CN105585678A - Polyethylene graft and preparation method thereof - Google Patents
Polyethylene graft and preparation method thereof Download PDFInfo
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- CN105585678A CN105585678A CN201410556730.XA CN201410556730A CN105585678A CN 105585678 A CN105585678 A CN 105585678A CN 201410556730 A CN201410556730 A CN 201410556730A CN 105585678 A CN105585678 A CN 105585678A
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Abstract
Polyethylene graft is modified polyethylene graft with polyethylene as a main chain and with maleic anhydride functionalized low-molecular-weight polybutadiene rubber as a long-chain branch. Low density polyethylene (LDPE) is used in grafting low-molecular-weight maleic polybutadiene. The grafting rate is 0.4-1.3 wt%. Melt flow index (MFI) of the low density polyethylene is within 10-50 g/10min, relative molecular mass of low-molecular-weight maleic polybutadiene is 1000-5000, and content of maleic anhydride is 6-11%. The preparation method of the polyethylene graft comprises the following steps: measuring polyethylene, low-molecular-weight maleic polybutadiene and an initiator and uniformly mixing, carrying out melt extrusion on the mixed materials by a screw extruder at 160-190 DEG C, and cooling and granulating so as to prepare the polyethylene graft.
Description
Technical field
The present invention relates to a kind of polycthylene grafted thing and preparation method thereof.
Background technology
Polyethylene is carried out to graft modification, on nonpolar strand, introduce polarity or functional form side group, not only be conducive to improve the interface compatibility between macromolecular material and inorganic filler, and be conducive to prepare high polymer alloy with other polar polymer blend, also can improve the adhesion property to many materials, the adhesive that processability is good simultaneously.
Maleic anhydride (MAH) Grafted Polyethylene (PE) is the most frequently used and the most effectively improves PE polarity and the method for gluing performance, oxygen on MAH molecule is with lone pair electrons, easily with polar material gluing or the alloying with unoccupied orbital, also can with the substance reaction that contains hydroxyl, amino, epoxy radicals etc., generate new polymers. The method of PE and MAH grafting has solution graft copolymerization, irradiation grafting, solid phase grafting, fusion-grafting etc., and wherein fusion-grafting is to apply more a kind of method of modifying, and it is under initator effect, the reaction in double screw extruder of PE and comonomer. The advantage of this method is that equipment simply, does not need other reactor design, and can produce continuously, the reaction time is shorter, production cost is lower; Shortcoming is reaction temperature higher (190～230 DEG C), and PE crosslinking side reaction is serious, and percent grafting is lower, and the unreacted monomer, the initator that remain in product are difficult to remove, and affect product property, are unsuitable for volatile monomer. The difficult problem that fusion-grafting exists is that PE, under the effect of peroxide, MAH, cross-linking reaction can occur, thereby causes the viscosity of graft to increase considerably, and rheological property is poor, extrudes difficulty.
Patent CN201010581163.5 discloses a kind of method that suspension method is prepared high density polyethylene (HDPE)-maleic anhydride graft copolymer, the copolymer grafted rate that the method makes is high, and cross-linking agent content goes to zero, and solvent load is few, equipment and process is simple, is convenient to large-scale production. The grafting method of its HDPE grafting MAH for to adopt suspension polymerization to carry out graft reaction in autoclave, mainly in autoclave, to add HDPE and sweller, MAH, interfacial agents, surfactant and water, stirring heats up makes HDPE melting, drip initator again and carry out Suspension Graft reaction, wherein initator is first dispersed in the sweller of HDPE. Patent " preparation method of Process of polyethylene adhesive for anticorrosion of steel pipe " (patent No. CN02112550.3) is that one thermal booster reaction grafting method is prepared Process of polyethylene adhesive for anticorrosion of steel pipe, the method is that base resin polyethylene and grafted monomers maleic anhydride are carried out to hot initiation grafting reaction in hot initiation grafting reactor, polar functional group in grafting in sub polyethylene subchain, thus Process of polyethylene adhesive for anticorrosion of steel pipe generated. Hot initiation grafting reactor is linked in sequence and is formed by screw extruder 1, static mixer 2, die head 3, grafted monomers maleic anhydride and base resin