use；
(4) spinning solution obtained by step (3) is fitted into syringe, then the syringe needle installed on syringe is sprayed as spinning
Head, then syringe is mounted on portable hand-held electrostatic spinning machine and constitutes electrostatic spinning apparatus, distance is then adjusted, is opened quiet
The switch of electric spinning device after spinning parameter is arranged, carries out electrostatic spinning, after spinning, gains is placed in 100 DEG C of progress
Heat treatment 2 hours after cooled down at room temperature, both the hollow iron oxide-Vingon electrostatic spinning hydrophobic fiber film.
It is sintered in the step (1) and is being warming up to 800 DEG C from 25 DEG C, heating rate is 1.5 DEG C/min, and heat preservation 3 is small
When, it is sintered in air, then cools to room temperature with the furnace.
In the step (4) in adjustment distance electrostatic spinning apparatus between receiver at a distance from be 9 centimetres.
Setting spinning parameter pushes away column speed 0.01-0.5ml/min for spinning solution in the step (3), and environment temperature is
25-45 DEG C, voltage 15-20kv, syringe needle internal diameter is 0.6-0.9mm, and syringe volume is 2-4ml, and spinneret is pivoted
Revolving 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 hollow iron oxide-Vingon electrostatic spinning hydrophobic fiber film preparation method, which is characterized in that including with
Lower step:
(1) 5-10 parts by weight iron chloride is added in suitable hydrochloric acid solution and is impregnated 20-50 minutes, appropriate parts by weight water tune is added
After saving pH5-7, the nano bamboo fiber of 50-60 parts by weight of ethanol and 1-5 parts by weight is added, water-bath is heated to 50- under nitrogen protection
It 90 DEG C, after the ammonium hydroxide of 5-8 parts by weight is added dropwise, reacts 3-5 hours, is sintered in tube furnace, obtains hollow iron oxide, for use；
(2) by 1-2 parts by weight nano silica powder and 0.1-0.3 parts by weight tetraethyl orthosilicate ultrasonic disperse in 50-80
In parts by weight dimethyl acetamide, step (1) gains are added, after then addition 1-5 parts by weight ammonium hydroxide is uniformly dispersed, at room temperature
It is stirred to react 4-8 hours, for use；
(3) 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, is mixed with step (2) gains, then heats to 75-85 DEG C and be stirred to react 12-16 hours, obtain
Spinning solution, for use；
(4) spinning solution obtained by step (3) is fitted into syringe, then installs syringe needle on syringe as spinning nozzle,
Syringe is mounted on portable hand-held electrostatic spinning machine again and constitutes electrostatic spinning apparatus, then adjusts distance, opens electrostatic
The switch of device for spinning, be arranged spinning parameter after, carry out electrostatic spinning, after spinning, by gains be placed in 80-150 DEG C into
Row heat treatment 1-3 hours after cooled down at room temperature, both the hollow iron oxide-Vingon electrostatic spinning hydrophobic fiber
Film.
2. a kind of hollow iron oxide-Vingon electrostatic spinning hydrophobic fiber film preparation method according to claim 1, special
Sign is, is sintered in the step (1) and is being warming up to 800 DEG C from 25 DEG C, heating rate is 1-2.5 DEG C/min, keeps the temperature 2-4
Hour, it is sintered in air, then cools to room temperature with the furnace.
3. a kind of hollow iron oxide-Vingon electrostatic spinning hydrophobic fiber film preparation method according to claim 1, special
Sign is, in the step (4) in adjustment distance electrostatic spinning apparatus between receiver at a distance from be 7-10 centimetres.
4. a kind of hollow iron oxide-Vingon electrostatic spinning hydrophobic fiber film preparation method according to claim 1, special
Sign is that setting spinning parameter pushes away column speed 0.01-0.5ml/min for spinning solution in the step (3), and environment temperature is
25-45 DEG C, voltage 15-20kv, syringe needle internal diameter is 0.6-0.9mm, and syringe volume is 2-4ml, and spinneret is pivoted
Revolving 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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| 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 CN107313176A (en) | 2017-11-03 |
| CN107313176B true CN107313176B (en) | 2019-03-26 |
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Citations (7)
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| WO2002020132A3 (en) * | 2000-09-05 | 2002-11-28 | Donaldson Co 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 |
| 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 |
Family Cites Families (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| KR101310523B1 (en) * | 2011-07-15 | 2013-09-23 | 삼성전기주식회사 | Porous sheet and method for manufacturing the same |
-
2017
- 2017-06-16 CN CN201710454788.7A patent/CN107313176B/en active Active
Patent Citations (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2002020132A3 (en) * | 2000-09-05 | 2002-11-28 | Donaldson Co 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 |
| 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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| CN107313176A (en) | 2017-11-03 |
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