CN110041694A - A kind of preparation method of low warp glass fiber enhancing nylon - Google Patents
A kind of preparation method of low warp glass fiber enhancing nylon Download PDFInfo
- Publication number
- CN110041694A CN110041694A CN201910397583.9A CN201910397583A CN110041694A CN 110041694 A CN110041694 A CN 110041694A CN 201910397583 A CN201910397583 A CN 201910397583A CN 110041694 A CN110041694 A CN 110041694A
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- nylon
- glass fiber
- preparation
- fiber enhancing
- low warp
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J5/00—Manufacture of articles or shaped materials containing macromolecular substances
- C08J5/04—Reinforcing macromolecular compounds with loose or coherent fibrous material
- C08J5/06—Reinforcing macromolecular compounds with loose or coherent fibrous material using pretreated fibrous materials
- C08J5/08—Reinforcing macromolecular compounds with loose or coherent fibrous material using pretreated fibrous materials glass fibres
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2377/00—Characterised by the use of polyamides obtained by reactions forming a carboxylic amide link in the main chain; Derivatives of such polymers
- C08J2377/02—Polyamides derived from omega-amino carboxylic acids or from lactams thereof
-
- 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
-
- 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
Abstract
The present invention relates to a kind of preparation method of low warp glass fiber enhancing nylon, comprising the following steps: cleaning glass fibre, hydrofluoric acid sprayed glass fiber surface, glass and nylon melting extrusion squeeze out that blank is cooling, is granulated.The mode that the present invention is corroded by using hydrofluoric acid spraying, improve the roughness of fiberglass surfacing, to improve the compatibility of glass fibre and nylon, the appearance (without fibre etc. is floated) of component made by material is not only improved, the mechanical property of component is also improved；Simultaneously relative to the mode for impregnating hydrofluoric acid corrosion, since starching amount is less, extent of corrosion can be controlled preferably, and made component has the regularity of better mechanical property and appearance.
Description
Technical field
The present invention relates to glass fiber reinforced nylon material field more particularly to a kind of preparation sides of low warp glass fiber enhancing nylon
Method.
Background technique
Glass fibre (GF), which enhances nylon (PA), has excellent mechanical property, heat resistance and chemical resistance, is widely used in
In the heavy parts shell such as automobile.But to be that moulded products can generate biggish for a distinct disadvantage of PA/GF reinforcing material
, there is the problem of buckling deformation in " floating fibre ", this is because the compatibility of glass and matrix is bad, glass can due to PA cladding not
It is exposed well.
Simultaneously because the section of GF usually used at present is circle, draw ratio is big, so that the degree of orientation of GF in the material
Relatively high, the orientation of glass in the flowing direction limits the contraction of resin；Induction crystallization of the PA around glass to make again
The longitudinal direction (flow direction) of product, which is shunk, to be less than laterally (direction vertical with flow direction), e.g., with the nylon of 30% fiberglass reinforced
Composite material, lateral shrinking percentage are 0.9%, and longitudinal shrinking percentage is 0.4%；This contraction unevenness exacerbates product and warpage occurs
The degree of deformation has seriously affected the appearance and product size of product, limits its answering in the demanding some products of appearance
With.
Certain methods are to be stuck up by the methods of optimization injection technological parameter, change products thickness and improvement cast gate to improve
Song, but there are significant limitations for use of these methods to material.The fiber that some researchers pass through the other small sizes of addition
Warpage issues are solved, although the resistance to warping energy of material can be improved, reinforcing effect is poorer than common glass.
For this purpose, provide it is a kind of can effectively maintain high-strength, Gao Gang, high tenacity, and prepared product surface is without buckling deformation
Glass fibre reinforced nylon, with meet automobile hub cover etc. more both required material have excellent mechanics and
Thermal property, while requiring that apparent mass is excellent, the application demand in the good large-scale product of toughness again, it is that the present invention to be solved
Certainly the problem of.
Summary of the invention
The present invention overcomes the deficiencies in the prior art, providing a kind of can effectively maintain high-strength, Gao Gang, high heat resistance, high-ductility
Property, and glass fibre reinforced nylon of the prepared product surface without buckling deformation.