polyethylene go out machine 1 from screw rod and are extruded into static mixer 2, and then clamp-on die head 3, finally extrude from die head 3 from static mixer 2. " thermal synthesis process for preparing grafted polyvinyl-maleic anhydride copolymer in solvent " (patent No. CN02112385.3) provide a kind of thermal synthesis process for preparing grafted polyvinyl-maleic anhydride copolymer in solvent, it is characterized in that in autoclave, put into polyvinyl resin, maleic anhydride, dispersant, initator and be total to monomer and be dissolved in solvent, under uniform temperature and time, react, then washing is dry, obtains grafted polyvinyl-maleic anhydride copolymer. Use it for the adhesive of polyethylene and metal composite pipe or plate, cementability is good, peel strength is high; For the bulking agent of polymer alloy, greatly improve the compatibility of polyethylene and other polymer, obtain the polymer alloy of excellent combination property; As the compatilizer of polyethylene and composite material of inorganic matter, make the significantly increase and impact flexibility remains unchanged of poly hot strength. " a kind of extruding graft process of polyvinyl wax " (patent No. CN00135633.X) relates to the graft process of by-product Tissuemat E in a kind of polythene production process. After material polyethylene wax, initator, grafted monomers are mixed, add screw extruder, control extrusion temperature 80-90 DEG C. Gained graft product acid number reaches 7-15mg/g. " LLDPE of graft modification-their preparation method and application " (patent No. CN88102228) announced a kind of phenylethylene/maleic anhydride grafted polyethylene. This polyethylene is extremely excellent impact modifier, there is very high UV resistant performance and toughness, do not make polyamide and polyester variable color with their modifications, be also suitable for tack coat, compatibility promoting agent and the adhesive accelerant of making adhesive or adhesive layer, heat-sealable layer, laminated film. The preparation of Grafted Polyethylene can by a kind of LLDPE higher than 110 DEG C of temperature, under shearing force effect, application free-radical initiator optional with under antioxidant condition, carry out conversion reaction with grafting material, and can under a kind of solvent exists, use. Patent CN200510049737.3 discloses a kind of high-density polycthylene grafted acryhic material and preparation method thereof, adopt high density polyethylene (HDPE) (HDPE), acrylic acid (AA), initator by certain proportioning Haake torque rheometer blend 20min at 160 DEG C, screw speed 60rpm, what after melt blending, obtain is exactly polycthylene grafted acryhic.
Summary of the invention
The object of the present invention is to provide a kind of polycthylene grafted thing, system taking polyethylene as main chain, maleation low molecular weight polybutadiene rubber is the modified poly ethylene graft of long-chain branch, described polycthylene grafted thing cross-linking agent is less, fluidity of molten is easy to control, preparation technology is simple and easy to do, and percent grafting is higher.
Another object of the present invention is also to provide the preparation method of described polycthylene grafted thing.
For realizing goal of the invention, the present invention by the following technical solutions:
A kind of polycthylene grafted thing, is modified by maleic acid anhydride graft polyethylene, it is characterized in that, described polycthylene grafted thing adopts low density polyethylene (LDPE) (LDPE) grafting low-molecular-weight maleation polybutadiene, and percent grafting is 0.4%-1.3%(percetage by weight).
Described polycthylene grafted thing is obtained by following component (in weight portion) melting graft reaction, comprising:
100 parts of low density polyethylene (LDPE)s (LDPE),
Low-molecular-weight maleation polybutadiene (PB-g-MAH) 1-10 part,
Initator 0.1-0.2 part.
Modified by maleic acid anhydride graft polyethylene of the present invention, maleic anhydride comes from PB-g-MAH(low-molecular-weight maleation polybutadiene). Described polycthylene grafted thing be taking polyethylene as main chain, low-molecular-weight maleic anhydride functionalized poly butadiene rubber is the modified poly ethylene graft of long-chain branch.
Described low density polyethylene (LDPE) is Powdered, and melt index (MFI) is 10-50g/10min.
Described PB-g-MAH(low-molecular-weight maleation polybutadiene), be viscous liquid, relative molecular mass is 1000-5000, the content of maleic anhydride is 6-11%.
Described initator is peroxide or azo-initiator, preferably from cumyl peroxide (DCP), dibenzoyl peroxide (BPO), di-tert-butyl peroxide (DTBP), two tertiary amyl peroxide (DTAP) or azo-bis-isobutyl cyanide etc.
