CN103172937B - A kind of Silane Grafted PPR pipe PP Pipe Compound and preparation method thereof - Google Patents
A kind of Silane Grafted PPR pipe PP Pipe Compound and preparation method thereof Download PDFInfo
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- CN103172937B CN103172937B CN201310125917.XA CN201310125917A CN103172937B CN 103172937 B CN103172937 B CN 103172937B CN 201310125917 A CN201310125917 A CN 201310125917A CN 103172937 B CN103172937 B CN 103172937B
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
- B29C—SHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
- B29C48/00—Extrusion moulding, i.e. expressing the moulding material through a die or nozzle which imparts the desired form; Apparatus therefor
- B29C48/03—Extrusion moulding, i.e. expressing the moulding material through a die or nozzle which imparts the desired form; Apparatus therefor characterised by the shape of the extruded material at extrusion
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Abstract
The invention discloses a kind of Silane Grafted PPR pipe PP Pipe Compound, expect that the ratio in 90: 10 ~ 95: 5 forms by A material and B by weight; A material consists of: PPR80 ~ 95, high density polyethylene(HDPE) 5 ~ 20, unsaturated silane 1-3, initiator 0.01-0.03, oxidation inhibitor 0.1-0.5, auxiliary crosslinking agent 0.1-2; B material consists of: PPR100, catalyzer 1-3, oxidation inhibitor 0.1-0.5, cocatalyst 1-5.Preparation method is A material and B material separately separately extruding pelletization, then A material and B expect in proportion compounding even after, namely can be used for direct extruding pipe material.Material resistance to impact shock of the present invention, creep resistance are good, can be widely used in the various duct products such as hot water pipe.Preparation method is simple, without the need to long-time high temperature poach process, is convenient to suitability for industrialized production application.
Description
Technical field
The invention belongs to PPR pipe field, be specifically related to a kind of Silane Grafted PPR pipe PP Pipe Compound and preparation method thereof.
Background technology
PPR pipe road product is made up of atactic copolymerized polypropene.It is after crosslinked polyethylene, polybutene tubing, another novel thermoplastic plastic pipe.The pipeline produced by PPR, have that quality is light, resistance toheat good, heat conductivility is lower, Young's modulus is less, the resistance of ducting is little, health, corrosion-resistant, long service life, easy for installation, connect the features such as reliable and material recoverable, various hot water pipe can be widely used in.But existing PPR pipe road also comes with some shortcomings, and mainly contains: rigidity and erosion-resisting characteristics poorer than metallic conduit, coefficient of linear expansion is comparatively large, and construction is easily broken, and creep properties is larger.Particularly because PPR pipe material molecule is linear structure, comparatively speaking the rigidity of PPR pipe and shock resistance poor.For meeting the different requirements of different goods to PPR performance, to overcome the deficiency existing for PPR pipe, someone has done a large amount of research work, but mainly concentrates on the aspects such as blending and modifying, whisker modified enhancing and thermal treatment.Such as:
Application number is the Chinese invention patent application disclosed " polypropene composition and tubing thereof " of CN99119655.4, said composition is mixed in the proper ratio by polymer grade polypropylene, chemical degradation polypropylene, polypropylene, ethylene/alpha-olefin copolymer, adds appropriate amount of addition agent (as stablizer, flow ability modifying agent, dispersion agent, tinting material etc.) composition.Adopt said composition by melt extruding the thin-walled property that can realize tubing, the wall thickness of this tubing, between 0.1-10mm, is applicable to the tubing of all size of water-saving irrigation system.
Application number is the Chinese invention patent application of CN200510017644.2 disclosed " polypropene composition and the method with said composition production modified polypropylene pipes ", a kind of polypropene composition of this disclosure of the invention, and the method for producing the whisker modified fiberglass reinforced polypropylene pipe of heat supply heating by said composition.In units of weight part, it is by polypropylene 50 ~ 100 parts, whisker 10 ~ 50 parts, lubricant 0.5 ~ 5 part, compound before the granulation of coupling agent 0.5 ~ 10 part composition, compound high-speed mixer is mixed, oven dry is placed on extruding pelletization in dual-screw-stem machine and forms combination pellet, a certain amount of polypropylene is rejoined, the polypropylene rejoined: combination pellet=1: 0.5 ~ 3, mixes with high-speed mixer again in combination pellet, be placed in single-screw machine, heating extruding pipe material, through Vacuum shaping, cooling and traction, forms the tubing of required specification.The fields such as applicable delivering hot water, geothermal heating are claimed in this invention, not only can improve heat resisting temperature, but also can increase the service life.
