CN106633391B - A kind of abductive approach of polypropylene/glass fiber interface scorching structure - Google Patents
A kind of abductive approach of polypropylene/glass fiber interface scorching structure Download PDFInfo
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- CN106633391B CN106633391B CN201611070812.9A CN201611070812A CN106633391B CN 106633391 B CN106633391 B CN 106633391B CN 201611070812 A CN201611070812 A CN 201611070812A CN 106633391 B CN106633391 B CN 106633391B
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K9/00—Use of pretreated ingredients
- C08K9/02—Ingredients treated with inorganic substances
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K7/00—Use of ingredients characterised by shape
- C08K7/02—Fibres or whiskers
- C08K7/04—Fibres or whiskers inorganic
- C08K7/14—Glass
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K9/00—Use of pretreated ingredients
- C08K9/04—Ingredients treated with organic substances
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K9/00—Use of pretreated ingredients
- C08K9/08—Ingredients agglomerated by treatment with a binding agent
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2205/00—Polymer mixtures characterised by other features
- C08L2205/24—Crystallisation aids
Abstract
The present invention provides a kind of glass fibre/polypropylene interface scorching structure abductive approach, this method prepares the stabilized aqueous dispersion liquid of carbon nanotubes and polypropylene nucleater first with wet grinding, the composition of the dispersion liquid is: 1~3% carbon nanotube, 0.5~2% surfactant, 0~1% polypropylene nucleater, 0~10% cosolvent, 84~98.5% deionized waters.Then infusion method is used, glass fibre is continuously infiltrated in carbon nanotube and nucleation agent dispersing liquid, prepare the glass fibre that there are carbon nanotube and polypropylene nucleater coating in surface, the presence of fiber surface carbon nanotube and nucleating agent can induce polypropylene to crystallize along fiber, scorching structure is formed in glass fibre/polypropylene interface, glass fibre and polyacrylic interface shear strength can be improved in the scorching structure of interface.
Description
Technical field
The present invention relates to a kind of abductive approach of polypropylene/glass fiber interface scorching structure, more specifically, being to be related to carbon
The dispersion in water of nanotube and polypropylene nucleater and infusion method continuous surface handle glass fibre, and this surface is contained carbon and received
The glass fibre of mitron and polypropylene nucleater can induce the formation of polypropylene/glass fiber interface scorching structure.
Background technique
Glass fibre reinforced polymer composites are widely used in the fields such as electrical, electronics, the energy and automobile.For fibre
The study on the modification of dimension enhancing polymer is mainly around polymeric matrix, the improvement of fibre reinforcement nature and fiber/poly-
Close three aspect expansion of improvement of object basal body interface property.Wherein fiber/resin interface is played between matrix resin and fiber
Function served as bridge, influence are puted forth effort to be transmitted to fiber by matrix.Polypropylene is a kind of low-density, the polymer of hemicrystalline, with automobile
The raising that industrial development, automotive light weight technology require, glass fiber reinforced polypropylene get the attention and apply.For glass
Fiber reinforced polypropylene material lacks active function groups on macromolecular chain, causes since polypropylene is a kind of non-polar polymer
The interface cohesion of polypropylene and glass fibre is poor.
The interface of polypropylene/glass fiber is improved can be by induction polypropylene in glass fibre interfacial crystallization, shape
It is realized at scorching structure.The presence of polypropylene/glass fiber interface scorching structure can improve the combination of matrix and fiber, mention
High interface shear strength.Commercial fiber glass itself does not have the ability of induction scorching structure, can be in order to form scorching structure
Nucleating agent is introduced into fiberglass surfacing.Nucleating agent is a kind of processing aid, can accelerate crystalling propylene, increases heterogeneous nucleation
Dot density reduces crystalline size, crystal grain refinement.One kind is provided in Chinese patent CN104356642 in fiberglass surfacing
The glass fiber compound material preparation method of the load nucleating agent of nucleating agent is introduced, introducing nucleating agent in fiberglass surfacing can be with
Fiberglass surfacing is set to generate a large amount of nucleating points, scorching structure is induced to be formed.However, nucleating agent is introduced separately into fiberglass surfacing
Few, caducous problem that there are introduction volumes, this will lead to fiberglass surfacing nucleation substance deficiency, scorching structural development is not filled
Point.
