CN101654535A - Halogen-free flame-retardant long glass fiber reinforcement recycled polypropylene material and preparation method thereof - Google Patents
Halogen-free flame-retardant long glass fiber reinforcement recycled polypropylene material and preparation method thereof Download PDFInfo
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Abstract
The invention discloses a halogen-free flame-retardant long glass fiber reinforcement recycled polypropylene material which comprises the following components in percentage by weight: 25%-55% of recycled polypropylene, 15%-40% of long glass fiber, 20%-35% of expansion type halogen-free flame retardant, 0.5%-3% of smoke inhibitor, 0.4%-0.8% of coupling agents, 3%-8% of compatilizer, 0.1%-0.3% of fat melting modifier, 0.2%-0.4% of antioxygen, 1%-4% of lubricating agents and 1%-3% of functional auxiliary agents. The preparation method comprises the following steps: placing the components except the long glass fiber in a high-speed stirrer to be uniformly stirred and then placing into a parallel double-screw extruder with preset temperature in sections, and then adding the long glass fiber inthe components, mixing and extruding together; cooling and drying, and finally granulating. The invention uses the recycled polypropylene as a bottom material and improves the flame-retardant propertyby adding the expansion type halogen-free flame retardant and the smoke inhibitor, has low cost, simple and easy manufacture and good comprehensive property and can be used in fields, i.e. home appliances, electrical appliances, automobile parts, and the like.
Description
Technical field
The present invention relates to the polymer modification technical field, design a kind of halogen-free intumescent flame-retardant long glass fiber reinforced recycled polypropylene material and preparation method thereof especially.
Background technology
The long glass fibres reinforced thermoplastics(RTP) has distinguishing features such as high strength, high rigidity, high-dimensional stability, low warpage, long service life, creep resistance be good, and possesses good moulding processability, be widely used in comprising the industry of automobile, communication, electronic apparatus, power tool etc. and civilian multi-field, particularly the application in automotive field is more extensive.Long glass fiber reinforced polypropylene is a kind of in the long glass fibres reinforced thermoplastics(RTP), is used to make the engine shield, instrument board framework, battery tray, chair framework, car front-end module, collision bumper, luggage carrier, spare tyre dish, splash pan, fan blade, engine pan, car roof lining frame etc. of car at present in a large number by people.But the oxygen index of existing long glass fiber reinforced polypropylene (LOI) is very low, and very easy burning and combustion heating amount are big, even can further promote burning by a large amount of unsaturated gases of generation in combustion processes.This just makes that long glass fiber reinforced polypropylene is not suitable for using on the occasion that can have relatively high expectations to Flame Retardancy, that is to say that people need carry out flame-retardant modifiedly just applying it on the occasion that can have relatively high expectations to Flame Retardancy to long glass fiber reinforced polypropylene.In order to strengthen the flame retardant resistance of long glass fiber reinforced polypropylene, people adopt halogen-containing fire retardant to carry out flame-retardant modified to long glass fiber reinforced polypropylene, but because halogen-containing fire retardant can produce a large amount of objectionable impuritiess in combustion processes, many countries promulgate a decree and control the content of halogen in the used fire retardant of long glass fiber reinforced polypropylene.
