CN101638493A - Long glass fiber reinforced recycled polypropylene material and preparation method thereof - Google Patents
Long glass fiber reinforced recycled polypropylene material and preparation method thereof Download PDFInfo
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Abstract
The invention discloses long glass fiber reinforced recycled polypropylene material and a preparation method thereof. The long glass fiber reinforced recycled polypropylene material comprises components according to mass percent: 25-55% of polypropylene, 30-60% of long glass fiber, 0.4-0.8% of coupling agent, 3-8% of graft of thermoplastic elastomer, 0.1-0.3% of fused finger modifier, 0.2-0.4% ofantioxygens, 1-4% of lubricant and 1-3% of selective assistant. The preparation method is as follows: mixing and stirring components except for long glass fiber, and then adding the components exceptfor long glass fiber to a screw extruder; adding long glass fiber, mixing, extruding, cooling, air drying and pelleting; as the fused finger modifier is added, the requirements on polypropylene are reduced; various recycled polypropylene materials can be used as backing material. The preparation method is simple and has low cost; the prepared long glass fiber einforced recycled polypropylene material has good comprehensive performances and can replace a plurality of metal parts to be applied to various fields.
Description
Technical field
The present invention relates to the enhancing modified technology of thermoplastics, specifically a kind of long glass fiber reinforced recycled polypropylene material and preparation method thereof.
Background technology
Reclaim the polyacrylic at present main branch Physical Processing of technology and two aspects of chemical process of utilizing.Utilize technical mainly containing in chemical process: polyacrylic chlorination, reclaim the Crosslinking of Polypropylene modification, methods such as polyacrylic catalytic pyrolysis and thermo-cracking.Because chemical recovery utilizes technology to have the restriction of a lot of technology and equipments, generally uses less.Using many is the Physical Processing utilization, at present enhancing modified more commonly.The method of traditional enhancing modified generally is by adding powder such as lime carbonate, talcum powder and adding staple fibre and realize.The method of the enhancing modified that these are commonly used all can not satisfy the demand of its high physicals, and its Application Areas is very limited.
And the technological breakthrough of preparation long glass fiber reinforced polypropylene material has solved the technological difficulties of these enhancing modified methods in the past.Can finally make long glass fibres reinforced thermoplastics(RTP) (LFRTP) by this technology.Characteristics such as this material has not only that intensity height, rigidity height, dimensional stability are good, low warpage, long service life, creep resistance are good, and has a good moulding processability, multiple forming method processing such as it can adopt injection, extrude, compacting, lamination, shaping cycle is short, therefore the production efficiency height is widely used in electric, electrician's component, machinery and a plurality of industries such as parts, instrument, aerospace, military use product, building and ornament materials, transport pipe and automobile making.
The principal element that influences the long glass fiber reinforced recycled polypropylene material physicals has three kinds: 1, polypropylene is a non-polar molecule, and is relatively poor with the interfacial adhesion of glass fibre, and improving its interfacial adhesion will have a significant impact its performance; 2, the content of glass fibre and length; 3, polyacrylic melting index in order to increase the dipping effect of glass fibre, adopts the high molten polypropylene that refers to usually.
All there are some shortcomings in the patent of present disclosed long glass fiber reinforced polypropylene, for example in the publication number CN 101338051A patent, need long glass fibres is carried out preheating and drying, make its surface temperature reach 60～80 ℃, then long glass fibres is introduced surface processing device at the liquid coupling agent of its surface infiltration, this kind method need increase support equipment, complex process, material cost is increased, and base resin is had certain selectivity, the molten polypropylene that refers in requiring to use.And for example publication number is in the CN 1810870A patent, in the material formula of preparation long glass fiber-reinforced polypropylene, unsaturated carboxylic acid or its acid anhydrides have directly been used, this class material can constitute very big harm to HUMAN HEALTH usually, can cause pharyngitis, laryngitis and bronchitis after the suction, eyes and skin to the people have the strong impulse effect, and meeting high heat has the incendiary of causing danger, constitutes very big hidden danger for operator and safety operation; And do not use coupling agent in this prescription, also not obvious to the effect of improving polypropylene and glass fibre interfacial adhesion.Use the compound mixed yarn of polypropylene fibre and glass fibre to prepare continuous long glass fiber-reinforced polypropylene materials for another example among the patent CN1962732A, this method is had relatively high expectations to material choice, is not suitable for adopting granular or the powdered polypropylene prepares long glass fiber-reinforced polypropylene materials.