As preferred version, described polycthylene grafted thing, comprises following component:
100 parts of low density polyethylene (LDPE)s, melt index is 20-40g/10min;
PB-g-MAH1-10 part,
Initator cumyl peroxide (DCP) 0.1-0.15 part.
Polycthylene grafted thing of the present invention adopts following methods preparation: polyethylene is mixed with after PB-g-MAH, initator metering, mixed material melt extrudes on screw extruder at the temperature of 160 DEG C～190 DEG C, product, through cooling, granulation, makes described polycthylene grafted thing.
In described method, mixed material comprises following component:
100 parts of low density polyethylene (LDPE)s (LDPE),
Low-molecular-weight maleation polybutadiene (PB-g-MAH) 1-10 part,
Initator 0.1-0.2 part.
Described low density polyethylene (LDPE) melt index is 10-50g/10min, and the relative molecular mass of described low-molecular-weight maleation polybutadiene is 1000-5000, and the content of maleic anhydride is 6-11%; Described initator is cumyl peroxide (DCP), dibenzoyl peroxide (BPO), di-tert-butyl peroxide (DTBP), two tertiary amyl peroxide (DTAP) or azo-bis-isobutyl cyanide etc.
Beneficial effect of the present invention: polycthylene grafted thing of the present invention, system taking polyethylene as main chain, maleation low molecular weight polybutadiene rubber is the modified poly ethylene graft of long-chain branch, described polycthylene grafted thing cross-linking agent is few, fluidity of molten is easy to control, preparation technology is simple and easy to do, and percent grafting is higher. The present invention, by fusion-grafting, is grafted to maleation polybutadiene on polyethylene main chain, has expanded the method for polycthylene grafted polar monomer or functional monomer, and the substantive percent grafting that has improved maleic anhydride.
Brief description of the drawings
The infrared spectrogram of modified poly ethylene graft prepared by Fig. 1 LDPE and embodiment of the present invention 1-5 thereof.
Detailed description of the invention
Below by specific embodiment, technical solutions according to the invention are further described in detail, but are necessary to point out that following examples, only for the description to summary of the invention, do not form limiting the scope of the invention.
Polycthylene grafted thing of the present invention be taking polyethylene as main chain, low-molecular-weight maleation polybutadiene rubber is the modified poly ethylene graft of long-chain branch, be the product of low density polyethylene (LDPE) fusion-grafting low-molecular-weight maleation polybutadiene, percent grafting is 0.4%-1.3%(percetage by weight). Described polycthylene grafted thing adopts following methods preparation:
1) PB-g-MAH, initator, LDPE are accurately weighed, initator is first evenly sprinkled upon on rubber, then mixes with PE, polyethylene is placed in high-speed mixer and is mixed with PB-g-MAH, DCP;
2) mixed material melt extrudes double screw extruder (draw ratio is 40, screw diameter be 35cm) is upper at the temperature of 160 DEG C～190 DEG C, and product is through cooling, granulation, and cooling and dicing is placed in 70 DEG C of baking ovens dries 6 hours.
The infrared spectrum of the modified poly ethylene graft that said method makes as shown in Figure 1, compared with LDPE, there is absworption peak at 1714cm-1 and 1790cm-1 place in polycthylene grafted thing, be the characteristic peak of maleic anhydride, show that maleic anhydride group has successfully been grafted on high fluidity LLDPE macromolecular main chain.
Melt index described in the present invention is according to GB/T3682-2000 standard testing, and test condition is 190 DEG C, 2.160Kg. The mensuration of percent grafting can calculate by infrared spectrum.
In following specific embodiment, the low density polyethylene (LDPE) melt index of employing is 10-50g/10min. PB-g-MAH(low-molecular-weight maleation polybutadiene), be viscous liquid, relative molecular mass is 1000-5000, the content (wt%) of maleic anhydride is 6-11%.
Embodiment 1
100 parts of low density polyethylene (LDPE)s (melt index is 20g/10min), PB-g-MAH1 part, DCP0.1 part are mixed to 3min in high-speed mixer under middling speed, through double screw extruder melt extrude, granulation, each section of temperature of double screw extruder is 160 DEG C-170 DEG C-180 DEG C-190 DEG C-190 DEG C-190 DEG C-180 DEG C-170 DEG C-170 DEG C, and screw speed is 120rpm.