Chinese patent CN 101418100A is that main raw material prepares the halogen-free flame-retardant long glass fiber reinforced polypropylene material through injection moulding with long glass fiber reinforced polypropylene master batch, halogen-free flameproof master batch, functional agent master batch, acrylic resin, has solved halogen-containing fire retardant can produce a large amount of objectionable impuritiess in combustion processes problem.But the technical scheme complex process of this patent disclosure, tooling cost height, and the disclosed halogen-free flame-retardant long glass fiber reinforced polypropylene material of this patent is that several raw materials mix the goods through injection moulding, have the serious stress concentration phenomenon, so that each position performance of goods is inhomogeneous and may have mass defect and potential safety hazard.Chinese patent CN 1807497A discloses the another method of preparation combustion-proof glass fiber reinforced polypropylene composite material, it adopts ammonium polyphosphate, trimeric cyanamide and tetramethylolmethane to form expansion type flame retardant and the compound preparation anti-flaming polypropylene material of polypropylene, this anti-flaming polypropylene material again with long glass fibres, glass mat is compound extrudes the preparation combustion-proof glass fiber reinforced polypropylene composite material through forcing machine.This method needs twice complete processing, have the high problem of tooling cost equally, and the ammonium polyphosphate temperature tolerance is relatively poor, decomposes through adding man-hour part ammonium polyphosphate for twice, and this is very big to the flame retardant effect influence.In addition, because three kinds of fire retardants being adopted all belong to organic low molecular substance with polyacrylic consistency difference in this method, produce " bloom " phenomenon to the material surface migration easily.
Summary of the invention
Technical problem to be solved by this invention provides that a kind of technology is simple, cost of manufacture is low, the halogen-free intumescent flame-retardant long glass fiber reinforced recycled polypropylene material of excellent performance, and further discloses this preparation methods.
For solving the problems of the technologies described above, the technical scheme that the present invention realizes is: a kind of halogen-free intumescent flame-retardant long glass fiber reinforced recycled polypropylene material, and its component cubage by mass percentage comprises: reclaim polipropene 25～55%, long glass fibres 15～40%, expanding halide-free fire-retardant 20～35%, press down fumicants 0.5～3%, coupling agent 0.4～0.8%, compatilizer 3～8%, the molten properties-correcting agent 0.1～0.3% that refers to, oxidation inhibitor 0.2～0.4%, lubricant 1～4%, functional agent 1～3%.
Reclaim polypropylene described in the said components and comprise 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 expanding halide-free fire-retardant selection is by the phosphorus-nitrogen containing flame retardant of appointing several combinations of substances to form in phosphoric acid ester, phosphoric acid salt, starch, tetramethylolmethane, trimeric cyanamide, Dyhard RU 100, the ammonium polyphosphate.The expansion type flame retardant that in reactor, is composited by several materials wherein preferably through chemical reaction.
But described fumicants comprises one or more in molybdenum oxide, ammonium octamolybdate, zinc oxide, the zinc borate, described coupling agent is one or both in silane coupling agent, the phthalate ester coupling agent, described compatilizer is the thermoplastic elastomer grafts, and the 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 is one or both the organo-peroxide that comprises in dicumyl peroxide (DCP) and the benzoyl peroxide, oxidation inhibitor is meant antioxidant 1010 and oxidation inhibitor 168, lubricant comprises one or more the mixture in polyethylene wax, stearic acid, calcium stearate, the ethylenebis Stearyl Amine (EBS), and described functional agent comprises one or more of ultraviolet-resistant absorbent, toner or Masterbatch.
The preparation method of above-mentioned halogen-free flame-retardant long glass fiber reinforcement recycled polypropylene material may further comprise the steps:
(1) will reclaim polypropylene, fire retardant, press down fumicants, coupling agent, compatilizer, moltenly refer to that properties-correcting agent, oxidation inhibitor, lubricant and functional 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: 130～140 ℃, 140～150 ℃, 140～150 ℃, 150～160 ℃, 150～160 ℃, 160～170 ℃, the screw speed of main frame is 250～330r/min, and the rotating speed of hopper feed screw rod is 24～35r/min, and then the material blended melting is extruded, long glass fibres fully soaks into by the mould adding at forcing machine die head place and with melt, and the drawn traction forms the continuous long glass fiber that polypropylene coats then.
(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 halogen-free flameproof roving glass fiber and strengthens and reclaim polypropylene granules.