Carbon nanotube is a kind of monodimension nanometer material, can regard a kind of as and be curled into pipe by hexagon arrangement carbon atomic layer
The carbon structure of shape.There is carbon nanotube high draw ratio, superior mechanical property, electric conductivity and heating conduction can be used as
The packing material of polymer is for polymer-modified.Carbon nanotube is found to have effect (Assouline E etc. of heterogeneous nucleation
In Journal of Polymer Science Part B Polymer Physics, 2003,41 (5): in 520), it can lure
It leads polypropylene and forms α crystalline substance.Carbon nanotube is due to its feature easy to reunite, it is difficult to disperse in polymer and solution, limit carbon and receive
The application of mitron.
Summary of the invention
It is an object of the present invention to solve to be introduced separately into nucleating agent to fiberglass surfacing introduction volume few, easy to fall off, glass
The problem that fiber surface nucleation substance is insufficient, scorching structural development is insufficient, and a kind of polypropylene/glass fiber interface provided
The abductive approach of scorching structure, specific embodiment are as follows:
A kind of abductive approach of polypropylene/glass fiber interface scorching structure, comprises the following specific steps that:
(1) preparation of carbon nanotube and nucleation agent dispersing liquid: 0~10g nucleating agent is dissolved in cosolvent, 100~
5~10min is stirred under 200rpm speed, is dissolved it sufficiently and is obtained nucleation agent dispersing liquid, by nucleation agent dispersing liquid and 5~20g
Surfactant is added in deionized water, and with the mixing speed of 100~200rpm, stirring 5~10min makes it sufficiently dissolve dispersion
Obtain suspension.Wet grinding device is added in suspension, 10~30g carbon nanotube is slowly added to, is fully ground to obtain 1kg carbon
The dispersion liquid of nanotube and nucleating agent mixing.
The composition of the carbon nanotube and nucleation agent dispersing liquid is as follows: 1~3% carbon nanotube, 0.5~2% surface-active
Agent, 0~1% polypropylene nucleater, 0~10% cosolvent, 84~98.5% deionized waters.
The carbon nanotube is multi-walled carbon nanotube, and diameter is in 15~50nm, and length is at 1~3 μm.
The surfactant is cetyl trimethylammonium bromide (CTAB), dodecyl sodium sulfate (SDS), dodecane
Base benzene sulfonic acid sodium salt (SDBS), kayexalate, sodium lignin sulfonate, polyvinylpyrrolidone (PVP), triton x-100,
One or more of Tween 80, carbon nanotube aqueous dispersion (TNWDIS).
The polypropylene nucleater is sodium benzoate, 1,3:2,4 dibenzyl sorbitols (DBS), 2,2 '-di-2-ethylhexylphosphine oxides
(4,6- di-tert-butyl-phenyl) sodium phosphate (NA11), 2,2 '-di-2-ethylhexylphosphine oxides (4,6- di-tert-butyl-phenyl) aluminum phosphate basic salt
(NA21), two rings [2.2.1] heptane dicarboxylic acid sodium (HPN-68L), one or more of in aromatic amides (TMB-5).
The cosolvent is one or more of methanol, ethyl alcohol, isopropanol, butanol, acetone, deionized water.
The wet grinding device is horizontal mill, and abrasive media is the zirconium pearl that diameter is 0.6~0.8mm, and grinding turns
Speed is 3000rpm, and milling time is 0.5~1h.
(2) continuous infiltration apparatus the continuous infiltration processing of glass fibre: is added in carbon nanotube and nucleation agent dispersing liquid
In immersion slot, by fiber coiling machine travel glass fibre by immersion slot and two sections of prebake cartridge heaters, table is continuously prepared
Contain the glass fibre volume of carbon nanotube and nucleating agent in face.By glass fibre volume dry 6 in 40~60 DEG C of convection oven~
12h。
The fiber coiling machine travel speed is 5~8m/min, and two sections of prebake heating barrel temperatures are in 100-200
℃。
The present invention using wet grinding preparation carbon nanotube and nucleating agent stable dispersion dispersion liquid, using infusion method by carbon
Nanotube and nucleating agent introduce fiberglass surfacing simultaneously, and method is simple and easy, can be with continuous production.Fiberglass surfacing carbon
The coating of nanotube and nucleating agent provides enough nucleation capabilities for fiberglass surfacing, can efficiently induce scorching structure
Formation, improve interface cohesion, improve interface shear strength.
Detailed description of the invention
Fig. 1 is after 1% carbon nano tube dispersion liquid in embodiment 4 is handled, and there is the glass fiber single filament of carbon nanotube on surface
The electromicroscopic photograph of sample.