Obtain through double screw extruder granulation taking polyethylene as main chain, the functionalized low molecular weight polybutadiene rubber of maleic anhydride is the modified poly ethylene graft of long-chain branch, percent grafting is 0.46%, melt index (2.16Kg) is 0.8g/10min.
Embodiment 2
100 parts of low density polyethylene (LDPE)s (melt index is 20g/10min), PB-g-MAH3 part, DCP0.1 part are mixed to 3min in high-speed mixer under middling speed, through double screw extruder melt extrude, granulation.
Obtain through double screw extruder granulation taking polyethylene as main chain, the functionalized low molecular weight polybutadiene rubber of maleic anhydride is the modified poly ethylene graft of long-chain branch, percent grafting is 0.61%, melt index (2.16Kg) is 0.9g/10min.
Embodiment 3
100 parts of low density polyethylene (LDPE)s (melt index is 20g/10min), PB-g-MAH5 part, DCP0.1 part are mixed to 3min in high-speed mixer under middling speed, through double screw extruder melt extrude, granulation.
Obtain through double screw extruder granulation taking polyethylene as main chain, the functionalized low molecular weight polybutadiene rubber of maleic anhydride is the modified poly ethylene graft of long-chain branch, percent grafting is 0.82%, melt index (2.16Kg) is 1.3g/10min.
Embodiment 4
100 parts of low density polyethylene (LDPE)s (melt index is 20g/10min), PB-g-MAH7 part, DCP0.1 part are mixed to 3min in high-speed mixer under middling speed, through double screw extruder melt extrude, granulation.
Obtain through double screw extruder granulation taking polyethylene as main chain, the functionalized low molecular weight polybutadiene rubber of maleic anhydride is the modified poly ethylene graft of long-chain branch, percent grafting is 0.86%, melt index (2.16Kg) is 1.2g/10min.
Embodiment 5
100 parts of low density polyethylene (LDPE)s (melt index is 20g/10min), PB-g-MAH10 part, DCP0.1 part are mixed to 3min in high-speed mixer under middling speed, through double screw extruder melt extrude, granulation.
Obtain through double screw extruder granulation taking polyethylene as main chain, the functionalized low molecular weight polybutadiene rubber of maleic anhydride is the modified poly ethylene graft of long-chain branch, percent grafting is 0.89%, melt index (2.16Kg) is 1.8g/10min.
Embodiment 6
100 parts of low density polyethylene (LDPE)s (melt index is 20g/10min), PB-g-MAH1 part, DCP0.15 part are mixed to 3min in high-speed mixer under middling speed, through double screw extruder melt extrude, granulation.
Obtain through double screw extruder granulation taking polyethylene as main chain, the functionalized low molecular weight polybutadiene rubber of maleic anhydride is the modified poly ethylene graft of long-chain branch, percent grafting is 0.49%, melt index (2.16Kg) is 0.4g/10min.
Embodiment 7
100 parts of low density polyethylene (LDPE)s (melt index is 20g/10min), PB-g-MAH3 part, DCP0.15 part are mixed to 3min in high-speed mixer under middling speed, through double screw extruder melt extrude, granulation.
Obtain through double screw extruder granulation taking polyethylene as main chain, the functionalized low molecular weight polybutadiene rubber of maleic anhydride is the modified poly ethylene graft of long-chain branch, percent grafting is 0.67%, melt index (2.16Kg) is 0.6g/10min.
Embodiment 8
100 parts of low density polyethylene (LDPE)s (melt index is 20g/10min), PB-g-MAH5 part, DCP0.15 part are mixed to 3min in high-speed mixer under middling speed, through double screw extruder melt extrude, granulation.
Obtain through double screw extruder granulation taking polyethylene as main chain, the functionalized low molecular weight polybutadiene rubber of maleic anhydride is the modified poly ethylene graft of long-chain branch, percent grafting is 1.18%, melt index (2.16Kg) is 1.0g/10min.
Embodiment 9
100 parts of low density polyethylene (LDPE)s (melt index is 20g/10min), PB-g-MAH7 part, DCP0.15 part are mixed to 3min in high-speed mixer under middling speed, through double screw extruder melt extrude, granulation.