Compared with prior art, the advantage that the present invention has is: (1) adopts the source to enrich and the low recovery polypropylene of cost is done material, and realization is turned waste into wealth, resource circulation utilization, reduces cost greatly.(2) expansion type flame retardant is compound through chemical reaction among the present invention, has improved molecular weight, effectively solves the problem of separating out of conventional expanded type fire retardant.The amount of being fuming when (3) add pressing down fumicants in the prescription and reduce material combustion effectively improves flame retardant effect.(4) the present invention adopts single stage method to prepare fire-retardant roving glass fiber enhancing and reclaims polypropylene material, effectively solves the fire retardant problem that easy decomposes, flame retardant effect reduce after repeatedly processing.(5) long glass fibres directly adds from the impregnation mold that the forcing machine die head goes out; avoid long glass fiber to be interrupted by screw rod shearing, guarantee from the grain bar that die head pulls out be the continuous long glass fiber that coats of polypropylene, length by dicing machine control particle is 5～50mm.(6) the present invention adopts and reclaims polypropylene and do bed material and add expanding halide-free fire-retardant, press down fumicants and improve flame retardant properties, and cost is low, making is simple and easy and over-all properties is good, can be applicable to fields such as household electrical appliances, electrical equipment, auto-parts.
Embodiment
Halogen-free flame-retardant long glass fiber reinforcement recycled polypropylene material disclosed by the invention, cubage by mass percentage comprises recovery polipropene 25～55%, long glass fibres 15～40%, expanding halide-free fire-retardant 20～35% presses down fumicants 0.5～3%, coupling agent 0.4～0.8%, compatilizer 3～8%, molten properties-correcting agent 0.1～0.3%, the oxidation inhibitor 0.2～0.4% of referring to, lubricant 1～4%, functional agent 1～3%.
Wherein, expanding halide-free fire-retardant adopts chemical method directly to be composited, and effectively solves expansion type flame retardant and adds the problem of separating out phenomenon in the superpolymer easily to.The selected phosphorus-nitrogen containing flame retardant of the application does not contain any halogen, belong to the novel environment friendly material, adopt directly compound being prepared of chemical method, solved the problem of separating out that expansion type flame retardant exists for many years always, and thermostability height (＞270 ℃), the flame retardant effect excellence when adding 30wt%, can reach UL94 (1.6mm) V-0 rank.Harmful heavy metal compositions such as not leaded, antimony, cadmium meet the RoHS of European Union requirement.
Added an amount of fumicants that presses down in the halogen-free intumescent flame-retardant long glass fiber reinforced recycled polypropylene material of the present invention, the amount of being fuming when helping to reduce material combustion reduces that material produces a large amount of toxic smokes in fire and the possibility that causes casualty accident.Coupling agent with the collaborative interfacial adhesion that can improve polypropylene and glass fibre as compatilizer well that uses of thermoplastic elastomer grafts, improves the comprehensive physicals of material as surface treatment agent.In addition, the thermoplastic elastomer grafts adopts elastomerics as matrix, improves the toughness of material greatly, but add too much elastomerics grafts the intensity of material and rigidity is reduced.Add an amount of molten finger properties-correcting agent in the material and can improve polyacrylic melt fluidity, improve the effect of impregnation may of glass fibre, but excessive molten finger properties-correcting agent reduces the impact property of material and elongation greatly, therefore need its addition of control.Add oxidation inhibitor and effectively prevent the oxidative degradation of material in processing and use.Add examples of suitable lubricants reduce material in the course of processing with the friction of equipment, cut down the consumption of energy and improve its flowability and release property.Auxiliary agents such as other pigment and uv-absorbing agent are selected to add according to demand.
Below by embodiment content of the present invention is further analyzed and described:
Embodiment 1
Carry out proportioning by following mass percent composition: reclaim polypropylene granules 43.2%, expanding halide-free fire-retardant 30%, press down fumicants molybdenum oxide 2%, with the silane coupling agent KH5500.5% of alcohol dilution, maleic anhydride graft polyolefin elastomer POE-g-MAH 5%, with the dicumyl peroxide DCP 0.1% of acetone diluted, antioxidant 1010 and oxidation inhibitor 168 each 0.1%, polyethylene wax 2%, stearic acid 1%, Masterbatch 1%.Preparation process is as follows:
Earlier above-mentioned material is joined in the homogenizer and stir.
