CN101914289A - Glassfiber-reinforced hydrolysis-resistant low-warpage nylon 66 composite material and preparation method thereof - Google Patents
Glassfiber-reinforced hydrolysis-resistant low-warpage nylon 66 composite material and preparation method thereof Download PDFInfo
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- CN101914289A CN101914289A CN2010102679837A CN201010267983A CN101914289A CN 101914289 A CN101914289 A CN 101914289A CN 2010102679837 A CN2010102679837 A CN 2010102679837A CN 201010267983 A CN201010267983 A CN 201010267983A CN 101914289 A CN101914289 A CN 101914289A
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
- B29C—SHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
- B29C48/00—Extrusion moulding, i.e. expressing the moulding material through a die or nozzle which imparts the desired form; Apparatus therefor
- B29C48/25—Component parts, details or accessories; Auxiliary operations
- B29C48/92—Measuring, controlling or regulating
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
- B29C—SHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
- B29C2948/00—Indexing scheme relating to extrusion moulding
- B29C2948/92—Measuring, controlling or regulating
- B29C2948/92504—Controlled parameter
- B29C2948/9258—Velocity
- B29C2948/9259—Angular velocity
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
- B29C—SHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
- B29C2948/00—Indexing scheme relating to extrusion moulding
- B29C2948/92—Measuring, controlling or regulating
- B29C2948/92504—Controlled parameter
- B29C2948/92704—Temperature
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
- B29C—SHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
- B29C2948/00—Indexing scheme relating to extrusion moulding
- B29C2948/92—Measuring, controlling or regulating
- B29C2948/92819—Location or phase of control
- B29C2948/92857—Extrusion unit
- B29C2948/92876—Feeding, melting, plasticising or pumping zones, e.g. the melt itself
- B29C2948/92885—Screw or gear
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
- B29C—SHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
- B29C2948/00—Indexing scheme relating to extrusion moulding
- B29C2948/92—Measuring, controlling or regulating
- B29C2948/92819—Location or phase of control
- B29C2948/92857—Extrusion unit
- B29C2948/92876—Feeding, melting, plasticising or pumping zones, e.g. the melt itself
- B29C2948/92895—Barrel or housing
Abstract
The invention provides a glassfiber-reinforced hydrolysis-resistant low-warpage nylon 66 composite material and a preparation method thereof. The glassfiber-reinforced hydrolysis-resistant low-warpage nylon 66 composite material comprises the following components in parts by weight: 50-85 parts of nylon 66, 10-40 parts of glassfibers, 2-10 parts of warpage deformation improvers, 0.5-2 parts of hydrolytic and heat stabilizers, 1-4 parts of compatilizers and 1-2 parts of other auxiliary agents, wherein the auxiliary agents are one or a mixture of more of a siloxane coupling agent and an antioxidant or a parting agent. The product has high strength and rigidity, also well solves the problems of easy warpage deformation and great dimension change of the product due to glassfiber addition, has both excellent hydrolytic resistance and temperature tolerance and also has good processability and attractive appearance.
Description
Technical field
The invention belongs to the modified polyamide technical field, relate to a kind of Glassfiber-reinforced hydrolysis-resistant low-warpage nylon dragon 66 matrix materials and preparation method thereof.This matrix material is mainly used in automobile hydroecium in the industries such as automobile, machinery, electrical equipment, engine parts, bearing, gear etc., use having for a long time under higher levels of humidity and the hot environment, contact water, alcohol, fat, organic solvent, and molded article is had the component of high request to buckling deformation and dimensional stability.
Background technology
Nylon 66 is a kind of broad-spectrum engineering plastics, is formed by hexanediamine, hexanodioic acid polycondensation, and its fusing point is 252-265 ℃, compares with the Other Engineering plastics to have excellent mechanical property and thermal characteristics preferably, as high strength, high-modulus, high rigidity; Higher relatively heat-drawn wire, after the adding glass fibre strengthened, heat-drawn wire can reach 250 ℃ (0.45MPa); Show excellent self-lubricating abrasion-resistant, antifatigue, creep resistant in addition; Good oil resistant and solvent borne.But because the wetting ability of amide group, the water-absorbent height of nylon 66 causes its dimensional stability relatively poor, and degradation is obvious under high humidity environment.Can significantly improve its over-all properties by the filling way, improve deficiency, become very common nylon 66 method of modifying so glass fibre is filled.
Continuous development along with industries such as automobile, machinery, electrical equipment, use to material also constantly proposes new requirement, lightweight, high-performance, environmental protection become new trend, and a large amount of metallic substance are replaced by engineering plastics, and nylon 66 is accounting for very consequence as representative wherein.
