CN102585346A - Halogen-free flame-retardant POE (Polyolefin Elastomer) compound material and preparation method thereof - Google Patents
Halogen-free flame-retardant POE (Polyolefin Elastomer) compound material and preparation method thereof Download PDFInfo
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- CN102585346A CN102585346A CN2012100490976A CN201210049097A CN102585346A CN 102585346 A CN102585346 A CN 102585346A CN 2012100490976 A CN2012100490976 A CN 2012100490976A CN 201210049097 A CN201210049097 A CN 201210049097A CN 102585346 A CN102585346 A CN 102585346A
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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
- B29C48/04—Particle-shaped
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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
- B29C48/36—Means for plasticising or homogenising the moulding material or forcing it through the nozzle or die
- B29C48/395—Means for plasticising or homogenising the moulding material or forcing it through the nozzle or die using screws surrounded by a cooperating barrel, e.g. single screw extruders
- B29C48/40—Means for plasticising or homogenising the moulding material or forcing it through the nozzle or die using screws surrounded by a cooperating barrel, e.g. single screw extruders using two or more parallel screws or at least two parallel non-intermeshing screws, e.g. twin screw extruders
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Abstract
The invention discloses a halogen-free flame-retardant POE (Polyolefin Elastomer) compound material and a preparation method thereof. The halogen-free flame-retardant POE compound material is prepared from the following components in parts by weight: 100 parts of POE resin, 70-140 parts of halogen-free compound retardant, 5-30 parts of modifier, 3-10 parts of lubricating dispersing agent and 0.1-0.6 parts of anti-oxidant. The preparation method comprises the following steps of: putting the POE resin, the halogen-free retardant, the modifying agent, the lubricating dispersing agent and the anti-oxidant into a high-speed mixing machine for mixing till the materials are heated to 65-75 DEG C through frication heat generated by mixing, discharging and cooling; and feeding a cooled mixed material into a double-screw extruder for melting and extruding, cooling an extruded bar stock with a water groove, and drawing into a granulating machine for granulating to obtain the halogen-free frame-retardant POE compound material. The elongation rate of the halogen-free flame-retardant POE compound material is over 600 percent, the oxygen index is over 30 percent, the liquidity of a melt is high, and the heat ageing resistance is high.
Description
Technical field
The present invention relates to a kind of polymer composite and preparation method thereof, be specifically related to a kind of halogen-free flameproof POE matrix material and preparation method thereof.
Background technology
The POE resin is that U.S. DOW chemical company is the new type polyolefin elastomerics of polymerization catalyst with the metallocene; It has advantages such as cheap, that forming process is easy with respect to other polyolefin elastomers, is widely used in fields such as automobile, electronic apparatus, building sealing, exerciser and polymer toughening modification.
POE belongs to inflammable material, and along with being on the increase of its application, it is flame-retardant modified imperative that it is carried out.Traditional halogen containing flame-retardant flame retarding efficiency is high, but can produce fatal toxic smog during its burning.
Summary of the invention
One of the object of the invention is to address the above problem, and a kind of halogen-free flameproof POE matrix material is provided.
Two of the object of the invention provides the preparation method of above-mentioned halogen-free flameproof POE matrix material.
The technical scheme that realizes one of the object of the invention is: a kind of halogen-free flameproof POE matrix material; Component by following weight part is processed: 100 parts of POE resins, 70～140 parts of Halogenless composite fire retardants, 5～30 parts of properties-correcting agent; 3～10 parts of lubrication dispersing agents, 0.1～0.6 part in oxidation inhibitor; Said Halogenless composite fire retardant by active hydrogen Natural manganese dioxide/active aluminium hydroxide and zinc borate and microcapsule red phosphorus according to 100: (2～10): the weight ratio of (8～20) is formed.
Described active hydrogen Natural manganese dioxide/active aluminium hydroxide is to be obtained by silane coupler modified micron order Marinco H/micron order white lake, and wherein the weight ratio of micron order Marinco H/micron order white lake and silane coupling agent is 100: 2～100: 4; Said micron order Marinco H/micron order white lake is meant that median size is Marinco H/white lake of 20 microns～200 microns.