In order to achieve the above objectives, the technical solution adopted by the present invention are as follows: provide a kind of low warp glass fiber enhancing nylon
Preparation method, it is characterised in that: the following steps are included:
(1) glass fibre is dipped into cleaning solution and is ultrasonically treated；Cleaning, drying later；
(2) hydrofluoric acid solution is sprayed to glass fibre using spraying device, hydrofluoric acid solution is made to be evenly distributed on glass fibers dimension table
Face；It stands later, cleaning, drying；
(3) it after mixing surface treated glass fibre with nylon, is passed through in extruder and melts, squeeze out；
(4) blank squeezed out carries out cooling treatment；
(5) it is granulated, obtains low warp glass fiber enhancing nylon.
As a preferred embodiment, in the step (1), the section of glass fibre is ellipse.
As a kind of more preferable scheme, in the step (1), the density of glass fibre is 2.2-2.66g/cm3。
As a preferred embodiment, in the step (1), 25-35 DEG C at a temperature of be ultrasonically treated 1-3min.
As a preferred embodiment, in the step (2), the concentration of hydrofluoric acid solution is 20-30wt%.
As a kind of more preferable scheme, in the step (2), time of repose 10-20s.
As a preferred embodiment, in the step (3), glass fibre and nylon press 3:7-12(mass ratio) proportion into
Row mixing.
As a kind of more preferable scheme, in the step (3), nylon be in glue nylon 6；Temperature of the nylon 6 at 230 DEG C
Under, the flow rate under 2.16kg load is 1.0-4.0g/10min.
As a preferred embodiment, in the step (3), extruder is double screw extruder；Glass fibre and nylon
Mixture residence time in double screw extruder is 1-2min；Pressure is 15-18MPa.
As a preferred embodiment, it in the step (4), is cooled down using 5-15 DEG C of recirculated water.
The beneficial technical effect of the present invention lies in: provide it is a kind of can effectively maintain high-strength, Gao Gang, high tenacity, and it is made
Glass fibre reinforced nylon of the standby product surface without buckling deformation.
(1) present invention improves the roughness of fiberglass surfacing by using the mode of hydrofluoric acid spraying corrosion, thus
The compatibility for improving glass fibre and nylon not only improves the appearance (without fibre etc. is floated) of component made by material, also mentions
The high mechanical property of component；Simultaneously relative to the mode for impregnating hydrofluoric acid corrosion, since starching amount is less, extent of corrosion can be more
It is controlled well, made component has the regularity of better mechanical property and appearance.
(2) ellipse is in the section for the glass fibre that the present invention uses；The cross section of ellipse is horizontal compared to conventional circle
Section reduces the orientation of glass, reduces the anisotropy of glass, so that it is made to further improve glass fiber reinforced nylon material
At component occur buckling deformation the problem of.
Specific embodiment
The invention will be further described combined with specific embodiments below.Following embodiment is only used for clearly illustrating
Technical solution of the present invention, and not intended to limit the protection scope of the present invention.
Embodiment 1
The present invention provides a kind of preparation methods of low warp glass fiber enhancing nylon, comprising the following steps:
(1) glass fibre is dipped into cleaning solution, is ultrasonically treated 1min at 35 DEG C；Cleaning, drying later；The work of the step
With are as follows: the impurity on cleaning glass surface；
(2) hydrofluoric acid solution is made to be evenly distributed on glass to the hydrofluoric acid solution of glass fibre spraying 20wt% using spraying device
Fiber surface；20s is stood later；Cleaning, drying later；The effect of the step is: being carried out using hydrofluoric acid to its surface
Processing, increases the roughness on its surface, to increase the affinity of glass fibre and nylon base, to improve glass fibre
Conjugation in nylon material；Simultaneously by the way of spraying, not only make the extent of corrosion of fiberglass surfacing more uniform,
The upper hydrofluoric acid amount to glass surface is less simultaneously, convenient for preferably control corrosion rate；
(3) by surface treated glass fibre with nylon by 3:7(mass ratio) proportion mix after, be passed through twin-screw extrusion
It melts, squeezes out in machine；The residence time is 1-2min in double screw extruder；Pressure is 15-18MPa；
(4) blank squeezed out, using 5-15 DEG C of circulating water；
(5) it is granulated, obtains low warp glass fiber enhancing nylon.
Wherein: nylon be in glue nylon 6；Nylon 6 230 DEG C at a temperature of, 2.16kg load under flow rate be
1.0-4.0g/10min。
Glass fibre is the glass fibre that section is ellipse, density 2.2-2.66g/cm3；The cross section of ellipse
Compared to conventional circular cross section, the orientation of glass is reduced, the anisotropy of glass is reduced, so as to improve fiberglass reinforced Buddhist nun
The problem of buckling deformation, occurs for component made by imperial material.
