CN102558753A - Reinforced toughened self-lubricating polyformaldehyde composite material and preparation method thereof - Google Patents
Reinforced toughened self-lubricating polyformaldehyde composite material and preparation method thereof Download PDFInfo
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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
- B29C48/03—Extrusion moulding, i.e. expressing the moulding material through a die or nozzle which imparts the desired form; Apparatus therefor characterised by the shape of the extruded material at extrusion
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Abstract
The invention discloses a reinforced toughened self-lubricating polyformaldehyde composite material and a preparation method thereof, belonging to the field of polymer materials and molding processing thereof. The polyformaldehyde composite material disclosed by the invention comprises the following components in percent by weight: 45-70 percent of POM (Polyoxymethylene), 10-30 percent of TPEE (Thermoplastic Polyether Ester Elastomer), 4-6 percent of polytetrafluoroethylene, 5-15 percent of glass fiber, 0.2-1 percent of antioxygen, 0.5-0.8 percent of formaldehyde absorbing agent, 0.3-0.5 percent of surface lubricating agent, 1-8 percent of zinc oxide whiskers, 0.1-0.2 percent of coupling agent and 1-2 percent of compatilizer. The polyformaldehyde composite material is prepared by adopting the method comprising the steps of: drying 10-30 percent of TPEE at a temperature of 100 DEG C for 2-4h; adding the dried TPEE in a high-speed mixing machine, adding the 45-70 percent of POM, the 4-6 percent of polytetrafluoroethylene, the 5-15 percent of glass fiber, the 0.2-1 percent of antioxygen, the 0.5-0.8 percent of formaldehyde absorbing agent, the 0.3-0.5 percent of surface lubricating agent, the 0.1-0.2 percent of coupling agent and the 1-2 percent of compatilizer for mixing for 15-20min at a room temperature; and adding a mixture obtained in the last step into an extruder, adding the 1-8 percent of zinc oxide whiskers from an exhaust hole on the dual-screw extruder, extruding and granulating, and injection-molding. The composite material provided by the invention has the advantages of dispersing uniformity, good mechanical property and better abrasion resistance.
Description
Technical field
The invention belongs to macromolecular material and forming process field thereof, be specifically related to toughness reinforcing self-lubricating polyformaldehyde matrix material of a kind of enhancing and preparation method thereof.
Background technology
Polyoxymethylene resin (POM) is the linear low-pole superpolymer that contains the oxidation methylene radical on a kind of main chain, and unprotected side chain, HMP, high crystalline have the excellent comprehensive performance, is described as " supersteel " perhaps " match steel ".POM has hardness, rigidity and the intensity of metalloid; In very wide temperature and humidity scope, good self lubricity and resistance to fatigue are arranged all; Being widely used in fields such as aviation, machinery, precision instrument, automobile, electronic apparatus, is one of five big general engineering plastic.Though POM has excellent comprehensive performances, its high crystalline makes its shock strength bad, and notch sensitivity is big, and molding shrinkage is high, has limited the application of POM in every field.In recent years, along with development of science and technology, precision instrument, electronic apparatus, various industrial machines etc. are constantly to miniaturized, lightness development, and the condition of power conduction is also more and more harsher, and single POM can't satisfy these working conditions.Thermoplastic polyester elastomer (TPEE) is the segmented copolymer that contains hard section of polyester and polyester soft segment, and TPEE has the elasticity of rubber and the intensity of engineering plastics, with the compound toughness that can well improve POM of POM; Four acicular type zinc oxide crystal whisker is easy to make its uniform distribution in matrix because its unique solid four needle-like three-dimensional structures, can isotropically improve the physicals of material, like performances such as wear-resisting, enhancing, damping, anti-skidding, noise control, suction ripples.
U.S. Pat 4804716 discloses the reinforced polyformaldehyde mixture to be made up of polyoxymethylene and TPUE, though its notched Izod impact strength surpasses 375J/m, does not mention the tensile strength and the elongation at break of matrix material in the patent.Chinese patent CN1546564A discloses the character and the preparation method of polyoxymethylene and thermoplastic polyurethane blended modifier, though the elongation at break of said composition and simple beam notched Izod impact strength make moderate progress, its tensile strength reduces a lot.
Summary of the invention
In order to overcome existing polyoxymethylene resin, the purpose of this invention is to provide a kind of toughness reinforcing self-lubricating polyformaldehyde matrix material of enhancing of excellent combination property in the deficiency that exists aspect toughness and the high-wearing feature.
Another object of the present invention provides the preparation method of the toughness reinforcing self-lubricating polyformaldehyde matrix material of a kind of above-mentioned enhancing.