Described properties-correcting agent is new LDPE (film grade) or high density polyethylene(HDPE).
Described lubrication dispersing agent is solid paraffin or polyethylene wax.
Described oxidation inhibitor is antioxidant 1010.
Two the technical scheme that realizes the object of the invention is: a kind of preparation method of halogen-free flameproof POE matrix material; Have following steps: 1. will pour in the high-speed mixer and mix according to POE resin, active hydrogen Natural manganese dioxide/active aluminium hydroxide, zinc borate, microcapsule red phosphorus, properties-correcting agent, lubrication dispersing agent and oxidation inhibitor that prescription takes by weighing; Make temperature of charge be increased to 65 ℃～75 ℃ until mixing the heat of friction that is produced, the discharging cooling; 2. cooled mixture is sent in the twin screw extruder and melt extrudes, the billot of being extruded gets into the dicing machine granulation through tank cooling, traction, promptly gets halogen-free flameproof POE matrix material.
Active hydrogen Natural manganese dioxide/the active aluminium hydroxide of above-mentioned steps described in 1. is to be obtained by silane coupler modified micron order Marinco H/micron order white lake, and wherein the weight ratio of micron order Marinco H/micron order white lake and silane coupling agent is 100: 2～100: 4; Said micron order Marinco H/micron order white lake is meant that median size is Marinco H/white lake of 20 microns～200 microns.The preparation method of said active hydrogen Natural manganese dioxide/active aluminium hydroxide is: according to proportioning micron order Marinco H/micron order white lake and silane coupling agent are poured into and mixed 5min～10min in the high-speed mixer; Make material temperature reach 110 ℃～120 ℃ until mixing the heat of friction that is produced, the discharging cooling promptly gets active hydrogen Natural manganese dioxide/active aluminium hydroxide.
The properties-correcting agent of above-mentioned steps described in 1. is new LDPE (film grade) or high density polyethylene(HDPE); Described lubrication dispersing agent is solid paraffin or polyethylene wax; Described oxidation inhibitor is antioxidant 1010.
Above-mentioned steps 2. in, twin screw extruder each the district temperature be: T
1=80 ℃～85 ℃, T
2=100 ℃～110 ℃, T
3=130 ℃～140 ℃, T
4=150 ℃～160 ℃, T
5=160 ℃～170 ℃, T
6=170 ℃～180 ℃, T
7=170 ℃～180 ℃, T
8=170 ℃～180 ℃, T
9=160 ℃～165 ℃, T
Mould=155 ℃～160 ℃.
The positively effect that the present invention has: (1) halogen-free flameproof POE of the present invention composite material by adopting these three kinds of halogen-free flame retardantss of Marinco H/white lake, zinc borate and microcapsule red phosphorus form Halogen composite flame retardant systems; Guarantee to make this matrix material not halogen-containing environmental sound on the one hand; There is good fire-retardant synergy in these three kinds of fire retardants on the other hand; Particularly the effect of knot charcoal is played in the adding of zinc borate effectively, can make this matrix material have good flame retardation effect, hang down the characteristics that cigarette, no poisonous and harmful and irritant gas produce, over-all properties is high.(2) one of fire retardant of halogen-free flameproof POE composite material by adopting of the present invention is active hydrogen Natural manganese dioxide/active aluminium hydroxide of handling through silane coupling agent; This active hydrogen Natural manganese dioxide/active aluminium hydroxide and POE resin have good avidity; Both help improving the mechanical property of this matrix material, helped improving the flowability of this Composite Melt again.And silane coupling agent not only plays the coupled action of inorganics and polymkeric substance therein, also has certain fire-retardant synergy, helps improving the overall flame effect of material, obviously is superior to adopting aluminate coupling agent or titanate coupling agent.(3) properties-correcting agent selected for use of halogen-free flameproof POE matrix material of the present invention is high density polyethylene(HDPE) or new LDPE (film grade), and they and POE resin have good consistency, and in the POE resin, can significantly play strengthening action, improve the intensity of this matrix material.(4) lubrication dispersing agent of halogen-free flameproof POE composite material by adopting of the present invention is solid paraffin or polyethylene wax; They can effectively reduce the melt flow resistance in this Composite Preparation or the processing; Help Halogenless composite fire retardant simultaneously and be dispersed in this matrix material, improve the flame retardant resistance and the mechanical property of this matrix material.(5) do not contain the liquid filling agent in the halogen-free flameproof POE matrix material of the present invention, can make this matrix material not have the liquid infiltration phenomenon, kept good surface appearance, and elasticity changed by high and low temperature little, high thermal resistance and winter hardiness are all better.(6) halogen-free flameproof POE fracture of composite materials elongation of the present invention is up to more than 600%; Oxygen index is up to more than 30%; And the good fluidity of melt (melt flow rate(MFR) is greater than 2.0g/10min), heat-resistant aging good (80 ℃, the tensile strength velocity of variation was less than 15% in 168 hours).
