CN106219989B - A kind of graphene is modified the preparation method of composite glass fiber - Google Patents
A kind of graphene is modified the preparation method of composite glass fiber Download PDFInfo
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- CN106219989B CN106219989B CN201610612845.5A CN201610612845A CN106219989B CN 106219989 B CN106219989 B CN 106219989B CN 201610612845 A CN201610612845 A CN 201610612845A CN 106219989 B CN106219989 B CN 106219989B
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- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
- C03C13/00—Fibre or filament compositions
-
- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03B—MANUFACTURE, SHAPING, OR SUPPLEMENTARY PROCESSES
- C03B37/00—Manufacture or treatment of flakes, fibres, or filaments from softened glass, minerals, or slags
- C03B37/01—Manufacture of glass fibres or filaments
- C03B37/02—Manufacture of glass fibres or filaments by drawing or extruding, e.g. direct drawing of molten glass from nozzles; Cooling fins therefor
-
- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
- C03C25/00—Surface treatment of fibres or filaments made from glass, minerals or slags
- C03C25/10—Coating
- C03C25/48—Coating with two or more coatings having different compositions
- C03C25/52—Coatings containing inorganic materials only
-
- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
- C03C25/00—Surface treatment of fibres or filaments made from glass, minerals or slags
- C03C25/66—Chemical treatment, e.g. leaching, acid or alkali treatment
- C03C25/68—Chemical treatment, e.g. leaching, acid or alkali treatment by etching
Abstract
The invention discloses a kind of graphenes to be modified composite glass fiber and preparation method thereof, and the preparation method comprises the following steps：（1）Prepare glass fibre；（2）Glass fibre pre-processes；（3）The dispersion solution that graphene quantum dot is configured to a concentration of 0.1 ~ 1mg/ml is weighed, solvent is water, acetone or dimethyl sulfoxide (DMSO)；80 ~ 100ml graphene quantum dots are stirred by ultrasonic and disperse solution, pretreated glass fibre is added thereto, ultrasonic agitation speed halves, and impregnates 30 ~ 60min；Glass fibre cleaning is taken out, is dried, for use；（4）It prepares graphene and is modified composite glass fiber.There is obtained composite glass fiber more excellent mechanical strength, products material to be easy to get, and be easy to industrialized production, by the further application range for expanding glass fiber compound material.
Description
Technical field
The present invention relates to the preparation methods that a kind of graphene is modified composite glass fiber.
Background technology
Glass fibre（English original name is：Glass fiber or fiberglass）It is a kind of inorganic non-gold haveing excellent performance
Belong to material, type is various, and advantage is good insulating, heat resistance is strong, corrosion resistance is good, high mechanical strength, but the disadvantage is that property is crisp, resistance to
Mill property is poor.It is usually to be manufactured through techniques such as high temperature melting, wire drawing, doff, woven fabrics as raw material using glass marble or discarded glass
At, a diameter of several microns of monofilament are equivalent to the 1/20 ~ 1/5 of a hairline to twenties meters microns, fine per beam
Dimension precursor is all made of hundreds of even thousands of monofilament.
Allotrope of the graphene as carbon is carbon atom has honeycomb structure by what sp2 orbital hybridizations were formed
Single layer two dimensional crystal material, good mechanical performance, chemical stability that graphene has etc. also will be in fields such as composite materials
It has broad application prospects.
Although graphene is coated on fiberglass surfacing with the physical property of reinforcing glass fiber currently, having, expand
It is in the application in the fields such as resin material, but improvement is not highly desirable, need to be further enhanced.
Invention content
Technical problem to be solved by the invention is to provide a kind of graphenes to be modified composite glass fiber and its preparation side
There is more excellent mechanical strength, products material to be easy to get, be easy to industrialized production for method, obtained composite glass fiber, will
Further expand the application range of glass fiber compound material.