Application number is the Chinese invention patent application disclosed " special-purpose multifunctional modified random polypropylene material for pipe and preparation method thereof " of CN200710030073.5, and this PP Pipe Compound is made up of atactic copolymerized polypropene, environmental protection fire retarding agent, the pre-dispersed masterbatch of mineral filler, anti-impact modifier, oxidation inhibitor, composite antibacterial masterbatch and dispersion agent.This invention also discloses the application of special-purpose multifunctional modified random polypropylene material for pipe in the irrigation system in cold and hot water building pipe, tap water and foodstuffs industry tubing system, floor heating and traditional heat supply heating system, farmland.This invention claims that the special material for tube of preparation has flame-proof antibiotic function, solve atactic copolymerized polypropene simultaneously and shrink large, that low temperature impact properties is poor problem, there is higher resistance toheat and fabulous mechanical property, and there is excellent thermostability, there is good anti-contracility and low temperature resistance property.
Application number is the Chinese invention patent application disclosed " a kind of composite auxiliary agent for random copolymerized polypropylene pipe material " of CN200810117477.2, this invention relates to a kind of composite auxiliary agent for random copolymerized polypropylene pipe material be polymerized through liquid phase noumenal method single loop reactors, forms by weight by compound system is composite: resisting ageing for long time performance aids 10 ~ 40 parts, processing aid 10 ~ 30 parts, compound modifying agent 20 ~ 50 parts and weather resisting agent 10 ~ 30 parts; Resisting ageing for long time performance aids is lactone stabilizer, Hinered phenols antioxidant and nontoxic amine antioxidants compound system; Processing aid is a kind of in fluoroelastomer or low-molecular(weight)polymer or mixture that any proportioning is several; Weather resisting agent is UV light absorber, organic nickel stablizer and hindered amines stabilizer compound system in photostabilizer; Compound modifying agent is the compound modifying agent that alpha-crystal form is converted into beta crystal.This invention is claimed and the processing characteristics of atactic copolymerized polypropene resin, mechanical property and environmental stress cracking resistance and resisting ageing for long time performance can be made to significantly improve.
Application number is the Chinese invention patent application disclosed " a kind of method of improving low-temperature impact resistance of random copolymerization polypropylene pipe " of CN201110335949.3, this invention comprises the processing of random copolymerization polypropylene pipe, random copolymerization polypropylene pipe is put into and is dried car, thermal treatment, taking-up cooling, inspection, thermal treatment is divided into three steps: one at the uniform velocity rises to 90 DEG C by room temperature, and the heating-up time is 20min; Two at the uniform velocity rise to 105-110 DEG C by 90 DEG C, and the heating-up time is 30min; Three under 105-110 DEG C of condition, thermal treatment 100-120min.This invention is claimed, by adopting above-mentioned technology, improve random copolymerization polypropylene pipe low-temperature impact resistance qualification rate, reducing production cost, improve economic benefit.Improve more than five times through this invention heat treated random copolymerization polypropylene pipe falling ball impact test at low temperature serviceability rate, impact serviceability rate and reach 8/10 ~ 10/10, but also improve the compressive strength of tubing, compatible effective unification of toughness and intensity.
Application number is the Chinese invention patent application disclosed " a kind of polyacrylic special material for tube " of CN201110439863.5, and this PP Pipe Compound is made up of copolymerization grade polypropylene, water-ground limestone, glass microballon, oxidation inhibitor.This invention claims that the tubing produced by this PP Pipe Compound is compared with plain polypropylene tubing, when other performances are constant, its heat-drawn wire can improve 20-30 DEG C, the rigidity of tubing improves greatly, its hardness can improve more than 1.5 times, linear expansivity reduces 30-40%, due to the raising of heat-drawn wire, expands the range of application of polypropylene pipe; Due to the raising of hardness, can reduce the quantity of suspension and support when built on stilts laying, due to the reduction of the coefficient of expansion, the impact of in use being expanded with heat and contract with cold reduces simultaneously, can reduce the consumption of loop expansion pipe.