Summary of the invention
The problem that the present invention need solve is to provide the long glass fiber reinforced recycled polypropylene material of the low and excellent property of a kind of cost, and further discloses this preparation methods.
The technical scheme that the present invention takes is: long glass fiber reinforced recycled polypropylene material, its component cubage by mass percentage comprises: polipropene 25～55%, long glass fibres 30～60%, coupling agent 0.4～0.8%, the grafts 3～8% of thermoplastic elastomer, molten properties-correcting agent 0.1～0.3%, oxidation inhibitor 0.2～0.4%, the lubricant 1～4% of referring to.
The composition component of long glass fiber reinforced recycled polypropylene material also includes the auxiliary agent of optimizing performance in the technique scheme, can select in ultraviolet-resistant absorbent, toner or the Masterbatch one or more.
Polypropylene described in the said components adopts salvage material to make, and comprises granular, powdery, blocky copolymerization or homo-polypropylene; Described long glass fibres adopts the continuous roving of alkali-free, and Fibre diameter is 12～20um, and number number is 1200～No. 2400.
Described coupling agent is one or both in silane coupling agent, the phthalate ester coupling agent.
Described thermoplastic elastomer grafts comprises the terpolymer EP rubber EPDM or the polyolefin elastomer POE of vinylformic acid, maleic anhydride or glycidyl acrylate graft modification.
Described molten finger properties-correcting agent comprises one or both in dicumyl peroxide DCP and the benzoyl peroxide.
Oxidation inhibitor mainly is meant antioxidant 1010 and oxidation inhibitor 168.
Described lubricant comprises a kind of or several mixture among polyethylene wax, stearic acid, calcium stearate, the ethylenebis Stearyl Amine EBS.
The preparation method of above-mentioned long glass fiber reinforced recycled polypropylene material may further comprise the steps:
(1) will reclaim polypropylene, coupling agent, thermoplastic elastomer grafts, molten refer to that properties-correcting agent, oxidation inhibitor, lubricant and other auxiliary agent join in the homogenizer and stir;
(2) material that stirs is joined in the hopper of parallel double-screw extruder, forcing machine is divided into six sections from the hopper to the die head, each section temperature is respectively: 150～170 ℃, 170～190 ℃, 180～200 ℃, 180～200 ℃, 180～200 ℃, 180～210 ℃; The screw speed of main frame is 280～350r/min, the rotating speed of hopper feed screw rod is 24～32r/min, and then the material blended melting extruded, long glass fibres fully floods by the special dies adding at forcing machine die head place and with melt, drawn traction then forms the continuous long glass fiber that polypropylene coats;
(3) the grain bar that step (2) is made is through tank cooling, and entering dicing machine after air-dry carries out granulation, makes roving glass fiber and strengthens and reclaim polypropylene granules.
Wherein, the length of prepared long glass fiber-reinforced polypropylene pellet is 5～50mm.
Compared with prior art, roving glass fiber of the present invention strengthens the unusual effect that reclaims polypropylene and preparation method thereof and is: the grafts that adds thermoplastic elastomer in (1) described material, it not only can improve the toughness of material, improve its erosion-resisting characteristics, can also play the effect of compatilizer with the coupling agent logotype, improve the interface binding power of polypropylene and glass fibre greatly, thereby improve the performance of material; (2) less demanding to the molten finger of polypropylene bed material, can improve polyacrylic flowability well by adding a spot of molten finger properties-correcting agent, thereby improve the dipping effect of glass fibre; (3) because less demanding to the molten finger of polypropylene bed material, the main employing reclaimed polypropylene as bed material in the preparation process, low cost of manufacture, and also the source is very abundant, realizes resource circulation utilization simultaneously, is beneficial to environment protection; (4) adopt the long glass fibres of jack per line number not can prepare the long glass fiber reinforced recycled polypropylene material of different glass fiber contents easily, the length of pellet device may command pellet is in the scope of 5～50mm.