The technical problems to be solved by the invention are achieved by the following technical programs：
A kind of graphene is modified the preparation method of composite glass fiber, includes the following steps：
（1）Prepare glass fibre：By 50 ~ 55% SiO2,10 ~ 15%B2O3,5 ~ 10%Na2O, 10 ~ 15%Al2O3,15 ~ 20%
It after CaO and 0.1 ~ 0.5% multi-walled carbon nanotube or porous graphene crushing, stirring mix, is placed in the corundum crucible of 400mL, uses
Si-Mo rod resistance furnace is melted, and charge temperature is 1370 DEG C, and melting clarifying temp is 1450 ± 10 DEG C, is come out of the stove in 1200 DEG C, is poured into a mould
Molding is sent into Muffle furnace, and in 500 DEG C of annealing, glass is made；Glass obtained is heated to the temperature 1050 of wire drawing viscosity
DEG C, it is drawn into the glass fibre of about 10 μm or so of diameter；
（2）Glass fibre pre-processes：After taking 5 ~ 50 parts of glass fibre split-phases, a concentration of 1 ~ 2mol/L's of 80 ~ 100ml
Acidleach processing is carried out in HCl solution, acidleach processing is carried out under the conditions of 90 ~ 95 DEG C of constant temperature, makes to separate in glass fibre
The NH4Cl solution of 5 ~ 10ml a concentration of 40% is added as buffer in acid in Na2O-B2O3 phased solns in acid, sour processing time is
30~60min；Through rinse dehydration, drying, pretreated glass fiber is obtained；
（3）Weigh graphene quantum dot（Grain size about 2 ~ 10nm）It is configured to the dispersion solution of a concentration of 0.1 ~ 1mg/ml, it is molten
Agent is water, acetone or dimethyl sulfoxide (DMSO)；Ultrasonic agitation（300 ~ 500W ultrasonic powers, 200 ~ 300rpm mixing speeds）80~100ml
Graphene quantum dot disperses solution, and pretreated glass fibre is added thereto, and ultrasonic agitation speed halves, and dipping 30 ~
During which 60min avoids fibre matting, influence to coat effect；Glass fibre cleaning is taken out, is dried, for use；
（4）Weigh the graphene dispersion solution that graphene is configured to a concentration of 0.2 ~ 0.8mg/ml, solvent be water, acetone or
Dimethyl sulfoxide (DMSO)；Ultrasonic agitation（300 ~ 500W ultrasonic powers, 200 ~ 300rpm mixing speeds）80 ~ 100ml graphene dispersions are molten
Step is added in liquid（3）Glass fibre obtained is stirred by ultrasonic 10min, then moves in the reaction kettle of polytetrafluoroethylene (PTFE), 80 ~
15 ~ 30min is kept the temperature at 120 DEG C；
（5）Glass fibre cleaning is taken out, drying obtains graphene and is modified composite glass fiber.
The present invention has the advantages that：
Compared to common glass fibre, the composite glass fiber obtained by the present invention has more excellent mechanics strong
Degree, products material are easy to get, and are easy to industrialized production, by the further application range for expanding glass fiber compound material.Compound glass
Glass fiber can be as the filler of injected plastics material, to increase the mechanical performance of plank, bulk.
Specific implementation mode
With reference to embodiment, the present invention will be described in detail, and embodiment is only the preferred embodiment of the present invention,
It is not limitation of the invention.
