CN105524327A - Polyethylene composition and preparation method thereof - Google Patents
Polyethylene composition and preparation method thereof Download PDFInfo
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- CN105524327A CN105524327A CN201410578790.1A CN201410578790A CN105524327A CN 105524327 A CN105524327 A CN 105524327A CN 201410578790 A CN201410578790 A CN 201410578790A CN 105524327 A CN105524327 A CN 105524327A
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- polyethylene composition
- carbon black
- polyethylene
- coupling agent
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Abstract
The invention relates to a polyethylene composition. The polyethylene composition comprises a high density polyethylene-linear low density polyethylene mixture as a base resin, a polyethylene molecule-grafted alkenyl silane coupling agent product and alkenyl silane coupling agent-modified carbon black. The invention also provides a preparation method of the polyethylene composition. Performances of the polyethylene composition satisfy use requirements of a low pressure thin wall irrigation pipe. The polyethylene composition has good strength, good flexibility, good processing properties, excellent aging resistance, ESCR resistance and hydrostatic pressure resistance.
Description
Technical field
The invention belongs to polymeric material field, be specifically related to a kind of polyethylene composition and preparation method thereof.
Background technology
Low pressure pipe irrigation is an effective engineering in water saving irrigation, by pump and management system, directly low pressure water flow is introduced field, ditch, furrow irrigated farmland.Low pressure water transportation pipe mainly adopts rigid polyvinyl chloride (PVC-U) pipe and polyethylene (PE) pipe of thin-walled.PE material has the over-all propertieies such as good snappiness, winter hardiness and internal pressure-resistant, and have excellent processing characteristics when extrusion moulding, meet High-speed machining requirement, therefore PE occupies main status in tubing raw material simultaneously.
Irrigating the qualitative performance requirements most important of tubing is exactly work-ing life, and ageing-resistant and resisting environmental stress and cracking (ESCR) performance of this and material is closely bound up.Irrigation pipe is general all to be laid on earth's surface, is often bent, and simultaneously directly by uviolizing, aging speed is very fast, and often work-ing life is less than half a year.And the extruded velocity of low pressure thin-walled irrigation pipe quickly (is greater than 100m/min) usually, single polyethylene is adopted to be difficult to reach requirement, modification must being carried out to polyethylene, mainly starting with from widening relative molecular mass distribution, also will consider that it is ageing-resistant, ESCR performance simultaneously.The domestic PE resin grade not being exclusively used in water saving irrigation at present, each producer uses the polyvinyl resin trade mark mixed and disorderly, most use high density polyethylene(HDPE) (HDPE), Low Density Polyethylene (LDPE) and linear low density polyethylene (LLDPE) blending use, to adapt to the different application field of product, meet the requirement of production technique and cost simultaneously.
Chinese patent CN103571007A discloses a kind of composition of drip irrigation zone material; composition comprises polyvinyl resin, black masterbatch, PPA modifier, calcium stearate; by adding the problems such as appropriate modifier solves difficult forming in the process of producing product of drip irrigation zone, production efficiency is low, visual appearance is poor in polyvinyl resin; improve Product processing performance simultaneously; decrease a mouthful mould buildup; improve product appearance quality, improve the first-time qualification rate of product.
Chinese patent CN1693356 discloses a kind of material compositions of ultrathin strap of trickle irrigation, composition includes medium-density polyethylene, ethene-vinyl acetate copolymer, Low Density Polyethylene, high density polyethylene(HDPE), carbon black, nano-calcium carbonate, make the production cost of ultrathin strap of trickle irrigation and former drip irrigation zone cost reduce by 1/3rd, production rate improves more than three times.
Chinese patent CN103665508A discloses a kind of drip irrigation pipe polyethylene composition, each component comprises HDPE, LDPE, metallocene PE, oxidation inhibitor, carbon black and fluorine-containing processing aid, there is good intensity, snappiness, ageing-resistant and processing characteristics, but its ESCR time is only greater than 200h.
Composition in above-mentioned patent all adopts HDPE and LDPE blended as matrix resin, the thin-walled property of tubing can be realized by high speed extrusion, prepared drip irrigation pipe all shows well in intensity, snappiness, processing characteristics and ageing-resistant performance etc., is applicable to the tubing that water-saving irrigation system is used.But do not carry out suitable pre-treatment to carbon black in above-mentioned patent in preparation process, therefore carbon black dispersion is poor, thus the mechanics of material and processing characteristics is caused to decline.Drip irrigation pipe is generally laid on earth's surface, is directly shined upon and soaks with rainwater, and tubing is often bent and squeezing action in construction and use, ageing-resistant, the ESCR performance deficiency all to some extent of current drip irrigation pipe material used.
