CN103694417B - A kind of politef and high density polyethylene (HDPE) are blended the preparation method of bulking agent - Google Patents
A kind of politef and high density polyethylene (HDPE) are blended the preparation method of bulking agent Download PDFInfo
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- CN103694417B CN103694417B CN201310730599.XA CN201310730599A CN103694417B CN 103694417 B CN103694417 B CN 103694417B CN 201310730599 A CN201310730599 A CN 201310730599A CN 103694417 B CN103694417 B CN 103694417B
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- 239000004700 high-density polyethylene Substances 0.000 title claims abstract description 37
- 238000002360 preparation method Methods 0.000 title claims abstract description 12
- 239000004067 bulking agent Substances 0.000 title claims abstract description 11
- 229950000845 Politef Drugs 0.000 title claims abstract description 10
- 239000000178 monomer Substances 0.000 claims abstract description 26
- 229910052799 carbon Inorganic materials 0.000 claims abstract description 18
- 239000004721 Polyphenylene oxide Substances 0.000 claims abstract description 17
- 229920000570 polyether Polymers 0.000 claims abstract description 17
- FPYJFEHAWHCUMM-UHFFFAOYSA-N Maleic anhydride Chemical compound O=C1OC(=O)C=C1 FPYJFEHAWHCUMM-UHFFFAOYSA-N 0.000 claims abstract description 9
- 229920001684 low density polyethylene Polymers 0.000 claims abstract description 9
- 239000004702 low-density polyethylene Substances 0.000 claims abstract description 9
- 238000006243 chemical reaction Methods 0.000 claims description 7
- CSCPPACGZOOCGX-UHFFFAOYSA-N acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims description 6
- 239000003999 initiator Substances 0.000 claims description 4
- 238000007664 blowing Methods 0.000 claims description 3
- 150000002978 peroxides Chemical class 0.000 claims description 3
- 238000003756 stirring Methods 0.000 claims 1
- 229920001903 high density polyethylene Polymers 0.000 abstract description 24
- 239000004810 polytetrafluoroethylene Substances 0.000 abstract description 11
- 229920001343 polytetrafluoroethylene Polymers 0.000 abstract description 11
- 230000000694 effects Effects 0.000 abstract description 6
- 238000002156 mixing Methods 0.000 abstract description 5
- 239000004698 Polyethylene (PE) Substances 0.000 abstract description 3
- 238000005253 cladding Methods 0.000 abstract description 3
- 229920000578 graft polymer Polymers 0.000 abstract description 3
- 229920000141 poly(maleic anhydride) Polymers 0.000 abstract description 3
- 229920000642 polymer Polymers 0.000 abstract description 3
- 239000003795 chemical substances by application Substances 0.000 abstract description 2
- 239000000463 material Substances 0.000 description 13
- 125000002023 trifluoromethyl group Chemical group FC(F)(F)* 0.000 description 9
- 229920003023 plastic Polymers 0.000 description 8
- 239000004033 plastic Substances 0.000 description 8
- 239000000203 mixture Substances 0.000 description 5
- 239000002808 molecular sieve Substances 0.000 description 4
- 125000000876 trifluoromethoxy group Chemical group FC(F)(F)O* 0.000 description 4
- 239000000956 alloy Substances 0.000 description 3
- 229910045601 alloy Inorganic materials 0.000 description 3
- REDXJYDRNCIFBQ-UHFFFAOYSA-N aluminium(3+) Chemical class [Al+3] REDXJYDRNCIFBQ-UHFFFAOYSA-N 0.000 description 3
- 230000003078 antioxidant Effects 0.000 description 3
- 239000003963 antioxidant agent Substances 0.000 description 3
- 229920000098 polyolefin Polymers 0.000 description 3
- 229920005989 resin Polymers 0.000 description 3
- 239000011347 resin Substances 0.000 description 3
- 239000000779 smoke Substances 0.000 description 3
- 229920001169 thermoplastic Polymers 0.000 description 3
- 239000004416 thermosoftening plastic Substances 0.000 description 3
- HBMJWWWQQXIZIP-UHFFFAOYSA-N Silicon carbide Chemical compound [Si+]#[C-] HBMJWWWQQXIZIP-UHFFFAOYSA-N 0.000 description 2
- RTZKZFJDLAIYFH-UHFFFAOYSA-N diethyl ether Chemical compound CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 description 2
- 239000000314 lubricant Substances 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 239000002245 particle Substances 0.000 description 2