General glass fibre reinforced modified nylon 66 is that a lot of producers use production as a very classical mode, sales volume is very big on the market of present stage, also there is some difference on performance and stability for the product of different manufacturers, require loading level also to have respectively according to difference, external producer such as Dupont, BASF, Rhodia etc., be divided into different grades according to different demands, as high rigidity, uvioresistant, wear-resisting, super tough or the like.
But also not based on the glass enhancing, have anti-hydrolysis heatproof function concurrently, the special product that has also possessed low buckling deformation that common Reinforced Nylon was short of, characteristics that dimensional stability is good, the present invention in order to fill up this blank, satisfies the requirement of specific product just.
Summary of the invention
The present invention relates to a kind of Glassfiber-reinforced hydrolysis-resistant low-warpage nylon dragon 66 matrix materials and preparation method thereof, on glass fibre enhanced basis, have anti-hydrolysis temperature tolerance concurrently, it is good also to have possessed low buckling deformation, dimensional stability that common Reinforced Nylon was short of especially, both kept the due very good mechanical properties of material, and satisfied the service requirements of product, kept good dimensional stability and apparent at special dimension.
Be to realize that above-mentioned requirements, the present invention introduced nylon 66, glass fibre, anti-hydrolysis and thermo-stabilizer, buckling deformation activator, compatilizer and other auxiliary agents etc. of low viscosity, high workability.Low viscosity wherein, high workability nylon 66 base-materials have guaranteed the flowability and the processed-type of material monolithic, anti-hydrolysis alkali free glass fibre is except providing certain anti-hydrolysis function, its diameter is thinner, work in-process disperses more even, the better properties performance can be arranged, an amount of buckling deformation activator in the mechanical property that keeps the material excellence simultaneously, improved the shortcoming of the serious and poor dimensional stability of traditional glass fiber enhanced nylon 66 material buckling deformation greatly, anti-hydrolysis and thermo-stabilizer provide unexistent long-term resistance to hydrolysis of general material and long-term temperature tolerance for material, compatilizer effectively raises the associativity between nylon 66 base-materials and each other component, guarantee the toughness of material, other auxiliary agents are to the processibility of material, release property, oxidation-resistance and good apparent the providing safeguard of product.Each component also can exert an influence to other performances in the performance in a certain respect at strongthener, so the usage quantity of each component and different classes of each other cooperation, synergistic just become another core content among the present invention.
The weight proportion of this Glassfiber-reinforced hydrolysis-resistant low-warpage nylon dragon 66 matrix materials is as follows:
Nylon 66 50-85 weight parts
Glass fibre 10-40 weight part
Buckling deformation activator 2-10 weight part
Anti-hydrolysis and thermo-stabilizer 0.5-2 weight part
Compatilizer 1-4 weight part
Other auxiliary agents 1-2 weight part,
Described other auxiliary agents are one or more mixing in siloxanes coupling agent, oxidation inhibitor or the releasing agent.
Above-mentioned matrix material preferably is made up of the raw material of following weight part:
Nylon 66 55-65 weight parts
Glass fibre 20-30 weight part
Buckling deformation activator 2-5 weight part
Anti-hydrolysis and thermo-stabilizer 0.5-2 weight part
Compatilizer 1-4 weight part
Other auxiliary agents 1-2 weight part,
Described other auxiliary agents are one or more mixing in siloxanes coupling agent, oxidation inhibitor or the releasing agent.
Described oxidation inhibitor is Hinered phenols and phosphorous acid esters are compound, releasing agent is soap (preferred stearate, as calcium stearate, stearic amide), a kind of in organosilicon or the wax.
Described Nylon 66 intrinsic viscosity is: 2.3-3.2; Glass fibre is the anti-hydrolysis glass fibre of alkali-free, and the glass diameter is 9-13 μ m; The buckling deformation activator is one or more mixing in ultra-fine hollow, solid glass micro-bead, the ceramic fine bead; Anti-hydrolysis and thermo-stabilizer belong to the oxidation inhibitor of copper compound class and the mixture or the polycarbodiimide of synergistic agent, for example: auxiliary agent H3337, Stabaxol-P; Compatilizer is a maleic anhydride grafts, and the grafts base material can be among ethylene-octene copolymer, terpolymer EP rubber, PE and the SEBS one or more, and percentage of grafting is controlled at 0.8-1.0%.