Summary of the invention
For the problems referred to above, the invention provides a kind of polyethylene composition, its by high density polyethylene(HDPE) (HDPE) and linear low density polyethylene (LLDPE) blended based on resin, and comprise polyethylene molecule graft olefin silane coupling agent product and by the coupling agent modified carbon black of described alkenyl silanes.Technical scheme of the present invention, while meeting high speed extrusion, improves the environmental stress cracking resistance (ESCR) of material.
In a concrete embodiment, by weight, the effective polyethylene composition of described low pressure irrigation comprises following component:
A. high density polyethylene(HDPE), 100 parts;
B. linear low density polyethylene, 10-100 part, preferred 20-40 part;
C. oxidation inhibitor, 0.1-2 part;
D. the carbon black of modification, 1-5 part, preferred 2-3 part;
E. alkenyl silanes coupling agent, 1-5 part, preferred 2-4 part;
F. initiator, 0.1-1 part.
In a concrete embodiment, described alkenyl silanes coupling agent is vinyl alkenyl silanes coupling agent, and its general formula is CH
2=CH
2-(CH
2)
n-SiX
3, wherein X is selected from methoxyl group, oxyethyl group, methoxy ethoxy, three tert.-butoxies, acetoxyl group, and n is selected from 0,1,2 and 3.
In a concrete embodiment, described oxidation inhibitor is selected from least one in phenols, hindered amines and phosphite ester kind antioxidant.Such as described oxidation inhibitor can be four [β-(3,5-di-tert-butyl-hydroxy phenyl) propionic acid] pentaerythritol ester, three [2.4-di-tert-butyl-phenyl] phosphorous acid ester, β-positive octadecanol ester of (3,5-di-tert-butyl-hydroxy phenyl) propionic acid etc.
In a concrete embodiment, the particle diameter of the carbon black of described modification is 20-50nm.
In a concrete embodiment, described initiator can be the initiator of this area routine, preferred organo-peroxide, more preferably dialkyl peroxide, such as dicumyl peroxide, di-t-butyl peroxide etc.
The present invention also provides a kind of preparation method of above-mentioned polyethylene composition, comprises the following steps:
Steps A, adopts high-energy ball milling method by carbon black particle refinement, is coated on the carbon blacksurface after refinement by the described alkenyl silanes coupling agent being dissolved in solvent simultaneously, obtains the carbon black of modification in the mode of spraying;
Step B, by described high density polyethylene(HDPE), described linear low density polyethylene, described oxidation inhibitor, described initiator and described modified carbon black premix, then melt blending, subsequently extruding pelletization, obtain described polyethylene composition.
In an embodiment, the mass fraction of each raw material is respectively:
A. high density polyethylene(HDPE), 100 parts;
B. linear low density polyethylene, 10-100 part, preferred 20-40 part;
C. oxidation inhibitor, 0.1-2 part;
D. the carbon black of modification, 1-5 part, preferred 2-3 part;
E. alkenyl silanes coupling agent, 1-5 part, preferred 2-4 part;
F. initiator, 0.1-1 part.
In steps A of the present invention, by the method for pulverizing limit, limit coating, more easily realize the miniaturization of carbon black, the carbon black particle of employing can be technical grade carbon black, and the particle diameter of the carbon black after refinement is preferably 20-50nm.
In the preparation process in accordance with the present invention ,-the SiX in described alkenyl silanes coupling agent
3group can form Si-O-CB key with carbon black particle surface bonding, simultaneously its other end thiazolinyl can with PE macromolecular chain graft reaction.The combination of carbon blacksurface and PE molecular chain is more firm, and in composition, remaining small molecules content is less, greatly can improve the resistance to ESCR performance of composition.
In a concrete embodiment, steps A also comprises ball milling and the carbon black applying alkenyl silanes coupling agent sieves, and removes unnecessary solvent at 95-105 DEG C, obtain alkenyl silanes coupling agent modified after carbon black.Preferably, to dynamics be controlled in the process of ball milling, avoid the temperature of material more than 105 DEG C.The hydroxyl of the X group in alkenyl silanes coupling agent and carbon blacksurface or carboxyl are combined and form Si-O-CB key, to reach the object of surface modification.