Fig. 2 is that the surface in embodiment 4 has carbon nanotube monofilament glass fibre/polypropylene scorching structure petrographic microscope to shine
Piece.
Fig. 3 be in embodiment 6 be nucleated agent dispersing liquid processing containing 1% carbon nanotube and 0.5%TMB-5 after, there is carbon on surface
The electromicroscopic photograph of the glass fiber single filament of nanotube and TMB-5.
Fig. 4 is that the surface in embodiment 6 has carbon nanotube and TMB-5 monofilament glass fibre/polypropylene specimen scorching structure
Petrographic microscope photo.
Fig. 5 is not infiltrate processing commercial fiber glass monfil surface electromicroscopic photograph in comparative example.
Fig. 6 is not infiltrate processing monofilament glass fibre/polypropylene specimen petrographic microscope photo in comparative example.
Specific embodiment
Particular content of the invention is further illustrated with specific case study on implementation below.The content of present invention is not limited only to implement
Example, other change and modification made under without departing substantially from spirit and scope of the invention to those skilled in the art are still
Within that scope of the present invention.
Embodiment 1
Carbon nano tube dispersion liquid is prepared, the composition of the dispersion liquid is: multi-walled carbon nanotube 1%, dodecyl sodium sulfate
0.5%, deionized water 98.5%.Lauryl sodium sulfate is previously dissolved in deionized water, stirring 10min sufficiently dissolves, then
It is slowly added to carbon nanotube to grinding device, grinds 1h, revolving speed 3000rpm, abrasive media is 0.6~0.8mm zirconium pearl.
Embodiment 2
Carbon nano tube dispersion liquid is prepared, the composition of the dispersion liquid is: multi-walled carbon nanotube 1%, sodium lignin sulfonate
0.5%, deionized water 98.5%.Sodium lignin sulfonate is dissolved in deionized water, stirring 10min sufficiently dissolves, then to grinding
Device is slowly added to carbon nanotube, grinds 1h, revolving speed 3000rpm, and abrasive media is 0.6~0.8mm zirconium pearl.
Embodiment 3
Carbon nano tube dispersion liquid is prepared, the composition of the dispersion liquid is: multi-walled carbon nanotube 3%, neopelex
1.5%, deionized water 95.5%.Neopelex is dissolved in deionized water, stirring 10min sufficiently dissolves, then to
Grinding device is slowly added to carbon nanotube, grinds 1h, revolving speed 3000rpm, and abrasive media is 0.6~0.8mm zirconium pearl.
Embodiment 4
Carbon nano tube dispersion liquid is prepared, the composition of the dispersion liquid is: multi-walled carbon nanotube 1%, neopelex
0.5%, deionized water 98.5%.Neopelex is dissolved in deionized water, stirring 10min sufficiently dissolves, then to
Grinding device is slowly added to carbon nanotube, grinds 1h, revolving speed 3000rpm, and abrasive media is 0.6~0.8mm zirconium pearl.By continuous
Infiltration apparatus continuous processing glass fibre obtains the glass fibre for having carbon nanotube to surface, and by treated, glass fibre volume is put
Enter 40 DEG C of air dry ovens, dries 6h.Glass fibre volume after processing is separated into monfil and prepares monofilament glass fibre/poly- third
Alkene sample is for the shooting of scorching structure and interface shear strength test.The glass fibre is Chongqing world composite material
ER4305PM。
Fig. 1 is after 1% carbon nano tube dispersion liquid is handled, and surface has the Electronic Speculum of the glass fiber single filament sample of carbon nanotube to shine
Piece.
Fig. 2 is that surface has carbon nanotube monofilament glass fibre/polypropylene specimen scorching structure petrographic microscope photo.
Embodiment 5
Carbon nanotube and nucleating agent sodium benzoate dispersion liquid are prepared by wet grinding, the composition of the dispersion liquid is: multi wall
Carbon nanotube 1%, neopelex 0.5%, sodium benzoate 0.5%, deionized water 98%.Pass through continuous infiltration apparatus
Continuous processing glass fibre, obtains the glass fibre for having carbon nanotube and nucleating agent sodium benzoate to surface, will treated glass
Fiber rolls into 40 DEG C of air dry ovens, dries 6h.Glass fibre volume after processing is separated into monfil and prepares monofilament glass
Fiber/polypropylene sample is for the shooting of scorching structure and interface shear strength test.The glass fibre is that the Chongqing world is compound
The ER4305PM of material.