- 229910010271 silicon carbide Inorganic materials 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 239000004342 Benzoyl peroxide Substances 0.000 description 1
- XMJCOTSQMHGIPF-SNSGICDFSA-N COPP protocol Chemical compound ClCCN(CCCl)P1(=O)NCCCO1.CNNCC1=CC=C(C(=O)NC(C)C)C=C1.O=C1C=C[C@]2(C)[C@H]3C(=O)C[C@](C)([C@@](CC4)(O)C(=O)CO)[C@@H]4[C@@H]3CCC2=C1.C([C@H](C[C@]1(C(=O)OC)C=2C(=C3C([C@]45[C@H]([C@@]([C@H](OC(C)=O)[C@]6(CC)C=CCN([C@H]56)CC4)(O)C(=O)OC)N3C=O)=CC=2)OC)C[C@@](C2)(O)CC)N2CCC2=C1NC1=CC=CC=C21 XMJCOTSQMHGIPF-SNSGICDFSA-N 0.000 description 1
- 241000196324 Embryophyta Species 0.000 description 1
- OMPJBNCRMGITSC-UHFFFAOYSA-N Incidol Chemical compound C=1C=CC=CC=1C(=O)OOC(=O)C1=CC=CC=C1 OMPJBNCRMGITSC-UHFFFAOYSA-N 0.000 description 1
- 210000001138 Tears Anatomy 0.000 description 1
- 230000002411 adverse Effects 0.000 description 1
- -1 alkyl vinyl ether Chemical compound 0.000 description 1
- 238000005452 bending Methods 0.000 description 1
- 235000019400 benzoyl peroxide Nutrition 0.000 description 1
- 125000004432 carbon atoms Chemical group C* 0.000 description 1
- 125000002915 carbonyl group Chemical group [*:2]C([*:1])=O 0.000 description 1
- 239000000460 chlorine Substances 0.000 description 1
- 229910052801 chlorine Inorganic materials 0.000 description 1
- ZAMOUSCENKQFHK-UHFFFAOYSA-N chlorine atom Chemical compound [Cl] ZAMOUSCENKQFHK-UHFFFAOYSA-N 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 239000007822 coupling agent Substances 0.000 description 1
- 238000005336 cracking Methods 0.000 description 1
- 239000002270 dispersing agent Substances 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 239000005038 ethylene vinyl acetate Substances 0.000 description 1
- 239000003063 flame retardant Substances 0.000 description 1
- 229910052731 fluorine Inorganic materials 0.000 description 1
- 239000011737 fluorine Substances 0.000 description 1
- YCKRFDGAMUMZLT-UHFFFAOYSA-N fluorine atom Chemical compound [F] YCKRFDGAMUMZLT-UHFFFAOYSA-N 0.000 description 1
- 239000008187 granular material Substances 0.000 description 1
- 238000007731 hot pressing Methods 0.000 description 1
- 239000001257 hydrogen Substances 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- 125000004435 hydrogen atoms Chemical class [H]* 0.000 description 1
- 239000003112 inhibitor Substances 0.000 description 1
- 230000002401 inhibitory effect Effects 0.000 description 1
- 230000001050 lubricating Effects 0.000 description 1
- 239000012528 membrane Substances 0.000 description 1
- 238000000465 moulding Methods 0.000 description 1
- 230000003000 nontoxic Effects 0.000 description 1
- 231100000252 nontoxic Toxicity 0.000 description 1
- 229920001200 poly(ethylene-vinyl acetate) Polymers 0.000 description 1
- 238000006116 polymerization reaction Methods 0.000 description 1
- 229920000915 polyvinyl chloride Polymers 0.000 description 1
- 239000000843 powder Substances 0.000 description 1
- 230000001172 regenerating Effects 0.000 description 1
- 229920002545 silicone oil Polymers 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 238000001228 spectrum Methods 0.000 description 1
- 125000000391 vinyl group Chemical group [H]C([*])=C([H])[H] 0.000 description 1
- 238000010792 warming Methods 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
Abstract
A kind of politef and high density polyethylene (HDPE) are blended the preparation method of bulking agent and the invention provides a kind of politef and high density polyethylene (HDPE) the preparation method of bulking agent is blended: introduce the carbon perfluoroalkyl polyether monomer PAVE of a small amount of band double bond on maleic anhydride grafting Low Density Polyethylene compatilizer HDPE g MAH, generate polymaleic anhydride and the graft copolymer HDPE/MAH/PAVE of 2 kinds of monomer surface cladding high density polyethylene (HDPE)s of carbon perfluoroalkyl polyether, can be as compatilizer to improve the compatibility of PE/PTFE polymer.Compatibilization effect is better than the HDPE g MAH effect as Interfacial compatibilization agent, and PTFE/HDPE co-mixing system sufficiently can contact during being pulverized and mixed, scattered evenly.