Embodiment
(embodiment 1)
The halogen-free flameproof POE matrix material of present embodiment is processed by the component of following weight:
The POE resin of 100kg, the active hydrogen Natural manganese dioxide of 100kg, the zinc borate of 6kg, the microcapsule red phosphorus of 18kg, the antioxidant 1010 of the new LDPE (film grade) of 15kg, the solid paraffin of 4kg (fusing point is 50 ℃, down together) and 0.5kg.
The preparation method of above-mentioned halogen-free flameproof POE matrix material has following steps:
1. earlier with Nanjing of the micron order Marinco H (median size is 100 microns) of 200kg and 6kg forward the trade mark of chemical industry ltd production be that to pour rotating speed into be to mix 8min in 900 rev/mins of high-speed mixers for the silane coupling agent of KH-570; Make material temperature reach 115 ℃ until mixing the heat of friction that is produced; Discharging cooling then promptly gets active hydrogen Natural manganese dioxide.
Pouring the antioxidant 1010 of the solid paraffin of the new LDPE (film grade) of the microcapsule red phosphorus of the zinc borate of the POE resin of the above-mentioned active hydrogen Natural manganese dioxide that makes of 100kg and 100kg, 6kg, 18kg, 15kg, 4kg and 0.5kg into rotating speed is to mix in 900 rev/mins the high-speed mixer; Make temperature of charge be increased to 70 ℃ until mixing the heat of friction that is produced, mixture is sent under agitation is cooled to envrionment temperature in the cooling and stirring device then.
2. cooled mixture is sent in the twin screw extruder and melt extrudes; The billot of being extruded gets into the dicing machine granulation through tank cooling, traction, promptly gets halogen-free flameproof POE matrix material.The temperature in each district of twin screw extruder is: T
1=80 ℃～85 ℃, T
2=100 ℃～110 ℃, T
3=130 ℃～140 ℃, T
4=150 ℃～160 ℃, T
5=160 ℃～170 ℃, T
6=170 ℃～180 ℃, T
7=170 ℃～180 ℃, T
8=170 ℃～180 ℃, T
9=160 ℃～165 ℃, T
Mould=155 ℃～160 ℃.
(embodiment 2～embodiment 4)
The preparation method of each embodiment is identical with embodiment 1, and difference is the weight proportion of each component, specifically sees table 1.