The preparation method of Glassfiber-reinforced hydrolysis-resistant low-warpage nylon dragon 66 matrix materials the steps include:
Step 1: require to take by weighing raw material according to weight;
Step 2: nylon 66, buckling deformation activator, anti-hydrolysis and thermo-stabilizer, compatilizer and other auxiliary agents is even in high-speed mixer and mixing, mixing time 3-5min;
Step 3: mixed raw materials is added in the twin screw extruder, at temperature: 245-285 ℃, screw speed: with the glass fibre melt blending, extruding pelletization promptly obtains Glassfiber-reinforced hydrolysis-resistant low-warpage nylon dragon 66 matrix materials of the present invention under the 300-500rpm.
Beneficial effect of the present invention compared with the prior art:
When product of the present invention has high strength, high rigidity, well improved, had excellent long-term anti-hydrolysis temperature tolerance concurrently, and good processibility and outward appearance performance are arranged owing to add the easy buckling deformation of product behind the glass, problem that dimensional change is big.Be mainly used in automobile hydroecium in the industries such as automobile, machinery, electrical equipment, engine parts, bearing, gear etc. the product of particular requirement is arranged, use having for a long time under higher levels of humidity and the hot environment, contact water, alcohol, fat, organic solvent etc., and molded article is had the component of high request to buckling deformation and dimensional stability.
Description of drawings
Fig. 1 is an automobile hydroecium synoptic diagram.
Embodiment
By the following examples the present invention is further specified:
Below in conjunction with specific embodiment a kind of Glassfiber-reinforced hydrolysis-resistant low-warpage nylon dragon of the present invention 66 matrix materials are described in further details.
Produce the main equipment that uses: high mixer: with material uniform mixing 3-5min; Twin screw extruder: barrel zone temperature: 245-285 ℃, screw speed: 300-500rpm; Tank, dicing machine.
Embodiment 1
The resin intrinsic viscosity of nylon 66 is: 2.3-3.2,65 weight parts;
The anti-hydrolysis glass fibre of alkali-free, glass diameter are 9-13 μ m, 30 weight parts;
Hollow ceramic microspheres: 1100 orders, 2 weight parts;
Anti-hydrolysis and thermo-stabilizer: Stabaxol-P (polycarbodiimide, German Bayer company produces), 0.5 weight part;
Compatilizer: the MAH of percentage of grafting 0.8% (maleic anhydride) grafting EPDM (terpolymer EP rubber), 1 weight part;
Other auxiliary agents: oxygen alkane coupling agent: KH560, oxidation inhibitor: 1098 and 168 is composite, releasing agent: calcium stearate, according to (1: 1: 1 weight ratio) totally 1.5 weight parts.
The resin intrinsic viscosity of nylon 66 is: 2.3-3.2,60.5 weight parts;
The anti-hydrolysis glass fibre of alkali-free, glass diameter are 9-13 μ m, 30 weight parts;
Solid glass micro-bead: 1600 orders, 2 weight parts;
Anti-hydrolysis and thermo-stabilizer: Stabaxol-P, 2 weight parts;
Compatilizer: 1%MAH grafting POE, 4 weight parts
Other auxiliary agents: oxygen alkane coupling agent: KH560, oxidation inhibitor: 1098 and 168 is composite, releasing agent: calcium stearate, according to (1: 1: 1 weight ratio) totally 1.5 weight parts.
The resin intrinsic viscosity of nylon 66 is: 2.3-3.2,62.5 weight parts;
The anti-hydrolysis glass fibre of alkali-free, glass diameter are 9-13 μ m, 30 weight parts;
Ultra-fine hollow glass micropearl: 〉=3000 orders, 3 weight parts;
Anti-hydrolysis and thermo-stabilizer: Stabaxol-P, 1 weight part;
Compatilizer: 1%MAH grafting POE, 2 weight parts
Other auxiliary agents: oxygen alkane coupling agent: KH560, oxidation inhibitor: 1098 and 168 is composite, releasing agent: wax,
According to (1: 1: 1 weight ratio) totally 1.5 weight parts.
The resin intrinsic viscosity of nylon 66 is: 2.3-3.2,64.5 weight parts;
The anti-hydrolysis glass fibre of alkali-free, glass diameter are 9-13 μ m, 30 weight parts;
Hollow ceramic microspheres: 1100 orders, 2 weight parts;
Anti-hydrolysis and thermo-stabilizer: H3337 (nylon hydrolysis-resisting agent, German Bruggemann H series), 0.5 weight part;
Compatilizer: 0.8%MAH grafting EPDM, 1.5 weight parts;
Other auxiliary agents: oxygen alkane coupling agent: KH560, oxidation inhibitor: 1098 and 168 is composite, releasing agent: calcium stearate;
According to (1: 1: 1 weight ratio) totally 1.5 weight parts.