Embodiment 1
A kind of graphene is modified the preparation method of composite glass fiber, includes the following steps：
（1）Prepare glass fibre：51% SiO2,15%B2O3,6%Na2O, 10%Al2O3 and 18%CaO crushing, stirring is mixed
It after conjunction, is placed in the corundum crucible of 400mL, is melted with Si-Mo rod resistance furnace, charge temperature is 1370 DEG C, and melting clarifying temp is
It 1450 ± 10 DEG C, comes out of the stove in 1200 DEG C, moulding by casting is sent into Muffle furnace, and in 500 DEG C of annealing, glass is made；By glass obtained
Glass is heated to 1050 DEG C of the temperature of wire drawing viscosity, is drawn into the glass fibre of about 10 μm or so of diameter；
（2）Glass fibre pre-processes：After taking 45 parts of glass fibre split-phases, in the HCl solution of a concentration of 2mol/L of 100ml
Acidleach processing is carried out, acidleach processing is carried out under the conditions of 95 DEG C of constant temperature, and the Na2O-B2O3 phased solns separated in glass fibre are made
The NH4Cl solution of 5ml a concentration of 40% is added in acid, acid as buffer, sour processing time is 30min；Through rinse dehydration,
Drying, obtains pretreated glass fiber；
（3）Weigh graphene quantum dot（Grain size about 2nm）It is configured to the dispersion solution of a concentration of 0.3mg/ml, solvent is
Water, acetone or dimethyl sulfoxide (DMSO)；Ultrasonic agitation（500W ultrasonic powers, 200rpm mixing speeds）100ml graphene quantum dots point
Solution is dissipated, pretreated glass fibre is added thereto, ultrasonic agitation speed halves, and impregnates 60min, during which fiber is avoided to twine
Knot influences to coat effect；Glass fibre cleaning is taken out, is dried, for use；
（4）The graphene dispersion solution that graphene is configured to a concentration of 0.5mg/ml is weighed, solvent is water, acetone or diformazan
Base sulfoxide；Ultrasonic agitation（500W ultrasonic powers, 200rpm mixing speeds）Step is added in 80ml graphene dispersion solution（3）System
The glass fibre obtained is stirred by ultrasonic 10min, then moves in the reaction kettle of polytetrafluoroethylene (PTFE), 15min is kept the temperature at 100 DEG C；
（5）Glass fibre cleaning is taken out, drying obtains graphene and is modified composite glass fiber.
Embodiment 2
A kind of graphene is modified the preparation method of composite glass fiber, includes the following steps：
（1）Prepare glass fibre：51% SiO2,15%B2O3,6%Na2O, 10%Al2O3 and 18%CaO crushing, stirring is mixed
It after conjunction, is placed in the corundum crucible of 400mL, is melted with Si-Mo rod resistance furnace, charge temperature is 1370 DEG C, and melting clarifying temp is
It 1450 ± 10 DEG C, comes out of the stove in 1200 DEG C, moulding by casting is sent into Muffle furnace, and in 500 DEG C of annealing, glass is made；By glass obtained
Glass is heated to 1050 DEG C of the temperature of wire drawing viscosity, is drawn into the glass fibre of about 10 μm or so of diameter；
（2）Glass fibre pre-processes：After taking 20 parts of glass fibre split-phases, in the HCl solution of a concentration of 2mol/L of 100ml
Acidleach processing is carried out, acidleach processing is carried out under the conditions of 95 DEG C of constant temperature, and the Na2O-B2O3 phased solns separated in glass fibre are made
The NH4Cl solution of 5ml a concentration of 40% is added in acid, acid as buffer, sour processing time is 30min；Through rinse dehydration,
Drying, obtains pretreated glass fiber；
（3）Weigh graphene quantum dot（Grain size about 5nm）It is configured to the dispersion solution of a concentration of 0.1mg/ml, solvent is
Water, acetone or dimethyl sulfoxide (DMSO)；Ultrasonic agitation（500W ultrasonic powers, 200rpm mixing speeds）100ml graphene quantum dots point
Solution is dissipated, pretreated glass fibre is added thereto, ultrasonic agitation speed halves, and impregnates 60min, during which fiber is avoided to twine
Knot influences to coat effect；Glass fibre cleaning is taken out, is dried, for use；
（4）The graphene dispersion solution that graphene is configured to a concentration of 0.2mg/ml is weighed, solvent is water, acetone or diformazan
Base sulfoxide；Ultrasonic agitation（500W ultrasonic powers, 200rpm mixing speeds）Step is added in 100ml graphene dispersion solution（3）System
The glass fibre obtained is stirred by ultrasonic 10min, then moves in the reaction kettle of polytetrafluoroethylene (PTFE), 30min is kept the temperature at 80 DEG C；
（5）Glass fibre cleaning is taken out, drying obtains graphene and is modified composite glass fiber.