Embodiment 6
Carbon nanotube and nucleating agent TMB-5 dispersion liquid are prepared by wet grinding, the composition of the dispersion liquid is: multi wall carbon is received
Mitron 1%, neopelex 0.5%, TMB-5 0.5%, acetone 5%, deionized water 93%.TMB-5 is dissolved in third
It in ketone, then is dissolved in deionized water together with neopelex, wet grinding device and carbon nanotube one is then added
Play grinding preparation carbon nanotube and TMB-5 dispersion liquid.By continuous infiltration apparatus continuous processing glass fibre, obtaining to surface has carbon
The glass fibre of nanotube and nucleating agent TMB-5, by treated, glass fibre rolls into 40 DEG C of air dry ovens, dries 6h.
By after processing glass fibre volume separate monfil prepare monofilament glass fibre/polypropylene specimen be used for scorching structure shooting and
Interface shear strength test.
The glass fibre is the ER4305PM of Chongqing world composite material.
The TMB-5 for Shanxi coalification aromatic amides polypropylene nucleater TMB-5.
Fig. 3 is after being nucleated agent dispersing liquid processing containing 1% carbon nanotube and 0.5%TMB-5, and there are carbon nanotube and TMB- in surface
The electromicroscopic photograph of 5 glass fiber single filament.
Fig. 4 is that surface has carbon nanotube and TMB-5 monofilament glass fibre/polypropylene specimen scorching structure petrographic microscope to shine
Piece.
Comparative example
A monofilament glass fibre is removed from commercial fiber glass volume, monofilament glass fibre/polypropylene specimen is prepared and uses
In the shooting of scorching structure and interface shear strength test.The monofilament glass fibre is handled without any infiltration.
Fig. 5 is not infiltrate processing commercial fiber glass monofilament fiberglass surfacing electromicroscopic photograph.
Fig. 6 is not infiltrate processing monofilament glass fibre/polypropylene specimen petrographic microscope photo.
In embodiment in carbon nanotube and the dispersion particle diameter and particle diameter distribution index (PDI) column and table 1 of nucleation agent dispersing liquid.
Table 1
As shown in table 1, wet grinding preparation carbon nanotube and the equal particle size results explanation of nucleation agent dispersing liquid Z: comparison is implemented
Example 1~4, in the case where nucleating agent component is not added, embodiment 4 has optimum dispersion partial size.Comparative example 4~6 can be sent out
Existing nucleating agent does not have significantly to influence the dispersion effect of carbon nanotube after being added, and can form stable dispersions with carbon nanotube.
Interface shear strength described in embodiment 4~6 and comparative example, be according to polymer microlayer model unsticking method test and
, in each embodiment and comparative example interface shear strength test data column and table 2.
Scorching structure polarized light microscopy photo is that record is shot under isothermal crystal process in embodiment 4~6 and comparative example,
The isothermal crystal 5min at 130 DEG C records a photo every 30s, scorching thickness column when isothermal crystal 5min in table 2.
Table 2
As shown in table 1, it can produce scorching structure by the method for embodiment 4~6, and there is no scorching structure in comparative example
It generates, illustrates that the method according to the invention can induce the generation of scorching structure, and interface shear strength is improved, wherein
Embodiment 6 improves 58.1%.Comparative example 4, embodiment 5~6 have bigger scorching thickness and higher interface shearing strong
Degree illustrates the present invention while introducing carbon nanotube and nucleating agent and can efficiently induce scorching structure to the method for fiberglass surfacing
It generates, increases substantially interface shear strength.
Embodiment 7
Carbon nanotube and nucleating agent TMB-5 dispersion liquid are prepared, the composition of the dispersion liquid is: multi-walled carbon nanotube 3%,
TNWDIS1.5%, TMB-5 nucleating agent 1%, acetone 10%, deionized water 84.5%.TMB-5 is dissolved in acetone, then with 12
Sodium alkyl benzene sulfonate is dissolved in deionized water together, and then addition wet grinding device grinding together with carbon nanotube prepares carbon and receives
Mitron and TMB-5 dispersion liquid.By continuous infiltration apparatus continuous processing glass fibre, obtaining to surface has carbon nanotube and nucleating agent
The glass fibre of TMB-5, by treated, glass fibre rolls into 40 DEG C of air dry ovens, dries 6h.Glass fibers after handling
Dimension volume separate monfil prepare monofilament glass fibre/polypropylene specimen for scorching structure shooting and interface shear strength survey
Examination.
