CN102558753B - 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 a kind of enhancing toughened self-lubricating polyformaldehyde composite material and preparation method thereof.
Background technology
Polyformaldehyde resin (POM) is on a kind of main chain, to contain the linear low-pole superpolymer that is oxidized methylene radical, and unprotected side chain, high-melting-point, high crystalline, have excellent over-all properties, is described as " supersteel " or " match steel ".POM has hardness, rigidity and the intensity of metalloid, within the scope of very wide temperature and humidity, there are good self lubricity and resistance to fatigue, being widely used in the fields such as aviation, machinery, precision instrument, automobile, electronic apparatus, is one of five large general engineering plastic.Although POM has good over-all properties, its high crystalline makes its shock strength bad, and notch sensitivity is large, and molding shrinkage is high, has limited the application of POM in every field.In recent years, along with scientific and technological development, precision instrument, electronic apparatus, various industrial machines etc. are constantly to miniaturization, lightness development, and the condition of power conduction is also more and more harsher, and single POM cannot meet these working conditions.Thermoplastic polyester elastomer (TPEE) is the segmented copolymer that contains the 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, because the solid four needle-like three-dimensional structures of its uniqueness are easy to make it to be uniformly distributed in matrix, can isotropically improve the physicals of material, as performances such as wear-resisting, enhancing, damping, anti-skidding, noise control, suction ripples.
US Patent No. 4804716 discloses reinforced polyformaldehyde mixture and has been comprised of polyoxymethylene and Polyurethane Thermoplastic Elastomer, although its notched Izod impact strength surpasses 375J/m, does not mention tensile strength and the elongation at break of matrix material in patent.Chinese patent CN1546564A discloses character and the preparation method of polyoxymethylene and Blending Modification of Thermoplastic Polyurethane thing, although the elongation at break of said composition and simply supported beam notched Izod impact strength make moderate progress, its tensile strength reduces a lot.
Summary of the invention
In order to overcome existing polyformaldehyde resin in the deficiency existing aspect toughness and high-wearing feature, the object of this invention is to provide a kind of enhancing toughened self-lubricating polyformaldehyde composite material of excellent combination property.
Another object of the present invention is to provide a kind of preparation method of above-mentioned enhancing toughened self-lubricating polyformaldehyde composite material.
Technical scheme of the present invention is as follows:
The invention provides a kind of enhancing toughened self-lubricating polyformaldehyde composite material, this matrix material comprises following component and weight percentage:
POM 45～/0％，
TPEE 10～30％，
Tetrafluoroethylene 4～6%,
Glass fibre 5～15%,
Oxidation inhibitor 0.2～1%,
Formaldehyde absorbent 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 in homopolymerization POM or copolymerization POM.
Hard section of described TPEE consists of aromatic dicarboxylic acid and aliphatics or alicyclic diol, the residue of Ruan Duanwei long-chain fat Zu Anhuo long-chain fat family glycol; Preferably, the hard section of described thermoplastic polyester elastomer is polybutylene terephthalate, and soft section is tetrahydrofuran (THF) polyethers.
Described glass fibre is alkali free glass fibre.
Described oxidation inhibitor is selected from 1,3,5-trimethylammonium-2,4,6-tri-(3,5-di-tert-butyl-4-hydroxyl benzyl) benzene (antioxidant 330), four [methyl-β-(3,5-di-tert-butyl-hydroxy phenyl) propionic ester] pentaerythritol ester (antioxidant 1010), β-(3,5-di-tert-butyl-hydroxy phenyl) mixture of one or more in the positive octadecanol ester of propionic acid (antioxidant 1076), three [2.4-di-tert-butyl-phenyl] phosphorous acid ester (irgasfos 168) or two (the cruel base of 2,4-bis-) pentaerythritol diphosphites (S-9228).
Described formaldehyde absorbent is selected from one or more the mixture in Dyhard RU 100 or 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 molybdenumdisulphide.
Described ZnOw is four needle-likes.
Described coupling agent is selected from one or more the mixture in silane coupling agent γ-aminopropyl triethoxysilane (KH550), γ-glycidyl ether oxygen propyl trimethoxy silicane (KH560), titanate coupling agent sec.-propyl three stearic 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 styrene block copolymer grafted maleic anhydride (SEBS-g-MAH).
The present invention also provides a kind of preparation method of above-mentioned enhancing toughened self-lubricating polyformaldehyde composite material, and the method comprises the following steps:
(1) by 10～30%TPEE dry 2-4h at 100 ℃;
(2) dried TPEE is joined in high-speed mixer, add 45～70%POM, 4～6% tetrafluoroethylene, 5～15% glass fibre, 0.2～1% oxidation inhibitor, 0.5～0.8% formaldehyde absorbent, 0.3～0.5% surface lubricant, 0.1～0.2% coupling agent and 1～2% compatilizer at room temperature to mix 15-20min;
(3) compound of step (2) gained is joined in forcing machine, 1～8% ZnOw is added by the venting hole on twin screw extruder, extruding pelletization, injection moulding.
Each district's temperature of described twin screw extruder 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 after dry 3 hours, is used to injection moulding machine injection moulding at 100 ℃, and barrel temperature is 160～200 ℃, and die temperature is 40～100 ℃.
Compared with the existing technology, tool has the following advantages and beneficial effect in the present invention:
1, the matrix material that prepared by the present invention 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 meet 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 illustrated.