Cleaning solution is using conventional cleaning solution.
Embodiment 2
The present embodiment compared with Example 1, the difference is that:
In step (1): after glass fibre is dipped into cleaning solution, being ultrasonically treated 2min at 31 DEG C；
In step (2): being sprayed using the hydrofluoric acid solution of 25wt%, stand 15s later；
In step (3): surface treated glass fibre and nylon press 2:8(mass ratio).
Embodiment 3
The present embodiment compared with Example 1, the difference is that:
In step (1): after glass fibre is dipped into cleaning solution, being ultrasonically treated 3min at 25 DEG C；
In step (2): being sprayed using the hydrofluoric acid solution of 30wt%, stand 10s later；
In step (3): surface treated glass fibre and nylon press 2.5:7.5(mass ratio).
Comparative example 1
This comparative example compared with Example 1, the difference is that:
In step (2): by the way of 5s in the hydrofluoric acid solution that glass fibre is immersed in 20wt%, other with embodiment 1
It is identical.
Performance test:
PP composite material provided by embodiment 1-3 and comparative example 1 is subjected to injection moulding system on injection (mo(u)lding) machine
Sample, and be tested for the property.
Tensile strength test: reference standard: ISO527-2；Test condition: span 50mm.
Bending strength test: reference standard: ISO178；Test condition: span 64mm, speed 14mm/min.
Bending modulus test: reference standard: ISO178；Test condition: span 64mm, speed 2mm/min.
Impact strength test: reference standard: ISO179-1；Test condition: span 40mm.
Notch impact strength test: reference standard: ISO179-1；Test condition: span 40mm.
2 embodiment 1-3 of table and the test of the Material injection end properties of comparative example 1
| Number | Embodiment 1 | Embodiment 2 | Embodiment 3 | Comparative example 1 |
| Tensile strength/Mpa | 180 | 165 | 170 | 130 |
| Bending strength/Mpa | 240 | 225 | 230 | 200 |
| Bending modulus/Mpa | 7800 | 7500 | 7650 | 7350 |
| Impact strength/KJm-2 | 82 | 78 | 81 | 74 |
| Notch impact strength/KJm-2 | 15 | 13 | 14 | 10 |
| Appearance | Without warpage without floating fibre | Without warpage without floating fibre | Without warpage without floating fibre | There is warpage without floating fibre |
According to testing result it can be found that: component obtained by embodiment 1-3 has preferable mechanical property, and surface is without warpage
With floating fibre, illustrate that the compatibility of glass fibre and nylon is good；The mechanical property of comparative example is relatively poor simultaneously, and appearance has and sticks up
It is bent；This is because impregnate hydrofluoric acid although can also be improved the affinity of glass and nylon, using immersion by the way of, hydrogen fluorine
Starching amount of the acid on glass surface is larger, so etching process is more difficult to control, hydrofluoric acid is more serious to the destruction of glass, instead
Reduce the mechanical property of finished product and the regularity of appearance.
Based on the above description of the preferred embodiments of the present invention, through the above description, related personnel completely can be with
Without departing from the scope of the technological thought of the present invention', various changes and amendments are carried out.The technical scope of this invention
It is not limited to the contents of the specification, it is necessary to determine the technical scope according to the scope of the claims.
Claims (10)
1. a kind of preparation method of low warp glass fiber enhancing nylon, it is characterised in that: the following steps are included:
(1) glass fibre is dipped into cleaning solution and is ultrasonically treated；Cleaning, drying later；
(2) hydrofluoric acid solution is sprayed to glass fibre using spraying device, hydrofluoric acid solution is made to be evenly distributed on glass fibers dimension table
Face；It stands later, cleaning, drying；
(3) it after mixing surface treated glass fibre with nylon, is passed through in extruder and melts, squeeze out；
(4) blank squeezed out carries out cooling treatment；
(5) it is granulated, obtains low warp glass fiber enhancing nylon.
2. the preparation method of low warp glass fiber enhancing nylon according to claim 1, it is characterised in that: the step (1)
In, the section of glass fibre is ellipse.
3. the preparation method of low warp glass fiber enhancing nylon according to claim 2, it is characterised in that: the step (1)
In, the density of glass fibre is 2.2-2.66g/cm3。
4. the preparation method of low warp glass fiber enhancing nylon according to claim 1, it is characterised in that: the step (1)
In, 25-35 DEG C at a temperature of be ultrasonically treated 1-3min.