Technical scheme of the present invention is following:
The invention provides the toughness reinforcing self-lubricating polyformaldehyde matrix material of a kind of enhancing, this matrix material comprises following component and weight percentage:
POM 45～/0％，
TPEE 10～30％，
Tetrafluoroethylene 4～6%,
Spun glass 5～15%,
Oxidation inhibitor 0.2～1%,
Formaldehyde absorption agent 0.5～0.8%,
Surface lubricant 0.3～0.5%,
ZnOw 1～8%,
Coupling agent 0.1～0.2%,
Compatilizer 1～2%.
Described POM is selected from a kind of among homopolymerization POM or the copolymerization POM.
Hard section of described TPEE is made up of aromatic dicarboxylic acid and aliphatics or alicyclic diol, and soft section is the residue of long-chain fat family amine or long-chain fat family glycol; Preferably, the hard section of said thermoplastic polyester elastomer is a polybutylene terephthalate, and soft section is the THF polyethers.
Described spun glass is an alkali free glass fibre.
Described oxidation inhibitor is selected from 1; 3; 5-trimethylammonium-2,4,6-three (3; The 5-di-tert-butyl-4-hydroxyl benzyl) benzene (antioxidant 330), four [methyl-β-(3; The 5-di-tert-butyl-hydroxy phenyl) propionic ester] one or more mixture in pentaerythritol ester (antioxidant 1010), β-(3, the 5-di-tert-butyl-hydroxy phenyl) the positive octadecanol esters of propionic acid (antioxidant 1076), three [2.4-di-tert-butyl-phenyl] phosphorous acid esters (oxidation inhibitor 168) or two (2,4-two cruel bases) pentaerythritol diphosphites (S-9228).
Described formaldehyde absorption agent is selected from one or more the mixture in Dyhard RU 100 or the polymeric amide.
Described surface lubricant is selected from one or more the mixture in silicone resin, ethylene bis stearic acid amide (EBS), ethylene-acrylic acid copolymer (A-C540A), graphite or the molybdenumdisulphide.
Described ZnOw is four needle-likes.
Described coupling agent is selected from one or more the mixture in silane coupling agent γ-An Bingjisanyiyangjiguiwan (KH550), γ-glycidyl ether oxygen propyl trimethoxy silicane (KH560), titanate coupling agent sec.-propyl three hard esters acid titanic acid ester (TTS) or (two octyloxy tetra-sodium ester groups) ethylene titanic acid ester (titanate coupling agent 311).
Described compatilizer is selected from one or more the mixture in polypropylene grafted maleic anhydride (PP-G-MAH), ethylene-vinyl acetate copolymer or ethene-butylene and the styrene block copolymer grafted maleic anhydride (SEBS-g-MAH).
The present invention also provides the preparation method of the toughness reinforcing self-lubricating polyformaldehyde matrix material of a kind of above-mentioned enhancing, and this method may further comprise the steps:
(1) with 10～30%TPEE dry 2-4h under 100 ℃;
(2) drying is good TPEE joins in the high-speed mixer, adds 45～70%POM, 4～6% tetrafluoroethylene, 5～15% spun glass, 0.2～1% oxidation inhibitor, 0.5～0.8% formaldehyde absorption agent, 0.3～0.5% surface lubricant, 0.1～0.2% coupling agent and 1～2% compatilizer and at room temperature mixes 15-20min;
(3) compound with step (2) gained joins in the forcing machine, and 1～8% ZnOw is added by the venting hole on the twin screw extruder, extruding pelletization, injection moulding.
Described twin screw extruder is respectively distinguished temperature and is respectively: 140～150 ℃, and 160～170 ℃, 170～185 ℃, 180～195 ℃, 180～195 ℃, 180～195 ℃, 185～195 ℃ of head temperatures, screw speed 200-500 rev/min.
Described injection moulding is that the particle of producing is used the injection moulding machine injection moulding in drying under 100 ℃ after 3 hours, and barrel temperature is 160～200 ℃, and die temperature is 40～100 ℃.
The present invention compares with prior art, has following advantage and beneficial effect:
1, the matrix material of the present invention's preparation is uniformly dispersed, and mechanical property is good, and has good wear resistance, can be used for preparing gear, meter case etc.
2, the present invention has not only improved the mechanical property of matrix material, has also kept good machine-shaping property simultaneously.
3, the present invention can satisfy the performance requriements of power drive and transmission part under high temperature, high pressure, high heat condition.
Embodiment
Below in conjunction with embodiment the present invention is further described.
Embodiment 1
(1) with 10%TPEE (hard section is a polybutylene terephthalate, and soft section is the THF polyethers) dry 2-4h under 100 ℃;
(2) drying is good TPEE joins in the high-speed mixer, adds 70% homopolymerization POM, 4% tetrafluoroethylene, 5% spun glass, 0.6% oxidation inhibitor, 0.8% formaldehyde absorption agent, 0.4% surface lubricant, 0.2% coupling agent and 1% compatilizer and at room temperature mixes 15-20min;
(3) compound with step (2) gained joins in the forcing machine, and 8% ZnOw is added by the venting hole on the twin screw extruder, extruding pelletization, injection moulding.