Embodiment 5
The resin intrinsic viscosity of nylon 66 is: 2.3-3.2,60.5 weight parts;
The anti-hydrolysis glass fibre of alkali-free, glass diameter are 9-13 μ m, 30 weight parts;
Solid glass micro-bead: 1600 orders, 2 weight parts;
Anti-hydrolysis and thermo-stabilizer: H3337,2 weight parts;
Compatilizer: 1%MAH grafting POE, 4 weight parts
Other auxiliary agents: oxygen alkane coupling agent: KH560, oxidation inhibitor: 1098 and 168 is composite, releasing agent: calcium stearate; Totally 1.8 weight parts, (oxygen alkane coupling agent, oxidation inhibitor, releasing agent according to 1: 1: 1 weight ratio).
Embodiment 6
The resin intrinsic viscosity of nylon 66 is: 2.3-3.2,62.5 weight parts;
The anti-hydrolysis glass fibre of alkali-free, glass diameter are 9-13 μ m, 30 weight parts;
Ultra-fine hollow glass micropearl: 〉=3000 orders, 3 weight parts;
Anti-hydrolysis and thermo-stabilizer: H3337,1 weight part;
Compatilizer: 1%MAH grafting POE, 1.5 weight parts;
Other auxiliary agents: oxygen alkane coupling agent: KH560, oxidation inhibitor: 1098 and 168 is composite, releasing agent: organo-silicic oil is according to (1: 1: 1 weight ratio) totally 1.5 weight parts.
The method that the prescription of employing the foregoing description is specifically produced matrix material is:
Step 1: require to take by weighing raw material according to weight;
Step 2: nylon 66, buckling deformation activator, anti-hydrolysis and thermo-stabilizer, compatilizer and other auxiliary agents is even in high-speed mixer and mixing, mixing time 3-5min;
Step 3: mixed raw materials is added in the twin screw extruder, at temperature: 245-285 ℃, screw speed: under the 300-500rpm with the glass fibre melt blending, extruding pelletization, promptly.
The product performance test result that the foregoing description prepares is as shown in the table:
In the table, resistance to hydrolysis can testing method: behind the boiling 100h, test flexural strength conservation rate use anti-hydrolysis glass, and after adding hydrolysis-resisting agent, the flexural strength conservation rate is the highest to rise to 69.5% in the boiling water that batten is placed on.
Heat aging performance testing method: batten is placed in the ventilated drying oven, under 120 ℃, behind the 1000h, test tensile strength and notched Izod impact strength conservation rate, after adding thermo-stabilizer, the heat aging performance stretching strength retentivity of material is the highest to rise to 87.4%, and the notched Izod impact strength conservation rate is the highest to rise to 83.3%.
Embodiment 1-6 has provided the difference of performance under each different ratios, adjustment by each component ratio in the prescription, optimized of enhancement and the influence of each component to each performance of product, when making material keep good original mechanical property, in the middle of the test of anti-hydrolysis thermal ageing and low warpage, also shown excellent result.
The present invention feeds back product processing characteristics and apparent better in products such as automobile hydroecium and gear are produced, product shrinks homogeneity and improves a lot, integral smoothness is good, the tangible buckling deformation phenomenon of other same type of material do not occur, product percent of pass rises, and the post-treatment cost significantly reduces.
The dimensional stability test comparison:
Hydroecium design long (l) and wide (b) is: 635mm * 45mm, long (l) dimensional requirement: (635 ± 2) mm; Wide (b) dimensional requirement: (45 ± 0.25) mm.
With 30% glass filled nylon 66 is example:
Glassfiber-reinforced hydrolysis-resistant low-warpage nylon dragon 66 matrix materials of A for preparing according to the embodiment of the invention 6 methods,
B is common glass fiber enhanced nylon 66.
Size measuring wide (b), getting 1,2,3,4 four points of automobile hydroecium respectively is contrast points.Size such as table 3:
Two kinds of material water chamber size contrasts of table 3
Annotate: above data be between measuring result behind the injection moulding dimensional stabilizing, considered the material contracts rate during die design.
As can be seen from Table 3, width dimensions (b) aspect, the size deviation scope of A :-0.24%～0.22%, maximum deflection difference value is 0.24%, the maximum difference of b is 0.46%; The size deviation scope of B :-0.71%～0.36%, maximum deflection difference value is 0.71%, the maximum difference of b is 1.07%.Wherein point 2 positions of B have exceeded product dimensional requirement value.
Length dimension (l) aspect, the size deviation value of A is-0.11%; The size deviation value of B is-0.29%, near the lower limit of variation.Obvious flexural deformation takes place at length direction in B, needs anchor clamps to fix to guarantee the grazing and the planeness of length direction after the injection moulding, and A does not then have this phenomenon, and no buckling deformation that product is straight need not with fixing behind the anchor clamps again, and surface-brightening does not have floating fine.