Description
Technical field
The present invention relates to a kind of politef and high density polyethylene (HDPE) and the preparation method of bulking agent is blended.
Background technology
Resin material has the electric insulating quality of prominent physical and mechanical properties and chemical stability and excellence, has purposes widely in fields such as agricultural, national defense industry.And the HDPE used as tubing uses with the resistance to variations in temperature of its excellence, wear-resistant, corrosion-resistant, nontoxic, light weight, inexpensive, finished product manufacture and installs the favor day by day by people of the excellent properties such as the simple low cost of maintenance program.HDPE usage amount in every respect is very big at present, almost penetrates into the every aspect of life, the particularly application in terms of tubing and has reached the second of plastic pipe usage amount, is only only second to PVC.But, there are some more open defects in HDPE material in performance, especially it is in terms of physical and mechanical property, and as hot strength is on the low side, intensity is relatively low, and environmental stress cracking resistance is poor, and impact strength is low, and bending strength is low etc. limits its use.It addition, HDPE tubing can not bear higher operating pressure, therefore its wall thickness is the most made the thickest to increase ability to bear.HDPE material is modified the deficiency being to overcome it on properties, the defect that especially toughness is little, and then expands its range of application.
CN102382352 provides composition of HDPE/POE-g-MAH/ mesopore molecular sieve intermingling material and preparation method thereof, following compositions be configured to according to mass ratio: HDPE50%-60%, mesopore molecular sieve 30%-40%, POE-g-MAH10%, antioxidant (1010) 0.15%, lubricant (OPE) 0.15%.The shortcoming such as what the present invention can effectively solve in use to occur be such as easily deformed, easily rupturable, service life is short.The addition of self-control POE-g-MAH is a certain degree of improves the tear phenomenon in use produced not due to toughness, and the addition of lubricant OPE improves the processing characteristics of HDPE/POE-g-MAH/ mesopore molecular sieve intermingling material.Can be used for HDPE (high density polyethylene (HDPE))/RHDPE (the regenerative high-density polyethylene)/POE-g-MAH/ mesopore molecular sieve intermingling material of the engineering plastics such as tubing.
CN102101922 discloses a kind of wear-resistant thermoplastic resistance halogen-free low-smoke expansion flame-retarding polyolefin sheath plastic and preparation method thereof, component including following parts by weight: vistanex 50-80 part, compounding resin 0-20 part, grafted material 3-15 part, halogen-free expansion fire retardant 10-60 part, coupling agent 0.5-3 part, antioxidant 0.5-1.5 part, nanometer silicon carbide 1-10 part.Thermoplastic halogen-free and low-smoke expansion type flame-proof polyolefin sheathed plastic of the present invention and preparation method thereof, nanometer silicon carbide is added in co-mixing system, improve the wearability of thermoplastic halogen-free and low-smoke expansion type flame-proof polyolefin sheathed plastic, disclosure satisfy that the normal use demand under adverse circumstances, and improve its service life.Described grafted material is one or more in polyolefin-maleic anhydride grafted material, ethylene-vinyl acetate copolymer, HOPP or COPP.