Forcing machine is respectively distinguished temperature and is respectively: 140 ℃, and 160～170 ℃, 170～185 ℃, 180～195 ℃, 180～195 ℃, 180～195 ℃, 185～195 ℃ of head temperatures, screw speed 200-500 rev/min.The particle of producing was used the injection moulding machine injection moulding after under 100 ℃ dry 3 hours, barrel temperature is 160～200 ℃, and die temperature is 40～100 ℃.Table 1 is seen in the concrete consumption and the selection of various materials.The test performance of material is seen table 2.
Embodiment 2
(1) with 20%TPEE (hard section is a polybutylene terephthalate, and soft section is the THF polyethers) dry 2-4h under 100 ℃;
(2) drying is good TPEE joins in the high-speed mixer, adds 55% homopolymerization POM, 5% tetrafluoroethylene, 15% spun glass, 0.6% oxidation inhibitor, 0.6% formaldehyde absorption agent, 0.4% surface lubricant, 0.1% coupling agent and 2% compatilizer and at room temperature mixes 15-20min;
(3) compound with step (2) gained joins in the forcing machine, and 1.3% ZnOw is added by the venting hole on the twin screw extruder, extruding pelletization, injection moulding.
Forcing machine is respectively distinguished temperature and is respectively: 140～150 ℃, and 160～170 ℃, 170～185 ℃, 180～195 ℃, 180～195 ℃, 180～195 ℃, 185～195 ℃ of head temperatures, screw speed 200-500 rev/min.The particle of producing was used the injection moulding machine injection moulding after under 100 ℃ dry 3 hours, barrel temperature is 160～200 ℃, and die temperature is 40～100 ℃.Table 1 is seen in the concrete consumption and the selection of various materials.The test performance of material is seen table 2.
Embodiment 3
(1) with 30%TPEE (hard section is a polybutylene terephthalate, and soft section is the THF polyethers) dry 2-4h under 100 ℃;
(2) drying is good TPEE joins in the high-speed mixer, adds 45% homopolymerization POM, 6% tetrafluoroethylene, 10% spun glass, 0.6% oxidation inhibitor, 0.5% formaldehyde absorption agent, 0.4% surface lubricant, 0.2% coupling agent and 2% compatilizer and at room temperature mixes 15-20min;
(3) compound with step (2) gained joins in the forcing machine, and 5.3% ZnOw is added by the venting hole on the twin screw extruder, extruding pelletization, injection moulding.
Forcing machine is respectively distinguished temperature and is respectively: 140～150 ℃, and 160～170 ℃, 170～185 ℃, 180～195 ℃, 180～195 ℃, 180～195 ℃, 185～195 ℃ of head temperatures, screw speed 200-500 rev/min.The particle of producing was used the injection moulding machine injection moulding after under 100 ℃ dry 3 hours, barrel temperature is 160～200 ℃, and die temperature is 40～100 ℃.Table 1 is seen in the concrete consumption and the selection of various materials.The test performance of material is seen table 2.
Table 1
| Raw material | Embodiment 1 | Embodiment 2 | Embodiment 3 |
| Homopolymerization POM | 70 | 55 | 45 |
| TPEE | 10 | 20 | 30 |
| Tetrafluoroethylene | 4 | 5 | 6 |
| Alkali free glass fibre | 5 | 15 | 10 |
| Antioxidant 1010 | 0.2 | 0.2 | 0.2 |
| Oxidation inhibitor 168 | 0.4 | 0.4 | 0.4 |
| Dyhard RU 100 | 0.8 | 0.6 | 0.5 |
| Silicone resin GM-100 | 0.4 | 0.4 | 0.4 |
| Four acicular type zinc oxide crystal whisker | 8 | 1.3 | 5.3 |
| Titanic acid ester TTS | 0.2 | 0.1 | 0.2 |
| SEBS-g-MAH | 1 | 2 | 2 |
Table 2 has been listed the partial properties of the matrix material that above-mentioned three embodiment obtain, and pure tensile strength of gathering methyl alcohol is 63MPa, and the tensile strength of matrix material does not reduce; Notch shock is with respect to the pure 8KJ/m that gathers methyl alcohol
2Also improve a lot; Particularly frictional coefficient has reduced much with respect to pure 0.40 of the methyl alcohol that gathers.