5. the preparation method of low warp glass fiber enhancing nylon according to claim 1, it is characterised in that: the step (2)
In, the concentration of hydrofluoric acid solution is 20-30wt%.
6. the preparation method of low warp glass fiber enhancing nylon according to claim 5, it is characterised in that: the step (2)
In, time of repose 10-20s.
7. the preparation method of low warp glass fiber enhancing nylon according to claim 1, it is characterised in that: the step (3)
In, glass fibre is with nylon by 3:7-12(mass ratio) proportion mixed.
8. the preparation method of low warp glass fiber enhancing nylon according to claim 7, it is characterised in that: the step (3)
In, nylon be in glue nylon 6；Nylon 6 230 DEG C at a temperature of, the lower flow rate of 2.16kg load is 1.0-4.0g/
10min。
9. the preparation method of low warp glass fiber enhancing nylon according to claim 1, it is characterised in that: the step (3)
In, extruder is double screw extruder；The mixture of glass fibre and nylon residence time in double screw extruder is 1-
2min；Pressure is 15-18MPa.
10. the preparation method of low warp glass fiber enhancing nylon according to claim 1, it is characterised in that: the step (4)
In, it is cooled down using 5-15 DEG C of recirculated water.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201910397583.9A CN110041694A (en) | 2019-05-14 | 2019-05-14 | A kind of preparation method of low warp glass fiber enhancing nylon |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201910397583.9A CN110041694A (en) | 2019-05-14 | 2019-05-14 | A kind of preparation method of low warp glass fiber enhancing nylon |
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| CN110041694A true CN110041694A (en) | 2019-07-23 |
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| CN201910397583.9A Pending CN110041694A (en) | 2019-05-14 | 2019-05-14 | A kind of preparation method of low warp glass fiber enhancing nylon |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111253735A (en) * | 2020-03-30 | 2020-06-09 | 苏州润佳工程塑料股份有限公司 | Low-shrinkage nylon composite material |
| CN115948050A (en) * | 2022-08-12 | 2023-04-11 | 苏州润佳高分子材料有限公司 | Anti-warping glass fiber reinforced nylon material |
Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS58156546A (en) * | 1982-03-11 | 1983-09-17 | Nippon Telegr & Teleph Corp <Ntt> | Production of high-strength optical fiber |
| CN101652430A (en) * | 2007-04-03 | 2010-02-17 | 尤尼蒂卡株式会社 | Glass fiber reinforced polyamide resin composition |
| CN104310803A (en) * | 2014-10-10 | 2015-01-28 | 青岛海信电器股份有限公司 | Glass fiber, surface treatment method of glass fiber, plastic and shell |
| CN106543717A (en) * | 2016-11-05 | 2017-03-29 | 上海耐特复合材料制品有限公司 | A kind of saturating fibre nylon composite materials of high intensity |
| CN108976607A (en) * | 2018-08-11 | 2018-12-11 | 安徽华祺汽车装饰有限公司 | A kind of antistatic automobile interior material preparation method |
-
2019
- 2019-05-14 CN CN201910397583.9A patent/CN110041694A/en active Pending
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS58156546A (en) * | 1982-03-11 | 1983-09-17 | Nippon Telegr & Teleph Corp <Ntt> | Production of high-strength optical fiber |
| CN101652430A (en) * | 2007-04-03 | 2010-02-17 | 尤尼蒂卡株式会社 | Glass fiber reinforced polyamide resin composition |
| CN104310803A (en) * | 2014-10-10 | 2015-01-28 | 青岛海信电器股份有限公司 | Glass fiber, surface treatment method of glass fiber, plastic and shell |
| CN106543717A (en) * | 2016-11-05 | 2017-03-29 | 上海耐特复合材料制品有限公司 | A kind of saturating fibre nylon composite materials of high intensity |
| CN108976607A (en) * | 2018-08-11 | 2018-12-11 | 安徽华祺汽车装饰有限公司 | A kind of antistatic automobile interior material preparation method |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111253735A (en) * | 2020-03-30 | 2020-06-09 | 苏州润佳工程塑料股份有限公司 | Low-shrinkage nylon composite material |
| CN115948050A (en) * | 2022-08-12 | 2023-04-11 | 苏州润佳高分子材料有限公司 | Anti-warping glass fiber reinforced nylon material |
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Application publication date: 20190723 |
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