In a concrete embodiment, described in steps A, solvent is selected from alcohols, preferred alcohol, Virahol or the trimethyl carbinol or its any mixture; More preferably dehydrated alcohol.
The present invention also provides described polyethylene composition to prepare the application of low pressure irrigation pipe.Preferably, the wall thickness of described low pressure irrigation pipe is 0.50mm-1.2mm.
Composition of the present invention is according to polyethylene low pressure irrigation pipe performance requriements, and resin based on selection HDPE and LLDPE is blended, widens molecular weight distribution, improve processing characteristics, meet the needs of high speed extrusion.Carbon black add the intensity and ageing-resistant performance that can improve material, adopt high-energy ball milling method to improve dispersion of particles degree to the silane-modified nearly step of carbon blacksurface.Polyvinyl resin is by alkenyl silanes coupling agent fusion-grafting in twin-screw extrusion simultaneously, improves the resistance to ESCR performance of composition.Preparation technology is simple and reliable in addition, the grafting of carbon blacksurface modification and macromolecular chain all adopts same alkenyl silanes, make the combination of carbon black and PE molecular chain more firm, and the small-molecular-weight of remnants is greatly less in composition, the resistance to ESCR performance of further raising composition, has very high economic worth.
Embodiment
By the following examples effect of the present invention is described, but protection scope of the present invention is not limited in these embodiments, embodiment and " part " described in comparative example all refer to mass fraction.
1. raw materials used and reagent
High density polyethylene, density 0.954g/cm
3, melt flow rate (MFR) 0.13g/10min, Yanshan Petrochemical is produced.Linear low density polyethylene LLDPE, density 0.920g/cm
3, melt flow rate (MFR) 2.0g/10min, raises sub-petrochemical iy produced.
Antioxidant 1010, four [β-(3,5-di-tert-butyl-hydroxy phenyl) propionic acid] pentaerythritol ester, BASF AG's product.
Carbon black, Cabot N660 general purpose grade.
Alkenyl silanes coupling agent, selects vinyltrimethoxy silane (VTMS, 98%), lark prestige Products.
Initiator, dicumyl peroxide (DCP, 99%), lark prestige Products.
2. performance test standard and instrument
Tensile mechanical properties: by GB/T1040-2006 standard, rate of extension is 50mm/min, measures tensile yield strength and the elongation at break of different batten.Testing tool is German Zwick company Z020 type tensile testing machine.
Oxidation induction time (OIT): according to GB/T19466.6-2009 standard, adopts DSC to test the oxidation induction time of sample at 200 DEG C.Testing tool is PE company D8000DSC thermal analyzer.
Resisting environmental stress and cracking (ESCR) performance test: according to GB/T1842-2008 standard, calculates and determines the environmental stress cracking time F of sample when probability of damage is 50%
50, testing tool is Tokyo physics and chemistry apparatus Co., Ltd. HBS-1200 type constant temperature water tank.
The component of polyethylene composition in the different embodiment of table 1 and comparative example
Embodiment 1-8
In the present invention in embodiment 1-8 the preparation of polyethylene composition and performance test as follows:
1) surface modification of carbon black particle
Adopt high-energy ball milling method by carbon black particle refinement, alkenyl silanes coupling agent is dissolved in dehydrated alcohol simultaneously, immediately the solution containing vinyl silicane coupling agent is coated on carbon blacksurface in the mode of spraying.Adopt planetary high-energy ball mill, grinding element is agate ball.Milling parameters is: rotating speed 100r/min, and ball material mass ratio 20:1, Ball-milling Time is 20min.To dynamics be controlled in the process of ball milling, avoid the temperature of material more than 105 DEG C.Sieve after ball milling, at 105 DEG C, remove unnecessary solvent, obtain modified carbon black particle.The mass fraction of carbon black, vinyl silicane coupling agent is as shown in table 1.
2) melt blending of polyethylene composition is extruded
By HDPE, the LLDPE of the different numbers shown in table 1, oxidation inhibitor, initiator and modified carbon black premix in homogenizer, then through twin screw extruder melt blending at 180-210 DEG C, after extruding pelletization, obtain polyethylene composition of the present invention.
Comparative example 1
1) surface modification technology of carbon black particle is identical with embodiment 1-8, and the mass fraction of carbon black and silane is 3 parts.