Mixture is joined in the hopper of twin screw extruder, forcing machine is divided into six sections from the hopper to the die head again, each section temperature is set is respectively 135 ℃, 145 ℃, 148 ℃, 155 ℃, 158 ℃, 160 ℃, the screw speed of main control system is 280r/min, and the rotating speed of hopper feed screw rod is 33r/min.
To account for total mass per-cent again and be 15% long glass fibres adds from the mould of forcing machine die head, long glass fibres fully soaks into by the melt that mould enters back and polypropylene miser, forms the continuous long glass fiber that polypropylene coats through the traction tie rod then.Cooling, pelletizing make flame-retardant long glass fiber reinforcement recycled polypropylene material then.
Embodiment 2
Carry out proportioning by following mass percent composition: reclaim polypropylene granules 37.7%, expanding halide-free fire-retardant 30%, press down fumicants molybdenum oxide 2.0% and zinc oxide 0.5%, with the silane coupling agent KH5600.5% of alcohol dilution, maleic anhydride graft polyolefin elastomer POE-g-MAH 5%, with the dicumyl peroxide DCP 0.1% of acetone diluted, antioxidant 1010 and oxidation inhibitor 168 each 0.1%, polyethylene wax 2%, stearic acid 1%, Masterbatch 1%.Preparation process is as follows:
Earlier above-mentioned material is joined in the homogenizer and stir.
Mixture is joined in the hopper of twin screw extruder, forcing machine is divided into six sections from the hopper to the die head again, each section temperature is set is respectively 138 ℃, 140 ℃, 150 ℃, 155 ℃, 155 ℃, 160 ℃, the screw speed of main control system is 275r/min, and the rotating speed of hopper feed screw rod is 34r/min.
To account for total mass per-cent again and be 20% long glass fibres adds from the mould of forcing machine die head, long glass fibres fully soaks into by the melt that mould enters back and polypropylene miser, forms the continuous long glass fiber that polypropylene coats through the traction tie rod then.Cooling, pelletizing make flame-retardant long glass fiber reinforcement recycled polypropylene material then.
Embodiment 3
Carry out proportioning by following mass percent composition: reclaim polypropylene granules 31.3%, expanding halide-free fire-retardant 25%, press down fumicants molybdenum oxide 1.5%, with the silane coupling agent KH560 0.8% of alcohol dilution, maleic anhydride graft polyolefin elastomer POE-g-MAH 6%, with the dicumyl peroxide DCP 0.2% of acetone diluted, antioxidant 1010 and oxidation inhibitor 168 each 0.1%, polyethylene wax 2%, ethylenebis Stearyl Amine 1%, Masterbatch 2%.Preparation process is as follows:
Earlier above-mentioned material is joined in the homogenizer and stir.
Mixture is joined in the hopper of twin screw extruder, forcing machine is divided into six sections from the hopper to the die head again, each section temperature is set is respectively 140 ℃, 145 ℃, 150 ℃, 160 ℃, 160 ℃, 165 ℃, the screw speed of main control system is 265r/min, and the rotating speed of hopper feed screw rod is 35r/min.
To account for total mass per-cent again and be 30% long glass fibres adds from the mould of forcing machine die head, long glass fibres fully soaks into by the melt that mould enters back and polypropylene miser, forms the continuous long glass fiber that polypropylene coats through the traction tie rod then.Cooling, pelletizing make flame-retardant long glass fiber reinforcement recycled polypropylene material then.
Embodiment 4
Carry out proportioning by following mass percent composition: reclaim polypropylene granules 52.1%, expanding halide-free fire-retardant 20%, press down fumicants molybdenum oxide 0.5% and zinc borate 0.5%, with the silane coupling agent KH550 0.5% of alcohol dilution, maleic anhydride graft polyolefin elastomer POE-g-MAH 5%, with the dicumyl peroxide DCP 0.2% of acetone diluted, antioxidant 1010 and oxidation inhibitor 168 each 0.1%, polyethylene wax 3%, ethylenebis Stearyl Amine 1%, Masterbatch 2%.Preparation process is as follows:
Earlier above-mentioned material is joined in the homogenizer and stir.