The present inventor notices, the rigidity of PPR pipe is relative with shock resistance poor, and its basic reason is that PPR pipe molecule is linear structure.Meanwhile, the present inventor recognizes after the molecular change of linear structure reticulates structure, and the rigidity of polymer materials, resistance toheat, creep-resistant property and intensity all will significantly improve.The patent No. is the preparation method that the Chinese patent of ZL02151548.4 discloses a kind of Silane Grafted hdpe pipe.After polymkeric substance crosslinked with silicane, improve the mechanical property of material.But contriver finds: although PE and PP is under the effect of initiator, Silane Grafted reaction mechanism is the same, but the chemical reaction that PPR and PE occurs is different, PPR easily degrades under initiator effect, and PE can not degrade, the degraded of PPR has a negative impact to the mechanical property of tubing, and the technology that therefore cannot directly adopt this patent to point out is to improve the performance of PPR.
Summary of the invention
An object of the present invention is the Silane Grafted PPR pipe PP Pipe Compound providing a kind of shock strength good.
Two of object of the present invention is the preparation method providing a kind of Silane Grafted PPR pipe PP Pipe Compound.
By A material and B, Silane Grafted PPR pipe PP Pipe Compound of the present invention, expects that the ratio in 90: 10 ~ 95: 5 forms with parts by weight; Wherein
A material consists of: PPR80 ~ 95 weight part, high density polyethylene(HDPE) 5 ~ 20 weight part, unsaturated silane 1-3 weight part, initiator 0.01-0.03 weight part, oxidation inhibitor 0.1-0.5 weight part, auxiliary crosslinking agent 0.1-2 weight part; Described auxiliary crosslinking agent is stearic acid, oxystearic acid, PE-g-MAH(maleic anhydride grafted polyethylene), PP-g-MHA(maleic anhydride inoculated polypropylene) or the mixture of at least two kinds in them;
B material consists of: PPR100 weight part, catalyzer 1-3 weight part, oxidation inhibitor 0.1-0.5 weight part, cocatalyst 1-5 weight part; Wherein, described catalyzer is dibutyl tin laurate, tin dilaurate dioctyl tin, Phenylsulfonic acid or the mixture of at least two kinds in them; Described cocatalyst is metal oxide.
Described metal oxide is zinc oxide, calcium oxide or their mixture.
The melt index of the PPR used in described A material is less than 0.5g/10min (230 DEG C, 2.16kg).
The melt index of the high density polyethylene(HDPE) used in described A material is 2-5g/10min (190 DEG C, 2.16kg).
Described unsaturated silane is vinyltriethoxysilane, vinyltrimethoxy silane, vinyl front three Ethoxysilane or the mixture of at least two kinds in them.
Described initiator is peroxide initiator, as dicumyl peroxide, tert-butyl peroxide-3,5,5 Trimethylhexanoic acid ester or the mixture etc. of the two.
The oxidation inhibitor used in described A material is phosphite ester kind antioxidant, such as irgasfos 168.
The melt index of the PPR used in described B material is less than 0.5g/10min (230 DEG C, 2.16kg).
The oxidation inhibitor used in described B material is dihydroxyphenyl propane class, phosphite ester kind antioxidant or their mixture, as antioxidant 1010, irgasfos 168 etc. or their mixture.
The preparation method of Silane Grafted PPR pipe PP Pipe Compound of the present invention, A material and B material independent extruding pelletization separately, respectively comprises the following steps:
The preparation of A material:
After unsaturated silane and initiator being weighed in proportion, be fully uniformly mixed in airtight stainless steel mixing tank, the temperature of mixing tank controls between 23-27 DEG C, mixes rear for subsequent use;
Take PPR, high density polyethylene(HDPE), oxidation inhibitor and auxiliary crosslinking agent in proportion and put into mixing machine, stir fully; Then add the unsaturated silane mixed and initiator mixture gradually, stir fully and obtain initial formulation;
Initial formulation directly joins in parallel dual-screw extruding machine and carries out grafting granulation processing;
Forcing machine design temperature is by charging opening to mouth mould successively raised temperature 5-10 DEG C gradually, and the processing temperature of whole forcing machine controls at 110-230 DEG C;
It is 2-3 minute that the engine speed of forcing machine controls in the material residence time in an extruder;
The vacuum tightness of the vacuum extraction of forcing machine should lower than-0.08MPa;
A expects granulation final vacuum packed for standby use;
The preparation of B material:
Take PPR, catalyzer, oxidation inhibitor and cocatalyst in proportion, put into mixing machine, the temperature of mixing machine controls at 30-40 DEG C, and the material after mixing fully directly enters twin screw extruder granulation, and the temperature of forcing machine controls at 110-230 DEG C;
B expects granulation final vacuum packed for standby use;
A material and B material in proportion compounding even after, namely can be used for direct extruding pipe material.