Table 1
| ? | Embodiment 1 | Embodiment 2 | Embodiment 3 | Embodiment 4 |
| The POE resin | 100kg | 100kg | 100kg | 100kg |
| Active hydroxide | Active hydrogen Natural manganese dioxide 100kg | Active aluminium hydroxide 100kg | Active aluminium hydroxide 100kg | Active hydrogen Natural manganese dioxide 100kg |
| Zinc borate | 6kg | 8kg | 6kg | 10kg |
| Microcapsule red phosphorus | 18kg | 20kg | 14kg | 16kg |
| Properties-correcting agent | New LDPE (film grade) 15kg | High density polyethylene(HDPE) 10kg | High density polyethylene(HDPE) 10kg | High density polyethylene(HDPE) 12kg |
| Lubrication dispersing agent | Solid paraffin 2kg | Solid paraffin 5kg | Solid paraffin 6kg | Polyethylene wax 6kg |
| Antioxidant 1010 | 0.5kg | 0.8kg | 0.5kg | 0.7kg |
(application examples)
The halogen-free flameproof POE matrix material that embodiment 1～embodiment 4 is made joins the pulling-on piece of plasticating in two roller mills; Compression molding on tabletting machine; Adopt plastics standard test specimen sampling machine to produce standard test specimen; And by national standard to this standard test specimen make an experiment test its mechanical property and flame retardant resistance, test result is seen table 2.
Table 2
| Test performance | Performance index | Testing standard | Embodiment 1 | Embodiment 2 | Embodiment 3 | Embodiment 4 |
| Tensile strength/MPa | ﹥10.0 | GB/T 1042-2006 | 12.6 | 13.2 | 13.6 | 13.1 |
| Elongation at break/% | ﹥400 | GB/T 1042-2006 | 650 | 630 | 610 | 620 |
| Melt flow rate(MFR)/g10min -1 | ﹥2.0 | GB/T 3682-2000 | 3.2 | 2.8 | 2.5 | 2.3 |
| Oxygen index/% | ﹥25.0 | GB/T 2406-2009 | 31.5 | 32.1 | 30.6 | 31.0 |
| Vertical combustion | ﹥V-1 | GB/T 2408-2008 | V-0 | V-0 | V-0 | V-0 |
Claims (10)
1. halogen-free flameproof POE matrix material is characterized in that being processed by the component of following weight part:
100 parts of POE resins, 70～140 parts of Halogenless composite fire retardants, 5～30 parts of properties-correcting agent, 3～10 parts of lubrication dispersing agents, 0.1～0.6 part in oxidation inhibitor;
Said Halogenless composite fire retardant by active hydrogen Natural manganese dioxide/active aluminium hydroxide and zinc borate and microcapsule red phosphorus according to 100: (2～10): the weight ratio of (8～20) is formed.
2. halogen-free flameproof POE matrix material according to claim 1; It is characterized in that: described active hydrogen Natural manganese dioxide/active aluminium hydroxide is to be obtained by silane coupler modified micron order Marinco H/micron order white lake, and wherein the weight ratio of micron order Marinco H/micron order white lake and silane coupling agent is 100: 2～100: 4; Said micron order Marinco H/micron order white lake is meant that median size is Marinco H/white lake of 20 microns～200 microns.
3. halogen-free flameproof POE matrix material according to claim 1 is characterized in that: described properties-correcting agent is new LDPE (film grade) or high density polyethylene(HDPE).
4. halogen-free flameproof POE matrix material according to claim 1 is characterized in that: described lubrication dispersing agent is solid paraffin or polyethylene wax.
5. halogen-free flameproof POE matrix material according to claim 1 is characterized in that: described oxidation inhibitor is antioxidant 1010.
6. the preparation method of the described halogen-free flameproof POE of claim 1 matrix material is characterized in that having following steps:
1. will pour in the high-speed mixer according to POE resin, active hydrogen Natural manganese dioxide/active aluminium hydroxide, zinc borate, microcapsule red phosphorus, properties-correcting agent, lubrication dispersing agent and oxidation inhibitor that prescription takes by weighing and mix; Make temperature of charge be increased to 65 ℃～75 ℃ until mixing the heat of friction that is produced, the discharging cooling;
2. cooled mixture is sent in the twin screw extruder and melt extrudes, the billot of being extruded gets into the dicing machine granulation through tank cooling, traction, promptly gets halogen-free flameproof POE matrix material.
7. the preparation method of halogen-free flameproof POE matrix material according to claim 6; It is characterized in that: the active hydrogen Natural manganese dioxide/active aluminium hydroxide of step described in 1. is to be obtained by silane coupler modified micron order Marinco H/micron order white lake, and wherein the weight ratio of micron order Marinco H/micron order white lake and silane coupling agent is 100: 2～100: 4; Said micron order Marinco H/micron order white lake is meant that median size is Marinco H/white lake of 20 microns～200 microns.