Table 2
| Unit and testing standard | Embodiment 1 | Embodiment 2 | Embodiment 3 | |
| Tensile strength | MPa(ISO527) | 60 | 63 | 65 |
| Elongation at break | ％(ISO527) | 40 | 70 | 100 |
| Notched Izod impact strength | 2 KJ/m 2(ISO179/1eA) | 13 | 15 | 19 |
| Frictional coefficient | 0.120 | 0.125 | 0.130 |
The above-mentioned description to embodiment is can understand and use the present invention for ease of the those of ordinary skill of this technical field.The personnel of skilled obviously can easily make various modifications to these embodiment, and needn't pass through performing creative labour being applied in the General Principle of this explanation among other embodiment.Therefore, the invention is not restricted to the embodiment here, those skilled in the art are according to announcement of the present invention, and not breaking away from the improvement that category of the present invention makes and revise all should be within protection scope of the present invention.
Claims (10)
1. polyformaldehyde composite material, it is characterized in that: this matrix material comprises following component and weight percentage,
POM 45～70％，
TPEE 10～30％，
Tetrafluoroethylene 4～6%,
Spun glass 5～15%,
Oxidation inhibitor 0.2～1%,
Formaldehyde absorption agent 0.5～0.8%,
Surface lubricant 0.3～0.5%,
ZnOw 1～8%,
Coupling agent 0.1～0.2%,
Compatilizer 1～2%.
2. polyformaldehyde composite material according to claim 1 is characterized in that: described POM is selected from a kind of among homopolymerization POM or the copolymerization POM; Hard section of described TPEE is made up of aromatic dicarboxylic acid and aliphatics or alicyclic diol, and soft section is the residue of long-chain fat family amine or long-chain fat family glycol; Described spun glass is an alkali free glass fibre.
3. polyformaldehyde composite material according to claim 1; It is characterized in that: described oxidation inhibitor is selected from 1,3,5-trimethylammonium-2; 4; 6-three (3, the 5-di-tert-butyl-4-hydroxyl benzyl) benzene, four [methyl-β-(3, the 5-di-tert-butyl-hydroxy phenyl) propionic ester] pentaerythritol ester, β-(3; The 5-di-tert-butyl-hydroxy phenyl) mixture of one or more in the positive octadecanol ester of propionic acid, three [2.4-di-tert-butyl-phenyl] phosphorous acid esters or two (2,4-two cruel bases) pentaerythritol diphosphites.
4. polyformaldehyde composite material according to claim 1 is characterized in that: described formaldehyde absorption agent is selected from one or more the mixture in Dyhard RU 100 or the polymeric amide.
5. polyformaldehyde composite material according to claim 1 is characterized in that: described surface lubricant is selected from one or more the mixture in silicone resin, ethylene bis stearic acid amide, ethylene-acrylic acid copolymer, graphite or the molybdenumdisulphide; Described ZnOw is four needle-likes.
6. polyformaldehyde composite material according to claim 1 is characterized in that: described coupling agent is selected from one or more the mixture in silane coupling agent γ-An Bingjisanyiyangjiguiwan, γ-glycidyl ether oxygen propyl trimethoxy silicane, titanate coupling agent sec.-propyl three hard esters acid titanic acid ester or (two octyloxy tetra-sodium ester groups) ethylene titanic acid ester.
7. polyformaldehyde composite material according to claim 1 is characterized in that: described compatilizer is selected from one or more the mixture in polypropylene grafted maleic anhydride, ethylene-vinyl acetate copolymer or ethene-butylene and the styrene block copolymer grafted maleic anhydride.
8. the preparation method of the arbitrary described polyformaldehyde composite material of claim 1 to 7, it is characterized in that: this method may further comprise the steps,
(1) with 10～30%TPEE dry 2-4h under 100 ℃;
(2) drying is good TPEE joins in the high-speed mixer, adds 45～70%POM, 4～6% tetrafluoroethylene, 5～15% spun glass, 0.2～1% oxidation inhibitor, 0.5～0.8% formaldehyde absorption agent, 0.3～0.5% surface lubricant, 0.1～0.2% coupling agent and 1～2% compatilizer and at room temperature mixes 15-20min;
(3) compound with step (2) gained joins in the forcing machine, and 1～8% ZnOw is added by the venting hole on the twin screw extruder, extruding pelletization, injection moulding.
9. the preparation method of polyformaldehyde composite material according to claim 8, it is characterized in that: described twin screw extruder is respectively distinguished temperature and is respectively: 140～150 ℃, 160～170 ℃; 170～185 ℃; 180～195 ℃, 180～195 ℃, 180～195 ℃; 185～195 ℃ of head temperatures, screw speed 200-500 rev/min.
10. the preparation method of polyformaldehyde composite material according to claim 8; It is characterized in that: described injection moulding is to descend drying after 3 hours at 100 ℃ on the particle of producing; Use the injection moulding machine injection moulding, barrel temperature is 160～200 ℃, and die temperature is 40～100 ℃.
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