Embodiment 1
(1) by 10%TPEE (hard section is polybutylene terephthalate, and soft section is tetrahydrofuran (THF) polyethers) dry 2-4h at 100 ℃;
(2) dried TPEE is joined in high-speed mixer, add 70% homopolymerization POM, 4% tetrafluoroethylene, 5% glass fibre, 0.6% oxidation inhibitor, 0.8% formaldehyde absorbent, 0.4% surface lubricant, 0.2% coupling agent and 1% compatilizer at room temperature to mix 15-20min;
(3) compound of step (2) gained is joined in forcing machine, 8% ZnOw is added by the venting hole on twin screw extruder, extruding pelletization, injection moulding.
Each district's temperature of forcing machine 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 is dry at 100 ℃ used injection moulding machine injection moulding after 3 hours, and barrel temperature is 160～200 ℃, and die temperature is 40～100 ℃.The concrete consumption of various materials and selection are in Table 1.The test performance of material is in Table 2.
Embodiment 2
(1) by 20%TPEE (hard section is polybutylene terephthalate, and soft section is tetrahydrofuran (THF) polyethers) dry 2-4h at 100 ℃;
(2) dried TPEE is joined in high-speed mixer, add 55% homopolymerization POM, 5% tetrafluoroethylene, 15% glass fibre, 0.6% oxidation inhibitor, 0.6% formaldehyde absorbent, 0.4% surface lubricant, 0.1% coupling agent and 2% compatilizer at room temperature to mix 15-20min;
(3) compound of step (2) gained is joined in forcing machine, 1.3% ZnOw is added by the venting hole on twin screw extruder, extruding pelletization, injection moulding.
Each district's temperature of forcing machine 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 is dry at 100 ℃ used injection moulding machine injection moulding after 3 hours, and barrel temperature is 160～200 ℃, and die temperature is 40～100 ℃.The concrete consumption of various materials and selection are in Table 1.The test performance of material is in Table 2.
Embodiment 3
(1) by 30%TPEE (hard section is polybutylene terephthalate, and soft section is tetrahydrofuran (THF) polyethers) dry 2-4h at 100 ℃;
(2) dried TPEE is joined in high-speed mixer, add 45% homopolymerization POM, 6% tetrafluoroethylene, 10% glass fibre, 0.6% oxidation inhibitor, 0.5% formaldehyde absorbent, 0.4% surface lubricant, 0.2% coupling agent and 2% compatilizer at room temperature to mix 15-20min;
(3) compound of step (2) gained is joined in forcing machine, 5.3% ZnOw is added by the venting hole on twin screw extruder, extruding pelletization, injection moulding.
Each district's temperature of forcing machine 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 is dry at 100 ℃ used injection moulding machine injection moulding after 3 hours, and barrel temperature is 160～200 ℃, and die temperature is 40～100 ℃.The concrete consumption of various materials and selection are in Table 1.The test performance of material is in 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 |
| Irgasfos 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 the tensile strength of pure poly-methyl alcohol is 63MPa, and the tensile strength of matrix material does not reduce; Notch shock is with respect to the 8KJ/m of pure poly-methyl alcohol
2also improve a lot; Particularly frictional coefficient, has reduced much with respect to 0.40 of pure poly-methyl alcohol.
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 apply the invention for ease of those skilled in the art.Person skilled in the art obviously can easily make various modifications to these embodiment, and General Principle described herein is applied in other embodiment and needn't passes through performing creative labour.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 departing 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. a polyformaldehyde composite material, is characterized in that: this matrix material comprises following component and weight percentage,
Hard section of described TPEE consists of aromatic dicarboxylic acid and aliphatics or alicyclic diol, the residue of Ruan Duanwei long-chain fat Zu Anhuo long-chain fat family glycol;
Described ZnOw is four needle-likes.
2. polyformaldehyde composite material according to claim 1, is characterized in that: described POM is selected from a kind of in homopolymerization POM or copolymerization POM; Described glass fibre is 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-tri-(3,5-di-tert-butyl-4-hydroxyl benzyl) benzene, four [methyl-β-(3,5-di-tert-butyl-hydroxy phenyl) propionic ester] pentaerythritol ester, β-(3,5-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 absorbent is selected from one or more the mixture in Dyhard RU 100 or 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 molybdenumdisulphide.
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-aminopropyl triethoxysilane, γ-glycidyl ether oxygen propyl trimethoxy silicane, titanate coupling agent sec.-propyl three stearic 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 styrene block copolymer grafted maleic anhydride.
8. the preparation method of the arbitrary described polyformaldehyde composite material of claim 1 to 7, is characterized in that: the method comprises the following steps,
(1) by 10～30%TPEE dry 2-4h at 100 ℃;
(2) dried TPEE is joined in high-speed mixer, add 45～70%POM, 4～6% tetrafluoroethylene, 5～15% glass fibre, 0.2～1% oxidation inhibitor, 0.5～0.8% formaldehyde absorbent, 0.3～0.5% surface lubricant, 0.1～0.2% coupling agent and 1～2% compatilizer at room temperature to mix 15-20min;
(3) compound of step (2) gained is joined in forcing machine, 1～8% ZnOw is added by the venting hole on twin screw extruder, extruding pelletization, injection moulding.
9. the preparation method of polyformaldehyde composite material according to claim 8, it is characterized in that: each district's temperature of described twin screw extruder 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 after the particle of producing is dried to 3 hours at 100 ℃, use injection moulding machine injection moulding, barrel temperature is 160～200 ℃, and die temperature is 40～100 ℃.
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