8. the preparation method of halogen-free flameproof POE matrix material according to claim 7; It is characterized in that: the preparation method of said active hydrogen Natural manganese dioxide/active aluminium hydroxide is: according to proportioning micron order Marinco H/micron order white lake and silane coupling agent are poured into and mixed 5min～10min in the high-speed mixer; Make material temperature reach 110 ℃～120 ℃ until mixing the heat of friction that is produced, the discharging cooling promptly gets active hydrogen Natural manganese dioxide/active aluminium hydroxide.
9. the preparation method of halogen-free flameproof POE matrix material according to claim 6 is characterized in that: the properties-correcting agent of step described in 1. is new LDPE (film grade) or high density polyethylene(HDPE); Described lubrication dispersing agent is solid paraffin or polyethylene wax; Described oxidation inhibitor is antioxidant 1010.
10. the preparation method of halogen-free flameproof POE matrix material according to claim 6 is characterized in that: step 2. in, twin screw extruder each the district temperature be: T
1=80 ℃～85 ℃, T
2=100 ℃～110 ℃, T
3=130 ℃～140 ℃, T
4=150 ℃～160 ℃, T
5=160 ℃～170 ℃, T
6=170 ℃～180 ℃, T
7=170 ℃～180 ℃, T
8=170 ℃～180 ℃, T
9=160 ℃～165 ℃, T
Mould=155 ℃～160 ℃.
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| CN2012100490976A CN102585346A (en) | 2012-02-29 | 2012-02-29 | Halogen-free flame-retardant POE (Polyolefin Elastomer) compound material and preparation method thereof |
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Cited By (8)
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| CN103131114A (en) * | 2013-03-25 | 2013-06-05 | 上海交通大学 | Compound expansive flame-retardant thermoplastic elastomer composition and preparation method thereof |
| CN103131113A (en) * | 2013-03-25 | 2013-06-05 | 上海交通大学 | Halogen-free expanded flame-retardant thermoplastic elastomer composition and preparation method thereof |
| CN104194168A (en) * | 2014-08-26 | 2014-12-10 | 无锡杰科塑业有限公司 | Thermoplastic low-smoke zero-halogen flame-retardant polyolefin sheath material with high heat shock resistance and preparation method thereof |
| CN105419045A (en) * | 2015-11-27 | 2016-03-23 | 康平县塑编产业集群综合服务中心 | Halogen-free flame-retardant plastic weaving material and preparation method thereof |
| CN105504482A (en) * | 2013-09-29 | 2016-04-20 | 江苏理工学院 | Halogen-free flame-retardant linear low-density polyethylene material |
| CN105754200A (en) * | 2016-03-13 | 2016-07-13 | 贵州省材料产业技术研究院 | High-strength high-elasticity fiber reinforced POE (polyolefin elastomer) material and preparation method thereof |
| CN105778264A (en) * | 2014-08-11 | 2016-07-20 | 江苏理工学院 | Preparation method of halogen-free flame-retardant POE material |
| CN105860239A (en) * | 2014-08-11 | 2016-08-17 | 江苏理工学院 | Halogen-free flame-retardant POE material and preparation method thereof |
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| CN104194168A (en) * | 2014-08-26 | 2014-12-10 | 无锡杰科塑业有限公司 | Thermoplastic low-smoke zero-halogen flame-retardant polyolefin sheath material with high heat shock resistance and preparation method thereof |
| CN105419045A (en) * | 2015-11-27 | 2016-03-23 | 康平县塑编产业集群综合服务中心 | Halogen-free flame-retardant plastic weaving material and preparation method thereof |
| CN105754200A (en) * | 2016-03-13 | 2016-07-13 | 贵州省材料产业技术研究院 | High-strength high-elasticity fiber reinforced POE (polyolefin elastomer) material and preparation method thereof |
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Application publication date: 20120718 |