Mixture is joined in the hopper of twin screw extruder, forcing machine is divided into six sections from the hopper to the die head again, each section temperature is set is respectively 135 ℃, 140 ℃, 150 ℃, 160 ℃, 160 ℃, 160 ℃, the screw speed of main control system is 278r/min, and the rotating speed of hopper feed screw rod is 33r/min.
To account for total mass per-cent again and be 15% long glass fibres adds from the mould of forcing machine die head, long glass fibres fully soaks into by the melt that mould enters back and polypropylene miser, forms the continuous long glass fiber that polypropylene coats through the traction tie rod then.Cooling, pelletizing make flame-retardant long glass fiber reinforcement recycled polypropylene material then.
Embodiment 5
Carry out proportioning by following mass percent composition: reclaim polypropylene granules 36.1%, expanding halide-free fire-retardant 35%, press down fumicants molybdenum oxide 2% and zinc borate 1%, with the silane coupling agent KH5600.5% of alcohol dilution, maleic anhydride graft polyolefin elastomer POE-g-MAH 5%, with the dicumyl peroxide DCP 0.2% of acetone diluted, antioxidant 1010 and oxidation inhibitor 168 each 0.1%, polyethylene wax 3%, ethylenebis Stearyl Amine 1%, Masterbatch 1%.Preparation process is as follows:
Earlier above-mentioned material is joined in the homogenizer and stir.
Mixture is joined in the hopper of twin screw extruder, forcing machine is divided into six sections from the hopper to the die head again, each section temperature is set is respectively 135 ℃, 138 ℃, 145 ℃, 160 ℃, 160 ℃, 165 ℃, the screw speed of main control system is 275r/min, and the rotating speed of hopper feed screw rod is 32r/min.
To account for total mass per-cent again and be 15% 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 flame-retardant long glass fiber reinforcement recycled polypropylene material then.
The physical and mechanical property and the flame retardant properties of gained halogen-free intumescent flame-retardant long glass fiber reinforced recycled polypropylene material are as shown in the table in the foregoing description, data as can be seen from table, when the material proportion in selecting embodiment 3 prepares, though the halogen-free intumescent flame-retardant long glass fiber reinforced recycled polypropylene material elongation at break that makes is lower, but over-all properties is preferable, is preferred material proportion.
| Title | IZOD notched Izod impact strength [J/m] | Tensile strength [MPa] | Elongation at break [%] | Flexural strength [MPa] | Modulus in flexure [MPa] | Combustionproperty |
| Testing standard | ??ASTM?D256 | ?ASTM?D638 | ?ASTM?D638 | ??ASTM?D790 | ?ASTM?D790 | ??UL94 |
| Embodiment 1 | ??108.2 | ?83.2 | ?15 | ??106.6 | ??3852 | ??3.2mmV-0 |
| Embodiment 2 | ??124.2 | ?85.6 | ?16 | ??111.5 | ??4365 | ??3.2mmV-0 |
| Embodiment 3 | ??135.8 | ?90.2 | ?7 | ??113.6 | ??5261 | ??3.2mmV-1 |
| Embodiment 4 | ??122.9 | ?79.8 | ?30 | ??102.7 | ??3580 | ??3.2mmV-2 |
| Embodiment 5 | ??98.5 | ?84.8 | ?12 | ??108.5 | ??4053 | ??1.6mmV-0 |
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, a kind of halogen-free flame-retardant long glass fiber reinforcement recycled polypropylene material, it is characterized in that: its component cubage by mass percentage comprises: reclaim polipropene 25～55%, long glass fibres 15～40%, expanding halide-free fire-retardant 20～35% presses down fumicants 0.5～3%, coupling agent 0.4～0.8%, compatilizer 3～8%, molten properties-correcting agent 0.1～0.3%, the oxidation inhibitor 0.2～0.4% of referring to, lubricant 1～4%, functional agent 1～3%.