Owing to the chemical stability of politef is good, coefficient of friction low (coefficient of friction=0.05), PTFE and HDPE melt blending can be used to the self-lubricating material developing suitable platform needed for cable protection sleeve pipe, but owing to structure and the polarity spectrum of HDPE and PTFE are bigger, thus the compatibility between the two is less, the performance of co-mixing system can be caused during simple blend significantly to decline, add polyolefin-maleic anhydride grafted material and can partly improve the compatibility, but poor compatibility between high molecular polymer, mix the shortcoming such as uneven still can not to solve at all, have impact on the using effect in commercial plant.
Summary of the invention
For the deficiencies in the prior art, the invention provides a kind of politef and high density polyethylene (HDPE) and the preparation method of bulking agent is blended.
In a kettle., squeeze into pure water, polymerization inhibitor, add a certain amount of dispersant, initiator, maleic anhydride grafting Low Density Polyethylene compatilizer HDPE-g-MAH, carbon perfluoroalkyl polyether monomer PAVE, being warming up to reaction temperature, question response terminates. and dry closing bag, obtain this patent product powder body.
The present invention introduces the carbon perfluoroalkyl polyether monomer PAVE of a small amount of band double bond on maleic anhydride grafting Low Density Polyethylene compatilizer HDPE-g-MAH, generate polymaleic anhydride and the graft copolymer HDPE/MAH/PAVE of 2 kinds of monomer surface cladding high density polyethylene (HDPE)s of carbon perfluoroalkyl polyether, can be as compatilizer to improve the compatibility of PE/PTFE polymer.
The present invention provides a kind of politef and high density polyethylene (HDPE) that the preparation method of bulking agent is blended, and is realized by following steps:
By weight, 300-1000 part (preferably 500 parts) acetone is added in a kettle., by 100 parts of maleic anhydride grafting Low Density Polyethylene compatilizer HDPE-g-MAH, 0-20 part (preferably 8 parts) carbon perfluoroalkyl polyether monomer PAVE mixes, and adds 0.05-1 part peroxide initiator (preferably 0.2 part), stirs.Then from 60-100 DEG C of (preferably 80 DEG C) temperature reaction 10-15h (preferably 10h), reaction terminates rear blowing, dries and obtains this patent product.
Described maleic anhydride grafting Low Density Polyethylene compatilizer can use commercially available prod, such as: the JX-3 maleic anhydride grafting Low Density Polyethylene compatilizer that Nanjing multiple star macromolecular material company limited produces.
The preferred benzoyl peroxide of described peroxide initiator.
Described carbon perfluoroalkyl polyether monomer structure formula is as follows:
XCF2CF2(OCFXCF2)nOCF=CF2
In carbon perfluoroalkyl polyether formula, X is the member of a class, including fluorine, chlorine, hydrogen, chlorodifluoramethyl-and perfluoro-methyl, n is at least one in an integer, the summation of at least two is 1, p be at least one of integer be an integer, the total ether of the carbon atom in vinyl be less than 24.
As: CF3OCF2CF2CF2OCF=CF2、CF3CF2CF2OCF2CF2CF2OCF=CF2、CF3(OCF2CF2CF2)2OCF=CF2、CF3CF2CF2(OCF2CF2CF2)2OCF=CF2、CF3(OCF2CF2CF2)3OCF=CF2、CF3CF2CF2(OCF2CF2CF2)3OCF=CF2、CF3(OCF2CF2CF2)4OCF=CF2、CF3CF2CF2(OCF2CF2CF2)4OCF=CF2。CF3(OCF2CF2)3OCF=CF2、CF3OCF2OCF2CF2OCF=CF2、CF3O(CF2O)2CF2CF2OCF=CF2、CF3O(CF2O)4CF2CF2OCF=CF2、CF3O(CF2O)3CF2CF2OCF=CF2、CF3O(CF2O)5CF2CF2OCF=CF2、CF3CF2CF2OCF2OCF=CF2、CF3CF2OCF2OCF=CF2Deng.It is optimized for: CF3CF2CF2(OCF2CF2CF2)3OCF=CF2、CF3(OCF2CF2CF2)4OCF=CF2、CF3OCF2OCF2CF2OCF=CF2。
Beneficial effects of the present invention:
1) polymaleic anhydride and the graft copolymer of 2 kinds of monomer surface cladding high density polyethylene (HDPE)s of carbon perfluoroalkyl polyether
HDPE/MAH/PAVE is as bulking agent, and compatibilization effect is better than the HDPE-g-MAH effect as Interfacial compatibilization agent, and PTFE/HDPE co-mixing system sufficiently can contact during being pulverized and mixed, scattered evenly.