Carbon nanotube and nucleating agent are introduced fiberglass surfacing simultaneously using infusion method by the present invention, can overcome nucleating agent
It is introduced separately into that fiberglass surfacing introduction volume is few, caducous problem.Carbon nanotube can form network in fiberglass surfacing,
Nucleating agent distribution of particles is fixed in carbon managed network, can be with to guarantee that fiberglass surfacing has enough nucleation substances
The generation of efficient induction fiberglass surfacing scorching structure, guarantees the abundant development of scorching structure, improves interface cohesion, improves
Boundary strength.Carbon nanotube used in impregnation process and nucleating agent stable dispersions are prepared by wet grinding, wet process
Grinding can solve the dispersion of carbon nanotube in water, it is ensured that the coating effect of carbon nanotube and nucleating agent in impregnation process
Fruit.
Claims (4)
1. a kind of abductive approach of polypropylene/glass fiber interface scorching structure, which is characterized in that the scorching abductive approach includes
Following steps:
(1) the stabilized aqueous dispersion liquid of carbon nanotubes and polypropylene nucleater is prepared using wet grinding device, described point
The composition of dispersion liquid is: 1~3% carbon nanotube, 0.5~2% surfactant, 0~1% polypropylene nucleater, 0~10% hydrotropy
Agent, 84~98.5% deionized waters；The wet grinding device, the dispersion abrasive media used is the zirconium of 0.6~0.8mm
Pearl, grinding revolving speed are 3000rpm, milling time 1h；
(2) carbon nanotube and nucleating agent aqueous liquid dispersion that will be prepared in step (1), is packed into the immersion slot of continuous infiltration apparatus
In, by fiber coiling machine travel glass fibre, continuously prepare the glass that there are carbon nanotube and polypropylene nucleater coating in surface
Glass fiber；
(3) glass fibre obtained in step (2) is rolled into and dries 6~12h in convection oven under 40~60 °C, formed poly-
Propylene/glass fibre interface scorching structure.
2. a kind of abductive approach of polypropylene/glass fiber interface scorching structure according to claim 1, feature exist
In the carbon nanotube is the technical grade multi-walled carbon nanotube that diameter is less than 50nm；The surfactant is cetyl three
Methyl bromide ammonium, dodecyl sodium sulfate, neopelex, kayexalate, sodium lignin sulfonate, polyethylene
One or more of pyrrolidones, triton x-100, Tween 80, bromination octadecyl imidazolium.
3. a kind of abductive approach of polypropylene/glass fiber interface scorching structure according to claim 1, feature exist
In the polypropylene nucleater is sodium benzoate, 1,3:2,4 dibenzyl sorbitols, 2,2 '-di-2-ethylhexylphosphine oxides (4,6- bis- tertiary fourths
Base phenyl) sodium phosphate, 2,2 '-di-2-ethylhexylphosphine oxides (4,6- di-tert-butyl-phenyl) aluminum phosphate basic salt, two rings [2.2.1] heptane dicarboxyl
One or more of sour sodium, aromatic amides.
4. a kind of abductive approach of polypropylene/glass fiber interface scorching structure according to claim 1, feature exist
In the continuous infiltration apparatus is by a fiber immersion slot, two sections of prebake cartridge heaters and fiber coiling machine composition；Institute
Prebake heating barrel temperatures are stated at 100-200 °C.
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| CN107189209B (en) * | 2017-06-26 | 2019-12-31 | 西华大学 | Fiber/polypropylene composite material and preparation method thereof |
| CN111234471A (en) * | 2018-11-28 | 2020-06-05 | 合肥杰事杰新材料股份有限公司 | PBT composite material with low linear thermal expansion coefficient and preparation method thereof |
| CN110343290A (en) * | 2019-07-25 | 2019-10-18 | 赣州蓝风科技有限公司 | Composite nucleating agent and its preparation method and application |
| CN110922680A (en) * | 2019-11-15 | 2020-03-27 | 江苏东方电缆材料有限公司 | Basalt fiber reinforced and toughened polypropylene-based composite material and preparation method thereof |
| CN111393744B (en) * | 2020-03-26 | 2023-06-23 | 南京京锦元科技实业有限公司 | TPE material with antibacterial conductivity and preparation method thereof |
| CN112624631A (en) * | 2020-12-17 | 2021-04-09 | 四川轻化工大学 | Inducing method of glass fiber polypropylene interface transverse crystal structure |
| CN113402740B (en) * | 2021-06-16 | 2022-10-04 | 西南大学 | Method for inducing transverse crystal structure of polypropylene/bamboo fiber interface |
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