In sum, its preparation technology is succinct for long glass fiber reinforced recycled polypropylene material disclosed by the invention, and preparation cost is low, the finished-product material excellent combination property, and alternative most of metallic element is widely used in fields such as automobile, machinery, household electrical appliances manufacturing.
Embodiment
Long glass fiber reinforced recycled polypropylene material disclosed by the invention, cubage by mass percentage comprises polipropene 25～55%, long glass fibres 30～60%, coupling agent 0.4～0.8%, the grafts 3～8% of thermoplastic elastomer, molten properties-correcting agent 0.1～0.3%, oxidation inhibitor 0.2～0.4%, the lubricant 1～4% of referring to.Wherein can also add auxiliary agent 1～3% as required.Wherein, coupling agent with the collaborative interfacial adhesion that can improve polypropylene and glass fibre as compatilizer well that uses of thermoplastic elastomer grafts, is greatly improved the comprehensive physicals of material as surface treatment agent.In addition,, thereby can improve the toughness of material greatly, the intensity of material and rigidity will be reduced but add too much this elastomerics grafts because the thermoplastic elastomer grafts is to adopt elastomerics as matrix; Add an amount of molten finger properties-correcting agent and can improve polyacrylic melt fluidity, thereby can reduce requirement to the polypropylene material melting index, but excessive molten finger properties-correcting agent will make the impact property of material and elongation reduce greatly, therefore need its addition of control; The adding of oxidation inhibitor can effectively prevent the oxidative degradation of material in processing and use; Add examples of suitable lubricants will effectively improve material in the course of processing with the friction of machinery equipment, cut down the consumption of energy, and improve its flowability and release property; Auxiliary agents such as other pigment and uv-absorbing agent can be selected to add according to demand.
Embodiment 1
Carry out proportioning by following mass percent composition: reclaim polypropylene 39.2%, silane coupling agent KH5600.5% with alcohol dilution, maleic anhydride graft polyolefin elastomer POE-g-MAH5%, dicumyl peroxide DCP 0.1% with acetone diluted, antioxidant 1010 0.1%, oxidation inhibitor 1680.1%, polyethylene wax 3%, stearic acid 1%, Masterbatch 1%.
During preparation, at first above-mentioned material is joined in the homogenizer and stir;
Then mixture is joined in the hopper of twin screw extruder, forcing machine is divided into six sections from the hopper to the die head, each section temperature is set is respectively 165 ℃, 170 ℃, 180 ℃, 190 ℃, 200 ℃, 200 ℃, the screw speed of main control system is 280r/min, and the rotating speed of hopper feed screw rod is 30r/min;
To account for total mass per-cent again and be 50% long glass fibres adds from the mould of forcing machine die head, fully flood after stretching and drawing forms the long glass fibres that polypropylene coats with melt, cooling, pelletizing make long glass fiber reinforced recycled polypropylene material then.
The physicals of the above-mentioned long glass fiber reinforced recycled polypropylene material that makes is as shown in the table:
| Test event | Melt flow rate (MFR) | Tensile strength | Flexural strength | Modulus in flexure | The thermal distortion temperature |
| ??(g/10min) | ??(MPa) | ??(MPa) | ??(MPa) | Degree (℃) | |
| Testing method | ??GB/T?3682 | ??GB/T?1040.2 | ??GB/T?9341 | ??GB/T?9341 | ??GB/T?1634.2 |
| ??0.09 | ??84 | ??123 | ??6630 | ??135 |
As can be seen, the long glass fiber reinforced recycled polypropylene material that utilizes described method of patent of the present invention and formula rate to make all has preferable performance from aspects such as tensile strength, flexural strength, modulus in flexurees from the above table data.
Embodiment 2
Carry out proportioning by following mass percent composition: reclaim polypropylene granules 44.5%, silane coupling agent KH5501% with alcohol dilution, maleic anhydride graft polyolefin elastomer POE-g-MAH 8%, dicumyl peroxide DCP 0.2% with acetone diluted, antioxidant 1010 0.2%, oxidation inhibitor 1680.1%, polyethylene wax 3%, stearic acid 1%, Masterbatch 2%.