2) introducing of many carbonyls in alkyl vinyl ether, makes PTFE/HDPE blend intermolecular polarity improve, makes interfacial friction factor reduce.
Detailed description of the invention
Following example only further illustrate the present invention, are not to limit the scope of protection of the invention.
The present invention provides a kind of politef and high density polyethylene (HDPE) that the preparation method of bulking agent is blended, and is realized by following steps:
JX-3 maleic anhydride grafting Low Density Polyethylene compatilizer, Nanjing multiple star macromolecular material company limited produces.
By weight, 500 parts of acetone of interior addition in a kettle., by 100 parts of JX-3 maleic anhydrides grafting Low Density Polyethylene compatilizers, 8 parts of CF3CF2CF2(OCF2CF2CF2)3OCF=CF2Monomer mixes, and adds 0.2 part of peroxide benzoyl, stirs.80.Reaction 10-h, reaction terminates rear blowing, dries, obtains this patent product. numbered SX-1.
Embodiment 2
CF3CF2CF2(OCF2CF2CF2)3OCF=CF2Monomer weight number is 20 parts, and the other the same as in Example 1 obtains this patent product.Numbered SX-2.
Embodiment 3
CF3CF2CF2(OCF2CF2CF2)3OCF=CF2Monomer weight number is 5 parts, and the other the same as in Example 1 obtains this patent product.Numbered SX-2.
Embodiment 4
Carbon perfluoroalkyl polyether monomer PAVE monomer selects CF3(OCF2CF2CF2)4OCF=CF2, the other the same as in Example 1.The numbered SX-4 of products obtained therefrom.
Embodiment 5
Carbon perfluoroalkyl polyether monomer PAVE monomer selects CF3(OCF2CF2CF2)4OCF=CF2, the other the same as in Example 2.The numbered SX-5 of products obtained therefrom.
Embodiment 6
Carbon perfluoroalkyl polyether monomer PAVE monomer selects CF3(OCF2CF2CF2)4OCF=CF2, the other the same as in Example 3.The numbered SX-6. of products obtained therefrom
Embodiment 7
Carbon perfluoroalkyl polyether monomer PAVE monomer selects CF3OCF2OCF2CF2OCF=CF2, the other the same as in Example 1.The numbered SX-7. of products obtained therefrom
Embodiment 8
Carbon perfluoroalkyl polyether monomer PAVE monomer selects CF3OCF2OCF2CF2OCF=CF2, the other the same as in Example 2.The numbered SX-8. of products obtained therefrom
Embodiment 9
Carbon perfluoroalkyl polyether monomer PAVE monomer selects CF3OCF2OCF2CF2OCF=CF2, the other the same as in Example 3.The numbered SX-9. of products obtained therefrom
. embodiment 10
CF3CF2CF2(OCF2CF2CF2)3OCF=CF2Monomer weight number is 0 part, the other the same as in Example 1.The numbered SX-10. of products obtained therefrom
Embodiment 11
84.7%wtHDPE, 5%wt HDPE/MAH/PAVE bulking agent, 10%wt PTFE is added in high-speed mixer, 0.15%wt antioxidant, practices molding machine 150 DEG C at double rollers and begins to pratise, add the nucleator of 0.15%wt, at 180 DEG C, hot pressing film-making under the conditions of 50MPa, detects coefficient of friction.