PPR is the macromolecular material of ethene, propylene random copolymerization, and molecular structure is structure linearly.Under the macromolecular material of linear structure is subject to external load, molecule can Relative sliding, causes the mechanical property of material to reduce.And in PPR molecule, there is a large amount of tertiary carbons and a small amount of unsaturated double-bond, the H on polymer molecule tertiary carbon atom or a small amount of C=C double bond issue biochemical reaction in the effect of peroxide initiator, produce free radical.The free radical that this free radical and insatiable hunger silane double bond produce reacts, and obtains Silane Grafted PPR and expects.
But under the effect of peroxide initiator, PPR can generating portion degrade, and the mechanical property making PPR expect reduces.In order to overcome this problem, the present invention introduces a small amount of high density polyethylene(HDPE) in the composition, is used for making up the defect of PPR mechanical properties decrease because of degraded, improves macro property and the working (machining) efficiency of PPR pipe.The introducing of high density polyethylene(HDPE), also improves the percentage of grafting of material, thus improves the degree of crosslinking of PPR pipe.The present invention simultaneously, in grafting A expects, except employing aforesaid catalyzer, also introduces auxiliary crosslinking agent, is conducive to the percentage of grafting improving PPR material.In catalysis B expects, introduce cocatalyst, be conducive to the rate of crosslinking improving PPR material.Owing to present invention employs these technology aforesaid, Silane Grafted PPR at room temperature just can be cross-linked, for Chinese patent CN02151548.4, do not need the poach process of long term time, within very short time, just reach the degree of crosslinking of needs, thus make the technology of the present invention greatly reduce material preparation cost and simplify technique.
And after the molecular change of linear structure reticulates structure, the rigidity of polymer materials, resistance toheat, creep-resistant property and intensity all significantly improve.After polymkeric substance crosslinked with silicane, improve the mechanical property of material, so adopt Silane Grafted technology to make PPR pipe material generating network structure, thus the macro property of PPR pipe can be improved, reduce its coefficient of linear expansion.
Embodiment
The invention will be further described by the following examples.
In the embodiment of the present invention, the preparation method of each embodiment is as follows:
All adopt the preparation were established of two-step approach.Namely adopt two-step approach to prepare Silane Grafted PPR respectively and expect that (A material) and crosslinked with silicane catalysis PPR expect (B material).
The preparation method of A material:
After unsaturated silane and initiator being weighed in proportion, in airtight stainless steel mixing tank, be fully uniformly mixed about 5-10 minute, the temperature of mixing tank controls between 23-27 DEG C, mixes rear for subsequent use.
Take PPR, high density polyethylene(HDPE), oxidation inhibitor and auxiliary crosslinking agent in proportion and put into high-speed mixer, the rotating speed of high-speed mixer controls at 50-100 rev/min, stirs 8-10 minute.Then add the unsaturated silane mixed and initiator mixture gradually, now the rotating speed of mixing machine controls at 200-300 rev/min, stirs and obtains initial formulation after 3-5 minute.
Initial formulation directly joins in parallel dual-screw extruding machine and carries out grafting granulation processing.The technical parameter of parallel dual-screw extruding machine:
The length-to-diameter ratio (L/D) of forcing machine is at (40-52): between 1.
The heating zone number of forcing machine should between 12-16 section.
Vacuum extraction mouth is opened in 9-10 heating zone.
The working process parameter of parallel dual-screw extruding machine:
Forcing machine design temperature is by charging opening to mouth mould successively raised temperature 5-10 DEG C gradually, and the processing temperature of whole forcing machine controls at 110-230 DEG C.