Similar with embodiment 1, during preparation:
At first above-mentioned material is joined in the homogenizer and stir;
Then mixture is joined in the hopper of twin screw extruder, forcing machine is divided into six sections from the hopper to the die head, each section temperature is set is respectively 165 ℃, 170 ℃, 180 ℃, 190 ℃, 200 ℃, 200 ℃, the screw speed of main control system is 260r/min, and the rotating speed of hopper feed screw rod is 30r/min;
To account for total mass per-cent again and be 40% long glass fibres adds from the mould of forcing machine die head, fully flood after stretching and drawing forms the long glass fibres that polypropylene coats with melt, cooling, pelletizing make long glass fiber reinforced recycled polypropylene material then.
The physicals of the above-mentioned long glass fiber reinforced recycled polypropylene material that makes is as shown in the table:
| Test event | Melt flow rate (MFR) (g/10min) | Tensile strength (MPa) | Flexural strength (MPa) | Modulus in flexure (MPa) | Heat-drawn wire (℃) |
| Testing method | ??GB/T?3682 | ??GB/T?1040.2 | ??GB/T?9341 | ??GB/T?9341 | ??GB/T?1634.2 |
| ??0.17 | ??72 | ??111 | ??5360 | ??121 |
Embodiment 3
Carry out proportioning by following mass percent composition: reclaim polypropylene 48.8%, silane coupling agent KH5501.2% with alcohol dilution, maleic anhydride graft polyolefin elastomer POE-g-MAH 8%, dicumyl peroxide DCP 0.2% with acetone diluted, antioxidant 1010 0.15%, oxidation inhibitor 1680.15%, polyethylene wax 3%, stearic acid 1.5%, Masterbatch 2%.
Similar with embodiment 1, during preparation:
At first above-mentioned material is joined in the homogenizer and stir;
Then mixture is joined in the hopper of twin screw extruder, forcing machine is divided into six sections from the hopper to the die head, each section temperature is set is respectively 165 ℃, 170 ℃, 180 ℃, 190 ℃, 200 ℃, 200 ℃, the screw speed of main control system is 320r/min, and the rotating speed of hopper feed screw rod is 31r/min;
To account for total mass per-cent again and be 35% long glass fibres adds from the mould of forcing machine die head, fully flood after stretching and drawing forms the long glass fibres that polypropylene coats with melt, cooling, pelletizing make long glass fiber reinforced recycled polypropylene material then.
The physicals of the above-mentioned long glass fiber reinforced recycled polypropylene material that makes is as shown in the table:
| Test event | Melt flow rate (MFR) (g/10min) | Tensile strength (MPa) | Flexural strength (MPa) | Modulus in flexure (MPa) | Heat-drawn wire (℃) |
| Testing method | ??GB/T?3682 | ??GB/T?1040.2 | ??GB/T?9341 | ??GB/T?9341 | ??GB/T?1634.2 |
| ??0.30 | ??65 | ??97 | ??5100 | ??117 |
Embodiment 4
Carry out proportioning by following mass percent composition: reclaim polypropylene 59%, silane coupling agent KH5600.5% with alcohol dilution, maleic anhydride graft terpolymer EP rubber EPDM-g-MAH5%, dicumyl peroxide DCP 0.2% with acetone diluted, antioxidant 1010 0.2%, oxidation inhibitor 1680.1%, polyethylene wax 3%, stearic acid 1%, Masterbatch 1%.
During preparation, at first above-mentioned material is joined in the homogenizer and stir;
Then mixture is joined in the hopper of twin screw extruder, forcing machine is divided into six sections from the hopper to the die head, each section temperature is set is respectively 150 ℃, 170 ℃, 180 ℃, 180 ℃, 18 ℃, 180 ℃, the screw speed of main control system is 320r/min, and the rotating speed of hopper feed screw rod is 33r/min;
To account for total mass per-cent again and be 30% long glass fibres adds from the mould of forcing machine die head, fully flood after stretching and drawing forms the long glass fibres that polypropylene coats with melt, cooling, pelletizing make long glass fiber reinforced recycled polypropylene material then.