2, halogen-free flame-retardant long glass fiber reinforcement recycled polypropylene material according to claim 1, it is characterized in that: described recovery polypropylene comprises granular, powdery, blocky copolymerization or homo-polypropylene, described long glass fibres adopts the continuous roving of alkali-free, Fibre diameter is 12～20um, and number number is 1200～No. 2400.
3, halogen-free flame-retardant long glass fiber reinforcement recycled polypropylene material according to claim 1 is characterized in that: described expanding halide-free fire-retardant selection is by the phosphorus-nitrogen containing flame retardant of appointing several combinations of substances to form in phosphoric acid ester, phosphoric acid salt, starch, tetramethylolmethane, trimeric cyanamide, Dyhard RU 100, the ammonium polyphosphate.
4, halogen-free flame-retardant long glass fiber reinforcement recycled polypropylene material according to claim 3 is characterized in that: described expanding halide-free fire-retardant selection is by the expansion type phosphor nitrogen flame retardant of appointing several materials to be composited through chemical reaction in reactor in phosphoric acid ester, phosphoric acid salt, starch, tetramethylolmethane, trimeric cyanamide, Dyhard RU 100, the ammonium polyphosphate.
5, halogen-free flame-retardant long glass fiber reinforcement recycled polypropylene material according to claim 1 is characterized in that: but described fumicants selection is one or more in molybdenum oxide, ammonium octamolybdate, zinc oxide, the zinc borate.
6, halogen-free flame-retardant long glass fiber reinforcement recycled polypropylene material according to claim 1 is characterized in that: described coupling agent is one or both in silane coupling agent, the phthalate ester coupling agent.
7, halogen-free flame-retardant long glass fiber reinforcement recycled polypropylene material according to claim 1, it is characterized in that: described compatilizer is the thermoplastic elastomer grafts, and the thermoplastic elastomer grafts comprises the terpolymer EP rubber EPDM or the polyolefin elastomer POE of vinylformic acid, maleic anhydride or glycidyl acrylate graft modification.
8, halogen-free flame-retardant long glass fiber reinforcement recycled polypropylene material according to claim 1 is characterized in that: described molten finger properties-correcting agent is organo-peroxide, selects in dicumyl peroxide (DCP) and the benzoyl peroxide one or both.
9, halogen-free flame-retardant long glass fiber reinforcement recycled polypropylene material according to claim 1, it is characterized in that: oxidation inhibitor is meant antioxidant 1010 and oxidation inhibitor 168, lubricant comprises one or more the mixture in polyethylene wax, stearic acid, calcium stearate, the ethylenebis Stearyl Amine (EBS), and described functional agent comprises one or more of ultraviolet-resistant absorbent, toner or Masterbatch.
10, according to the preparation method of each described halogen-free flame-retardant long glass fiber reinforcement recycled polypropylene material of claim 1 to 9, may further comprise the steps:
(1) will reclaim polypropylene, fire retardant, press down fumicants, coupling agent, compatilizer, moltenly refer to that properties-correcting agent, oxidation inhibitor, lubricant and functional 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: 130～140 ℃, 140～150 ℃, 140～150 ℃, 150～160 ℃, 150～160 ℃, 160～170 ℃, the screw speed of main frame is 250～330r/min, and the rotating speed of hopper feed screw rod is 24～35r/min, and then the material blended melting is extruded, long glass fibres fully soaks into by the mould adding at forcing machine die head place and with melt, and the drawn traction forms the continuous long glass fiber that polypropylene coats then.
(3) the grain bar that step (2) is made is through tank cooling, and entering dicing machine after air-dry carries out granulation, makes fire-retardant roving glass fiber and strengthens and reclaim polypropylene granules.
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