Embodiment 3
A kind of graphene is modified the preparation method of composite glass fiber, includes the following steps：
（1）Prepare glass fibre：51% SiO2,15%B2O3,6%Na2O, 10%Al2O3 and 18%CaO crushing, stirring is mixed
It after conjunction, is placed in the corundum crucible of 400mL, is melted with Si-Mo rod resistance furnace, charge temperature is 1370 DEG C, and melting clarifying temp is
It 1450 ± 10 DEG C, comes out of the stove in 1200 DEG C, moulding by casting is sent into Muffle furnace, and in 500 DEG C of annealing, glass is made；By glass obtained
Glass is heated to 1050 DEG C of the temperature of wire drawing viscosity, is drawn into the glass fibre of about 10 μm or so of diameter；
（2）Glass fibre pre-processes：After taking 50 parts of glass fibre split-phases, in the HCl solution of a concentration of 2mol/L of 100ml
Acidleach processing is carried out, acidleach processing is carried out under the conditions of 95 DEG C of constant temperature, and the Na2O-B2O3 phased solns separated in glass fibre are made
The NH4Cl solution of 5ml a concentration of 40% is added in acid, acid as buffer, sour processing time is 30min；Through rinse dehydration,
Drying, obtains pretreated glass fiber；
（3）Weigh graphene quantum dot（Be made of three kinds of different-grain diameter equalizations, grain size be respectively 2 ~ 4nm, 5 ~ 7nm and 7 ~
10nm）It is configured to the dispersion solution of a concentration of 0.6mg/ml, solvent is water, acetone or dimethyl sulfoxide (DMSO)；Ultrasonic agitation（500W is super
Acoustical power, 200rpm mixing speeds）100ml graphene quantum dots disperse solution, and pretreated glass fibre is added thereto,
Ultrasonic agitation speed halves, and impregnates 60min, during which avoids fibre matting, influences to coat effect；Glass fibre cleaning is taken out, is dried
It is dry, for use；
（4）The graphene dispersion solution that graphene is configured to a concentration of 0.8mg/ml is weighed, solvent is water, acetone or diformazan
Base sulfoxide；Ultrasonic agitation（500W ultrasonic powers, 200rpm mixing speeds）Step is added in 80ml graphene dispersion solution（3）System
The glass fibre obtained is stirred by ultrasonic 10min, then moves in the reaction kettle of polytetrafluoroethylene (PTFE), 20min is kept the temperature at 120 DEG C；
（5）Glass fibre cleaning is taken out, drying obtains graphene and is modified composite glass fiber.
Embodiment 4
Based on the preparation method of embodiment 1, the difference is that：Step（1）, specially：By 50.9% SiO2,15%
B2O3,6%Na2O, 10%Al2O3,18%CaO and 0.1% multi-walled carbon nanotube（OD about 8nm）After crushing, stirring mixing, it is placed on
It in the corundum crucible of 400mL, is melted with Si-Mo rod resistance furnace, charge temperature is 1370 DEG C, and melting clarifying temp is 1450 ± 10
DEG C, it comes out of the stove in 1200 DEG C, moulding by casting is sent into Muffle furnace, and in 500 DEG C of annealing, glass is made；Glass obtained is heated to
1050 DEG C of the temperature of wire drawing viscosity is drawn into the glass fibre of about 10 μm or so of diameter.
Embodiment 5
Based on the preparation method of embodiment 1, the difference is that：Step（1）, specially：By 50.5% SiO2,15%
B2O3,6%Na2O, 10%Al2O3,18%CaO and 0.5% multi-walled carbon nanotube（OD about 8nm）After crushing, stirring mixing, it is placed on
It in the corundum crucible of 400mL, is melted with Si-Mo rod resistance furnace, charge temperature is 1370 DEG C, and melting clarifying temp is 1450 ± 10
DEG C, it comes out of the stove in 1200 DEG C, moulding by casting is sent into Muffle furnace, and in 500 DEG C of annealing, glass is made；Glass obtained is heated to