Claims (10)
1. Glassfiber-reinforced hydrolysis-resistant low-warpage nylon dragon 66 matrix materials is characterized in that this matrix material is made up of the raw material of following weight part:
Nylon 66 50-85 weight parts
Glass fibre 10-40 weight part
Buckling deformation activator 2-10 weight part
Anti-hydrolysis and thermo-stabilizer 0.5-2 weight part
Compatilizer 1-4 weight part
Other auxiliary agents 1-2 weight part
Described other auxiliary agents are one or more mixing in siloxanes coupling agent, oxidation inhibitor or the releasing agent.
2. Glassfiber-reinforced hydrolysis-resistant low-warpage nylon according to claim 1 dragon 66 matrix materials is characterized in that this matrix material is made up of the raw material of following weight part:
Nylon 66 55-65 weight parts
Glass fibre 20-30 weight part
Buckling deformation activator 2-5 weight part
Anti-hydrolysis and thermo-stabilizer 0.5-2 weight part
Compatilizer 1-4 weight part
Other auxiliary agents 1-2 weight part,
Described other auxiliary agents are one or more mixing in siloxanes coupling agent, oxidation inhibitor or the releasing agent.
3. Glassfiber-reinforced hydrolysis-resistant low-warpage nylon dragon 66 matrix materials according to claim 1 is characterized in that the resin intrinsic viscosity of described nylon 66 is: 2.3-3.2.
4. Glassfiber-reinforced hydrolysis-resistant low-warpage nylon dragon 66 matrix materials according to claim 1 is characterized in that described glass fibre is the anti-hydrolysis glass fibre of alkali-free, and the glass diameter is 9-13 μ m.
5. Glassfiber-reinforced hydrolysis-resistant low-warpage nylon according to claim 1 dragon 66 matrix materials is characterized in that described buckling deformation activator is one or more mixing in ultra-fine hollow, solid glass micro-bead or the ceramic fine bead.
6. Glassfiber-reinforced hydrolysis-resistant low-warpage nylon dragon 66 matrix materials according to claim 1 is characterized in that described anti-hydrolysis and thermo-stabilizer are the oxidation inhibitor of copper compound class and the mixture or the polycarbodiimide of synergistic agent.
7. Glassfiber-reinforced hydrolysis-resistant low-warpage nylon dragon 66 matrix materials according to claim 1, it is characterized in that described compatilizer is a maleic anhydride grafts, the grafts base material is one or more among ethylene-octene copolymer, terpolymer EP rubber, PE and the SEBS, and percentage of grafting is controlled at 0.8-1.0%.
8. Glassfiber-reinforced hydrolysis-resistant low-warpage nylon dragon 66 matrix materials according to claim 1 is characterized in that described oxidation inhibitor is that Hinered phenols and phosphorous acid esters are compound.
9. Glassfiber-reinforced hydrolysis-resistant low-warpage nylon according to claim 1 dragon 66 matrix materials is characterized in that described releasing agent is a kind of in soap, organosilicon or the wax.
10. the preparation method of claim 1 or 2 described Glassfiber-reinforced hydrolysis-resistant low-warpage nylon dragon 66 matrix materials the steps include:
Step 1: require to take by weighing raw material according to weight;
Step 2: nylon 66, buckling deformation activator, anti-hydrolysis and thermo-stabilizer, compatilizer and other auxiliary agents is even in high-speed mixer and mixing, mixing time 3-5min;
Step 3: mixed raw materials is added in the twin screw extruder, at temperature: 245-285 ℃, screw speed: under the 300-500rpm with the glass fibre melt blending, extruding pelletization, promptly.
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| CN102558847A (en) * | 2010-12-29 | 2012-07-11 | 合肥杰事杰新材料股份有限公司 | Hydrolysis resistant continuous carbon fiber reinforced nylon 6 material and preparation method thereof |
| CN102585495A (en) * | 2012-01-06 | 2012-07-18 | 聚威工程塑料(上海)有限公司 | Hydrolysis-resistant glass fiber reinforced polyamide 66 (PA66) composite material and preparation method thereof |
| CN102660119A (en) * | 2012-04-11 | 2012-09-12 | 常熟华林塑料有限公司 | High-performance nylon composite material and preparation method thereof |
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| CN103289391A (en) * | 2013-06-21 | 2013-09-11 | 苏州新区佳合塑胶有限公司 | Hydrolysis resistance PA 66 composition |
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Application publication date: 20101215 |