It is 2-3 minute that the engine speed of forcing machine controls in the material residence time in an extruder.
The vacuum tightness of the vacuum extraction of forcing machine should lower than-0.08MPa.
A material adopts water cooling granulation in granulation process, after granulation after 50-70 DEG C of vacuum-drying 30-60 minute, and aluminium plastic bag vacuum packaging.
The preparation method of B material:
Take PPR, catalyzer, oxidation inhibitor and cocatalyst in proportion, put into high-speed mixer, the rotating speed of mixing machine controls at 200-300 rev/min.The temperature of mixing machine controls at 30-40 DEG C.Mixing time is 10-15 minute.Mixed material directly enters twin screw extruder, and the temperature of forcing machine controls at 110-230 DEG C.
B material adopts water cooling granulation in granulation process, after granulation after 50-70 DEG C of vacuum-drying 30-60 minute, and aluminium plastic bag vacuum packaging.
A material and B material in proportion compounding even after, direct extruding pipe material.
The chemical constitution of the embodiment of the present invention tubing prepared as stated above and performance are in table 1.
Testing method illustrates:
1. gel content: ASTM D2655-1995;
2. shock strength: GB/T1843-1996;
3. drop impact experiment: GB/T11548-1989.
Typical starting material are:
A expects:
PPR:R4220 Sinopec yanshan petrochemical limited-liability company.
High density polyethylene(HDPE): 5000S Sinopec yanshan petrochemical limited-liability company.
Vinyltriethoxysilane: KBM-1003 Japan XINYUE.
Initiator: dicumyl peroxide (DCP) Lanzhou auxiliary reagent factory.
Oxidation inhibitor: the 168 rich Chemical Co., Ltd.s of Linyi City three.
Auxiliary crosslinking agent: polite company of stearic acid SA1810 Indonesia.
B expects:
PPR:R4220 Sinopec yanshan petrochemical limited-liability company.
Catalyzer: linear alkyl benzene sulphonic acid LABSA Henan Xing Ya tensio-active agent limited-liability company.
Oxidation inhibitor: the 1010 rich Chemical Co., Ltd.s of Linyi City three.
Cocatalyst: nano zine oxide Linan Bao Xinxin industry company limited.
As can be seen from Table 1, the excellent property of PPR pipe PP Pipe Compound of the present invention.The shock strength of tubing prepared therefrom significantly improves, and ageing-resistant performance significantly improves, and low temperature resistant drop impact performance is also significantly improved.
The composition and performance (in table 1, material consists of weight part) of table 1 embodiment of the present invention and comparative example
The composition and performance (continuous 1) of table 1 embodiment of the present invention and comparative example
The composition and performance (continuous 2) of table 1 embodiment of the present invention and comparative example
The composition and performance (continuous 3) of table 1 embodiment of the present invention and comparative example
The composition and performance (continuous 4) of table 1 embodiment of the present invention and comparative example
The composition and performance (continuous 5) of table 1 embodiment of the present invention and comparative example
The composition and performance (continuous 6) of table 1 embodiment of the present invention and comparative example
Claims (10)
1. a Silane Grafted PPR pipe PP Pipe Compound, is characterized in that expecting that the ratio in 90: 10 ~ 95: 5 forms with parts by weight by A material and B; Wherein
A material consists of: PPR 80 ~ 95 weight part, high density polyethylene(HDPE) 5 ~ 20 weight part, unsaturated silane 1-3 weight part, initiator 0.01-0.03 weight part, oxidation inhibitor 0.1-0.5 weight part, auxiliary crosslinking agent 0.1-2 weight part; Described auxiliary crosslinking agent is stearic acid, oxystearic acid or the mixture of at least two kinds in them;
B material consists of: PPR 100 weight part, catalyzer 1-3 weight part, oxidation inhibitor 0.1-0.5 weight part, cocatalyst 1-5 weight part; Wherein, described catalyzer is dibutyl tin laurate, tin dilaurate dioctyl tin, Phenylsulfonic acid or the mixture of at least two kinds in them; Described cocatalyst is metal oxide.
2. Silane Grafted PPR pipe PP Pipe Compound according to claim 1, is characterized in that described metal oxide is zinc oxide, calcium oxide or their mixture.