The physicals of the above-mentioned long glass fiber reinforced recycled polypropylene material that makes is as shown in the table:
| Test event | Melt flow rate (MFR) (g/10min) | Tensile strength (MPa) | Flexural strength (MPa) | Modulus in flexure (MPa) | Heat-drawn wire (℃) |
| Testing method | ??GB/T?3682 | ??GB/T?1040.2 | ??GB/T?9341 | ??GB/T?9341 | ??GB/T?1634.2 |
| ??0.35 | ??58 | ??86 | ??4500 | ??110 |
Above-mentioned only is the preferred embodiment of the present invention; these embodiment only are used to explain the present invention and can not be interpreted as limitation of the present invention; in not deviating from claim of the present invention, under the situation of claimed scope, can carry out various improvement and variation to above-mentioned embodiment.
Claims (10)
1, long glass fiber reinforced recycled polypropylene material, cubage by mass percentage includes: polipropene 25～55%, long glass fibres 30～60%, coupling agent 0.4～0.8%, the grafts 3～8% of thermoplastic elastomer, molten properties-correcting agent 0.1～0.3%, oxidation inhibitor 0.2～0.4%, the lubricant 1～4% of referring to.
2, long glass fiber reinforced recycled polypropylene material according to claim 1 is characterized in that: it is formed component and also includes the auxiliary agent of optimizing performance, can select in ultraviolet-resistant absorbent, toner or the Masterbatch one or more.
3, long glass fiber reinforced recycled polypropylene material according to claim 2 is characterized in that: described polypropylene adopts salvage material to make, and comprises granular, powdery, blocky copolymerization or homo-polypropylene; Described long glass fibres adopts the continuous roving of alkali-free, and Fibre diameter is 12～20um, and number number is 1200～No. 2400.
4, long glass fiber reinforced recycled polypropylene material according to claim 2 is characterized in that: described coupling agent is one or both in silane coupling agent, the phthalate ester coupling agent.
5, long glass fiber reinforced recycled polypropylene material according to claim 2 is characterized in that: described thermoplastic elastomer grafts comprises the terpolymer EP rubber EPDM or the polyolefin elastomer POE of vinylformic acid, maleic anhydride or glycidyl acrylate graft modification.
6, long glass fiber reinforced recycled polypropylene material according to claim 2 is characterized in that: described molten finger properties-correcting agent comprises one or both in dicumyl peroxide DCP and the benzoyl peroxide.
7, long glass fiber reinforced recycled polypropylene material according to claim 2 is characterized in that: described oxidation inhibitor comprises one or both in antioxidant 1010 or the oxidation inhibitor 168.
8, long glass fiber reinforced recycled polypropylene material according to claim 2 is characterized in that: described lubricant comprises a kind of or several mixture among polyethylene wax, stearic acid, calcium stearate, the ethylenebis Stearyl Amine EBS.
9, a kind of method for preparing each described long glass fiber reinforced recycled polypropylene material of claim 1～8 may further comprise the steps:
(1) will reclaim polypropylene, coupling agent, thermoplastic elastomer grafts, molten refer to that properties-correcting agent, oxidation inhibitor, lubricant and other auxiliary agent join in the homogenizer and stir;
(2) material that stirs is joined in the hopper of parallel double-screw extruder, forcing machine is divided into six sections from the hopper to the die head, each section temperature is respectively: 150～170 ℃, 170～190 ℃, 180～200 ℃, 180～200 ℃, 180～200 ℃, 180～210 ℃; The screw speed of main frame is 280～350r/min, the rotating speed of hopper feed screw rod is 24～32r/min, and then the material blended melting extruded, long glass fibres fully floods by the mould adding at twin screw extruder die head place and with melt, drawn traction then forms the continuous long glass fiber that polypropylene coats;
(3) the grain bar that step (2) is made is through tank cooling, and entering dicing machine after air-dry carries out granulation, makes the long glass fiber-reinforced polypropylene pellet.
10, the preparation method of long glass fiber reinforced recycled polypropylene material according to claim 9 is characterized in that: the length of prepared long glass fiber-reinforced polypropylene pellet is 5～50mm.
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