1050 DEG C of the temperature of wire drawing viscosity is drawn into the glass fibre of about 10 μm or so of diameter.
Embodiment 6
Based on the preparation method of embodiment 1, the difference is that：Step（1）, specially：By 50.7% SiO2,15%
B2O3,6%Na2O, 10%Al2O3,18%CaO and 0.3% porous graphene（2 ~ 5 layers, hole size about 3 ~ 6nm）Crushing, stirring mixes
Afterwards, it is placed in the corundum crucible of 400mL, is melted with Si-Mo rod resistance furnace, charge temperature is 1370 DEG C, and melting clarifying temp is
It 1450 ± 10 DEG C, comes out of the stove in 1200 DEG C, moulding by casting is sent into Muffle furnace, and in 500 DEG C of annealing, glass is made；By glass obtained
Glass is heated to 1050 DEG C of the temperature of wire drawing viscosity, is drawn into the glass fibre of about 10 μm or so of diameter.
Comparative example 1
A kind of graphene is modified the preparation method of composite glass fiber, includes the following steps：
（1）The sodium hydroxide solution that molar concentration is 8mol/L is configured, glass fibre is put into sodium hydroxide solution, is surpassed
Sonicated 60min obtains the glass fibre of surface roughening, through rinse dehydration, drying, obtains pretreated glass fiber；
（2）The graphene dispersion solution that graphene is configured to a concentration of 0.5mg/ml is weighed, solvent is water, acetone or diformazan
Base sulfoxide；Ultrasonic agitation（500W ultrasonic powers, 200rpm mixing speeds）Step is added in 80ml graphene dispersion solution（1）System
The glass fibre obtained is stirred by ultrasonic 10min, then moves in the reaction kettle of polytetrafluoroethylene (PTFE), 15min is kept the temperature at 100 DEG C；
（3）Glass fibre cleaning is taken out, drying obtains graphene and is modified composite glass fiber.
Comparative example 2
A kind of graphene is modified the preparation method of composite glass fiber, includes the following steps：
（1）Prepare glass fibre：51% SiO2,15%B2O3,6%Na2O, 10%Al2O3 and 18%CaO crushing, stirring is mixed
It after conjunction, is placed in the corundum crucible of 400mL, is melted with Si-Mo rod resistance furnace, charge temperature is 1370 DEG C, and melting clarifying temp is
It 1450 ± 10 DEG C, comes out of the stove in 1200 DEG C, moulding by casting is sent into Muffle furnace, and in 500 DEG C of annealing, glass is made；By glass obtained
Glass is heated to 1050 DEG C of the temperature of wire drawing viscosity, is drawn into the glass fibre of about 10 μm or so of diameter；
（2）The graphene dispersion solution that graphene is configured to a concentration of 0.5mg/ml is weighed, solvent is water, acetone or diformazan
Base sulfoxide；Ultrasonic agitation（500W ultrasonic powers, 200rpm mixing speeds）Step is added in 80ml graphene dispersion solution（1）System
The glass fibre obtained is stirred by ultrasonic 10min, then moves in the reaction kettle of polytetrafluoroethylene (PTFE), 15min is kept the temperature at 100 DEG C；
（3）Glass fibre cleaning is taken out, drying obtains graphene and is modified composite glass fiber.
Graphene made from embodiment 1 ~ 6 and comparative example 1 ~ 2 is modified composite glass fiber and commercially available glass fibre by normal
Rule method is applied in resin composite materials（Below by taking nylon material as an example）And quantitative measurement is carried out, as a result it see the table below：
Embodiments of the present invention above described embodiment only expresses, the description thereof is more specific and detailed, but can not
Therefore it is interpreted as the limitation to the scope of the claims of the present invention, as long as skill obtained in the form of equivalent substitutions or equivalent transformations
Art scheme should all be fallen within the scope and spirit of the invention.