2) the melt extruding of polyethylene composition: by the carbon black after 100 parts of HDPE, 1 part of oxidation inhibitor, 1 part of initiator and 3 parts of surface modifications in homogenizer after premix, again through twin screw extruder melt blending at 180-210 DEG C, after extruding pelletization, obtain the polyethylene composition not containing LLDPE component in comparative example 1.
Comparative example 2
1) carbon black particle does not adopt alkenyl silanes coupling agent to carry out surface modification.
2) the melt extruding of polyethylene composition: by 100 parts of HDPE, 20 parts of LLDPE, 1 part of oxidation inhibitor, 1 part of initiator and 3 parts of unmodified carbon black in homogenizer after premix, again through twin screw extruder melt blending at 180-210 DEG C, after extruding pelletization, obtain the polyethylene composition in comparative example 2.
The polyethylene composition that embodiment 1-8 and comparative example 1-2 is obtained is made into standard batten through compression moulding, stamping-out, and carry out corresponding mechanics, ageing-resistant and ESCR performance test according to GB, acquired results is as shown in table 2.
The polyethylene composition that embodiment 1-8 obtains the most at last prepares the thin-walled drip irrigation pipe (wall thickness 0.50mm, nominal pressure 100kPa) of internal diameter 16.0mm by single screw extrusion machine, Screw Extrusion temperature 190-230 DEG C, extruded velocity is 100m/min.The resistance to hydrostatic pressure performance of drip irrigation pipe goods according to GB19812.3-2008 standard 20 DEG C, keep 60min under 180kPa, test its breakage, result is as shown in table 2 equally.
Table 2
In sum, the properties of polyethylene composition of the present invention meets the service requirements of low pressure thin-walled irrigation pipe, except having good intensity, snappiness and processing characteristics, also has excellent ageing-resistant, resistance to ESCR and resistance to hydrostatic pressure performance.
Claims (10)
1. a polyethylene composition, its by high density polyethylene(HDPE) and linear low density polyethylene blended based on resin, and comprise polycthylene grafted alkenyl silanes coupling agent product and by the coupling agent modified carbon black of described alkenyl silanes.
2. the effective polyethylene composition of low pressure irrigation according to claim 1, is characterized in that, by weight, comprises following component:
A. high density polyethylene(HDPE), 100 parts;
B. linear low density polyethylene, 10-100 part;
C. oxidation inhibitor, 0.1-2 part;
D. the carbon black of modification, 1-5 part;
E. alkenyl silanes coupling agent, 1-5 part;
F. initiator, 0.1-1 part.
3. polyethylene composition according to claim 2, is characterized in that, described alkenyl silanes coupling agent is vinyl silicane coupling agent, and its general formula is CH
2=CH
2-(CH
2)
n-SiX
3, wherein X is selected from methoxyl group, oxyethyl group, methoxy ethoxy, three tert.-butoxies, acetoxyl group, and n is selected from 0,1,2 and 3.
4. the polyethylene composition according to Claims 2 or 3, is characterized in that, described oxidation inhibitor is selected from least one in phenols, hindered amines and phosphite ester kind antioxidant.
5. the polyethylene composition according to any one of claim 1-4, is characterized in that, the particle diameter of the carbon black of described modification is 20-50nm.
6. the polyethylene composition according to any one of claim 2-5, is characterized in that, described initiator is organo-peroxide.
7. a preparation method for polyethylene composition according to any one of claim 1-6, comprises the following steps:
Steps A, adopts high-energy ball milling method by carbon black particle refinement, is coated on the carbon blacksurface after refinement by the described alkenyl silanes coupling agent being dissolved in solvent simultaneously, obtains the carbon black of modification in the mode of spraying;
Step B, by described high density polyethylene(HDPE), described linear low density polyethylene, described oxidation inhibitor, described initiator and described modified carbon black premix, then melt blending, subsequently extruding pelletization, obtain described polyethylene composition.
8. method according to claim 7, is characterized in that, the particle diameter of the carbon black after described refinement is 20-50nm.
9. the method according to claim 7 or 8, is characterized in that, described solvent is alcoholic solvent.
10. the polyethylene composition according to any one of claim 1-6 or prepared the application of low pressure irrigation pipe by the polyethylene composition that preparation method according to any one of claim 7-9 obtains.