3. Silane Grafted PPR pipe PP Pipe Compound according to claim 1 and 2, is characterized in that the melt index of the PPR used during described A expects is less than 0.5g/10min (230 DEG C, 2.16kg).
4. Silane Grafted PPR pipe PP Pipe Compound according to claim 1 and 2, is characterized in that the melt index of the high density polyethylene(HDPE) used during described A expects is 2-5g/10min (190 DEG C, 2.16kg).
5. Silane Grafted PPR pipe PP Pipe Compound according to claim 1 and 2, is characterized in that described unsaturated silane is vinyltriethoxysilane, vinyltrimethoxy silane, vinyl front three Ethoxysilane or the mixture of at least two kinds in them.
6. Silane Grafted PPR pipe PP Pipe Compound according to claim 1 and 2, is characterized in that described initiator is peroxide initiator.
7. Silane Grafted PPR pipe PP Pipe Compound according to claim 1 and 2, is characterized in that the oxidation inhibitor used during described A expects is phosphite ester kind antioxidant.
8. Silane Grafted PPR pipe PP Pipe Compound according to claim 1 and 2, is characterized in that the melt index of the PPR used during described B expects is less than 0.5g/10min (230 DEG C, 2.16kg).
9. Silane Grafted PPR pipe PP Pipe Compound according to claim 1 and 2, the oxidation inhibitor that it is characterized in that using during described B expects is dihydroxyphenyl propane class, phosphite ester kind antioxidant or their mixture.
10. prepare a method for Silane Grafted PPR pipe PP Pipe Compound as claimed in claim 1, it is characterized in that A material and B material independent extruding pelletization separately, respectively comprise the following steps:
The preparation of A material:
After unsaturated silane and initiator being weighed in proportion, be fully uniformly mixed in airtight stainless steel mixing tank, the temperature of mixing tank controls between 23-27 DEG C, mixes rear for subsequent use;
Take PPR, high density polyethylene(HDPE), oxidation inhibitor and auxiliary crosslinking agent in proportion and put into mixing machine, stir fully; Then add the unsaturated silane mixed and initiator mixture gradually, stir fully and obtain initial formulation;
Initial formulation directly joins in parallel dual-screw extruding machine and carries out grafting granulation processing;
Forcing machine design temperature is by charging opening to mouth mould successively raised temperature 5-10 DEG C gradually, and the processing temperature of whole forcing machine controls at 110-230 DEG C;
It is 2-3 minute that the engine speed of forcing machine controls in the material residence time in an extruder;
The vacuum tightness of the vacuum extraction of forcing machine should lower than-0.08MPa;
A expects granulation final vacuum packed for standby use;
The preparation of B material:
Take PPR, catalyzer, oxidation inhibitor and cocatalyst in proportion, put into mixing machine, the temperature of mixing machine controls at 30-40 DEG C, and the material after mixing fully directly enters twin screw extruder granulation, and the temperature of forcing machine controls at 110-230 DEG C;
B expects granulation final vacuum packed for standby use;
A material and B material in proportion compounding even after, namely can be used for direct extruding pipe material.
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| CN109181201A (en) * | 2018-07-13 | 2019-01-11 | 安阳崇高纳米材料科技有限公司 | PP moves the preparation method of assembled floor-board material, the floor made of the material and floor |
| CN112390996B (en) * | 2020-10-29 | 2022-08-30 | 江西格林循环产业股份有限公司 | Modified regenerated polyethylene plastic for plastic pipeline and preparation method thereof |
| CN115011058B (en) * | 2022-07-11 | 2024-04-16 | 青岛科技大学 | Reinforced polypropylene composite material and preparation method thereof |
| CN116003912B (en) * | 2023-02-10 | 2024-01-09 | 创合新材料科技江苏有限公司 | Special polypropylene reinforcing material for micro-crosslinked high-pressure-resistant water pump and preparation method and application thereof |
| CN117624789B (en) * | 2023-12-01 | 2024-04-16 | 杭州佳磊环保科技有限公司 | Modified polypropylene composite pipe and preparation process thereof |
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| CN1869119A (en) * | 2005-05-27 | 2006-11-29 | 青岛大学 | Preparation method of partly cross-linked dystectic strength polypropylene |
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