Claims (1)
1. a kind of graphene is modified the preparation method of composite glass fiber, include the following steps：
（1）Prepare glass fibre：By 51% SiO2、15%B2O3、6%Na2O、10%Al2O3After being mixed with 18%CaO crushing, stirrings, put
In the corundum crucible of 400mL, with Si-Mo rod resistance furnace be melted, charge temperature be 1370 DEG C, melting clarifying temp be 1450 ±
It 10 DEG C, comes out of the stove in 1200 DEG C, moulding by casting is sent into Muffle furnace, and in 500 DEG C of annealing, glass is made；Glass obtained is heated
To 1050 DEG C of the temperature of wire drawing viscosity, it is drawn into the glass fibre of 10 μm of diameter；
（2）Glass fibre pre-processes：After taking 20 parts of glass fibre split-phases, carried out in the HCl solution of a concentration of 2mol/L of 100mL
Acidleach is handled, and acidleach processing is carried out under the conditions of 95 DEG C of constant temperature, and the Na separated in glass fibre is made2O-B2O3Phased soln in acid,
The NH of 5mL a concentration of 40% is added in acid4For Cl solution as buffer, sour processing time is 30min；Through rinse dehydration, dry,
Obtain pretreated glass fiber；
（3）The graphene quantum dot for weighing grain size 5nm is configured to the dispersion solution of a concentration of 0.1mg/mL, and solvent is water, acetone
Or dimethyl sulfoxide (DMSO)；100mL graphene quantum dots are stirred by ultrasonic and disperse solution, pretreated glass fibre is added thereto,
Ultrasonic agitation speed halves, and impregnates 60min, during which avoids fibre matting, influences to coat effect；Glass fibre cleaning is taken out, is dried
It is dry, for use；
（4）The graphene dispersion solution that graphene is configured to a concentration of 0.2mg/mL is weighed, solvent is that water, acetone or dimethyl are sub-
Sulfone；100mL graphene dispersion solution is stirred by ultrasonic, step is added（3）Glass fibre obtained is stirred by ultrasonic 10min, then moves
Into the reaction kettle of polytetrafluoroethylene (PTFE), 30min is kept the temperature at 80 DEG C；
（5）Glass fibre cleaning is taken out, drying obtains graphene and is modified composite glass fiber.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| RU2737438C1 (en) * | 2020-06-18 | 2020-11-30 | Акционерное общество "НПО Стеклопластик" | Method of producing high-temperature resistant silica fiber |
Families Citing this family (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109098030A (en) * | 2018-08-24 | 2018-12-28 | 宿迁南航新材料与装备制造研究院有限公司 | A kind of preparation method of graphene modified glass-fiber paper |
| CN111087176A (en) * | 2018-10-23 | 2020-05-01 | 南京化学工业园环保产业协同创新有限公司 | Graphene material composite glass and preparation method thereof |
| CN112663330B (en) * | 2019-12-24 | 2023-01-06 | 中科量子(广东)医疗技术有限公司 | Fiber, non-woven fabric, mask cloth and mask containing nano graphene and preparation method |
| CN111267427B (en) * | 2020-03-03 | 2022-04-19 | 长安大学 | Anti-impact light plastic cover plate material for cable duct and preparation method thereof |
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| CN101003418A (en) * | 2006-07-14 | 2007-07-25 | 上海兰度科技有限公司 | Composite Nano fiber of directional arranged Nano carbon tube, high-speed preparation device, and preparation method |
| CN104163578A (en) * | 2014-07-22 | 2014-11-26 | 杭州杭复新材料科技有限公司 | Preparation method of graphene coated composite glass fiber |
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| RU2737438C1 (en) * | 2020-06-18 | 2020-11-30 | Акционерное общество "НПО Стеклопластик" | Method of producing high-temperature resistant silica fiber |
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