(it is auspicious that coefficient of friction presses document Ling Jing, Lin Jianqing, Zhao Xihua. development [J] Xiamen University journal (natural science edition) .2001 of silicone oil/HDPE self-lubricating cable protection sleeve pipe, method described in 40 (5): 1090-1094 measures)
| Production code member | Coefficient of friction |
| SX-1 | 0.17 |
| SX-2 | 0.14 |
| SX-3 | 0.18 |
| SX-4 | 0.15 |
| SX-5 | 0.12 |
| SX-6 | 0.17 |
| SX-7 | 0.16 |
| SX-8 | 0.16 |
| SX-9 | 0.19 |
| SX-10 | 0.27 |
| HDPE resin | 0.33 |
Because fusing point difference is bigger, PTFE not meltedization at such a temperature, it it is still solid particle, PTFE particle is distributed in " island structure " in plastic alloy, friction between rubbing surface and plastic alloy, actually rubbing surface with expose that " these " islands " being made up of PE granule on sea level contact; so frictional force between the two can be substantially reduced .HDPE/MAH/PAVE has double membrane structure; form one layer of antifriction lubricating layer on rubbing surface, make PTFE/HDPE plastic alloy have good self-lubricating property.
Claims (1)
1. a politef and high density polyethylene (HDPE) are blended the preparation method of bulking agent, it is characterised in that include with
Lower step:
By weight, interior addition 300-1000 part acetone in a kettle., by 100 parts of maleic anhydrides grafting
Low Density Polyethylene compatilizer, 5-20 part carbon perfluoroalkyl polyether monomer, this carbon perfluoroalkyl polyether monomer is that molecular formula is
CF3CF2CF2(OCF2CF2CF2)3OCF=CF2、CF3(OCF2CF2CF2)4OCF=CF2、CF3OCF2OCF2CF2OCF=
CF2In one, add 0.05-1 part peroxide initiator, stir, then from 60-100 DEG C
Temperature reaction 10-15h, reaction terminates rear blowing, dries and obtains product.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201310730599.XA CN103694417B (en) | 2013-12-14 | A kind of politef and high density polyethylene (HDPE) are blended the preparation method of bulking agent |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201310730599.XA CN103694417B (en) | 2013-12-14 | A kind of politef and high density polyethylene (HDPE) are blended the preparation method of bulking agent |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN103694417A CN103694417A (en) | 2014-04-02 |
| CN103694417B true CN103694417B (en) | 2016-11-30 |
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Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1526756A (en) * | 2003-03-05 | 2004-09-08 | 扬子石油化工股份有限公司 | Permanent self-lubricating polyolefin composition and its prepn |
| CN102101922A (en) * | 2009-12-22 | 2011-06-22 | 上海新上化高分子材料有限公司 | Wear-resistance halogen-free low-smoke expansion flame-retarding polyolefin sheath plastic and preparation method thereof |
| CN102382352A (en) * | 2011-10-24 | 2012-03-21 | 沈阳化工大学 | Composition of HDPE/POE-g-MAH/mesoporous molecular sieve blended material and preparation method thereof |
| CN102585338A (en) * | 2011-01-13 | 2012-07-18 | 苏州汉扬精密电子有限公司 | Anti-wear halogen-free flame-retardant cable material |
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1526756A (en) * | 2003-03-05 | 2004-09-08 | 扬子石油化工股份有限公司 | Permanent self-lubricating polyolefin composition and its prepn |
| CN102101922A (en) * | 2009-12-22 | 2011-06-22 | 上海新上化高分子材料有限公司 | Wear-resistance halogen-free low-smoke expansion flame-retarding polyolefin sheath plastic and preparation method thereof |
| CN102585338A (en) * | 2011-01-13 | 2012-07-18 | 苏州汉扬精密电子有限公司 | Anti-wear halogen-free flame-retardant cable material |
| CN102382352A (en) * | 2011-10-24 | 2012-03-21 | 沈阳化工大学 | Composition of HDPE/POE-g-MAH/mesoporous molecular sieve blended material and preparation method thereof |
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