Obtain through double screw extruder granulation taking polyethylene as main chain, the functionalized low molecular weight polybutadiene rubber of maleic anhydride is the modified poly ethylene graft of long-chain branch, percent grafting is 1.25%, melt index (2.16Kg) is 0.9g/10min.
Embodiment 10
100 parts of low density polyethylene (LDPE)s (melt index is 20g/10min), PB-g-MAH10 part, DCP0.15 part are mixed to 3min in high-speed mixer under middling speed, through double screw extruder melt extrude, granulation.
Obtain through double screw extruder granulation taking polyethylene as main chain, the functionalized low molecular weight polybutadiene rubber of maleic anhydride is the modified poly ethylene graft of long-chain branch, percent grafting is 1.29%, melt index (2.16Kg) is 1.3g/10min.
Claims (9)
1. a polycthylene grafted thing, is characterized in that, described polycthylene grafted thing adopts grafted low density polyethylene low-molecular-weight maleation polybutadiene, percentage meter by weight, and percent grafting is 0.4%-1.3%.
2. polycthylene grafted thing according to claim 1, is characterized in that, described polycthylene grafted thing is obtained by following component melts graft reaction, in weight portion, comprising:
100 parts of low density polyethylene (LDPE)s,
Low-molecular-weight maleation polybutadiene 1-10 part,
Initator 0.1-0.2 part.
3. polycthylene grafted thing according to claim 1 and 2, is characterized in that, the melt index of described low density polyethylene (LDPE) is at 10-50g/10min.
4. polycthylene grafted thing according to claim 1 and 2, is characterized in that, the relative molecular mass of described low-molecular-weight maleation polybutadiene is 1000-5000, and the content of maleic anhydride is 6-11%.
5. polycthylene grafted thing according to claim 1 and 2, is characterized in that, described initator is peroxide or azo-initiator.
6. polycthylene grafted thing according to claim 5, is characterized in that, described initator is selected from cumyl peroxide, dibenzoyl peroxide, di-tert-butyl peroxide, two tertiary amyl peroxide or azo-bis-isobutyl cyanides.
7. the preparation method of a polycthylene grafted thing, it is characterized in that: polyethylene is mixed with after low-molecular-weight maleation polybutadiene, initator metering, mixed material melt extrudes on screw extruder at the temperature of 160 DEG C～190 DEG C, product, through cooling, granulation, makes described polycthylene grafted thing.
8. the preparation method of polycthylene grafted thing according to claim 7, is characterized in that: in described method, mixed material comprises following component:
100 parts of low density polyethylene (LDPE)s,
Low-molecular-weight maleation polybutadiene 1-10 part,
Initator 0.1-0.2 part.
9. according to the preparation method of the polycthylene grafted thing described in claim 7 or 8, it is characterized in that: described low density polyethylene (LDPE) melt index is 10-50g/10min, the relative molecular mass of described low-molecular-weight maleation polybutadiene is 1000-5000, the content of maleic anhydride is 6-11%, and described initator is cumyl peroxide, dibenzoyl peroxide, di-tert-butyl peroxide, two tertiary amyl peroxide or azo-bis-isobutyl cyanides.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN110144243A (en) * | 2019-05-30 | 2019-08-20 | 重庆伊泰鹏方合成新材料研究院有限公司 | Modified Fischer-Tropsch wax rubber and preparation method thereof |
| CN113166319A (en) * | 2018-11-30 | 2021-07-23 | 陶氏环球技术有限责任公司 | Ethylene-based polymer composition with branching and process for producing the same |
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| WO2003025037A2 (en) * | 2001-09-19 | 2003-03-27 | Exxonmobil Chemical Patents Inc. | Adhesive components and process for manufacture |
| US20070232170A1 (en) * | 2005-12-22 | 2007-10-04 | Atwood Kenneth B | Polyester and modified fluoropolymer blends |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN113166319A (en) * | 2018-11-30 | 2021-07-23 | 陶氏环球技术有限责任公司 | Ethylene-based polymer composition with branching and process for producing the same |
| CN110144243A (en) * | 2019-05-30 | 2019-08-20 | 重庆伊泰鹏方合成新材料研究院有限公司 | Modified Fischer-Tropsch wax rubber and preparation method thereof |
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