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Cited By (11)
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| CN107022142A (en) * | 2017-04-20 | 2017-08-08 | 安徽春辉仪表线缆集团有限公司 | A kind of DOPO derivatives grafts siloxanes flame retarding reaction type cable material and preparation method thereof |
| CN107705898A (en) * | 2017-10-31 | 2018-02-16 | 四川力智久创知识产权运营有限公司 | A kind of tension PE cable |
| CN107919190A (en) * | 2017-10-31 | 2018-04-17 | 四川力智久创知识产权运营有限公司 | A kind of tension polyvinyl chloride cable |
| CN111675842A (en) * | 2020-07-01 | 2020-09-18 | 上海中塑管业有限公司 | Be used for polyolefin gas tubular product and performance detection device thereof |
| CN113637250A (en) * | 2021-08-20 | 2021-11-12 | 赤途实业(上海)有限公司 | Polymer composition for container cover and container cover |
| CN113845713A (en) * | 2021-10-18 | 2021-12-28 | 甘肃青龙管业有限责任公司 | Puncture-resistant inlaid patch type drip irrigation tape and preparation method thereof |
| CN114193869A (en) * | 2022-01-04 | 2022-03-18 | 浙江红饰和家居有限公司 | Functional wall cloth and preparation method thereof |
| CN114456509A (en) * | 2021-11-15 | 2022-05-10 | 廊坊北化高分子材料有限公司 | Modified polyolefin for low-melting-point carbon black master batch and preparation method thereof |
| CN115011019A (en) * | 2022-06-23 | 2022-09-06 | 青岛优派普环保科技股份有限公司 | High-strength PE gas pipe and preparation method thereof |
| CN115038749A (en) * | 2020-01-30 | 2022-09-09 | 博里利斯股份公司 | Polymer composition |
| CN115490949A (en) * | 2022-10-21 | 2022-12-20 | 日丰企业集团有限公司 | PEXb pipe with high shape memory function |
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Cited By (16)
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| CN107022142A (en) * | 2017-04-20 | 2017-08-08 | 安徽春辉仪表线缆集团有限公司 | A kind of DOPO derivatives grafts siloxanes flame retarding reaction type cable material and preparation method thereof |
| CN107705898A (en) * | 2017-10-31 | 2018-02-16 | 四川力智久创知识产权运营有限公司 | A kind of tension PE cable |
| CN107919190A (en) * | 2017-10-31 | 2018-04-17 | 四川力智久创知识产权运营有限公司 | A kind of tension polyvinyl chloride cable |
| CN115038749A (en) * | 2020-01-30 | 2022-09-09 | 博里利斯股份公司 | Polymer composition |
| CN111675842A (en) * | 2020-07-01 | 2020-09-18 | 上海中塑管业有限公司 | Be used for polyolefin gas tubular product and performance detection device thereof |
| CN113637250B (en) * | 2021-08-20 | 2023-08-18 | 赤途实业(上海)有限公司 | Polymer composition for container cover and container cover |
| CN113637250A (en) * | 2021-08-20 | 2021-11-12 | 赤途实业(上海)有限公司 | Polymer composition for container cover and container cover |
| CN113845713A (en) * | 2021-10-18 | 2021-12-28 | 甘肃青龙管业有限责任公司 | Puncture-resistant inlaid patch type drip irrigation tape and preparation method thereof |
| CN114456509A (en) * | 2021-11-15 | 2022-05-10 | 廊坊北化高分子材料有限公司 | Modified polyolefin for low-melting-point carbon black master batch and preparation method thereof |
| CN114456509B (en) * | 2021-11-15 | 2023-12-05 | 廊坊北化高分子材料有限公司 | Modified polyolefin for low-melting-point carbon black master batch and preparation method thereof |
| CN114193869A (en) * | 2022-01-04 | 2022-03-18 | 浙江红饰和家居有限公司 | Functional wall cloth and preparation method thereof |
| CN114193869B (en) * | 2022-01-04 | 2024-03-22 | 浙江红饰和家居有限公司 | Functional wall cloth and preparation method thereof |
| CN115011019A (en) * | 2022-06-23 | 2022-09-06 | 青岛优派普环保科技股份有限公司 | High-strength PE gas pipe and preparation method thereof |
| CN115011019B (en) * | 2022-06-23 | 2022-12-16 | 青岛优派普环保科技股份有限公司 | High-strength PE (polyethylene) gas pipe and preparation method thereof |
| CN115490949A (en) * | 2022-10-21 | 2022-12-20 | 日丰企业集团有限公司 | PEXb pipe with high shape memory function |
| CN115490949B (en) * | 2022-10-21 | 2023-11-07 | 日丰企业集团有限公司 | PEXb tubular product with high shape memory function |
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Application publication date: 20160427 |