CN101735537A - Blended material of ethylene-vinyl alcohol copolymer and high-density polyethylene and method for preparing same - Google Patents
Blended material of ethylene-vinyl alcohol copolymer and high-density polyethylene and method for preparing same Download PDFInfo
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- CN101735537A CN101735537A CN200910214042A CN200910214042A CN101735537A CN 101735537 A CN101735537 A CN 101735537A CN 200910214042 A CN200910214042 A CN 200910214042A CN 200910214042 A CN200910214042 A CN 200910214042A CN 101735537 A CN101735537 A CN 101735537A
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Abstract
The invention belongs to the technical field of blending processing of copolymers and discloses a blended material of an ethylene-vinyl alcohol copolymer and high-density polyethylene. The blended material comprises the following components in percentage by weight: 50.0 to 80.1 percent of ethylene-vinyl alcohol copolymers, 10.0 to 30.0 percent of high-density polyethylene, 5.0 to 15.0 percent of flexibilizer, 4.8 to 15 percent of compatilizer, and 0.1 to 1.0 percent of antioxidant. The invention also discloses a method for preparing the blended material. The blended material has high gas resisting property of EVOH as well as high moisture resisting property of HDPE; the product cost is effectively lowered; the EVOH/HDPE blended material is good in toughness, the normal-temperature and the low-temperature impact strengths of the EVOH/HDPE blended material are obviously higher than those of the EVOH, and the application range of EVOH is widened.
Description
Technical field
The invention belongs to the polymer blending processing technique field, be specifically related to a kind of ethylene-vinyl alcohol copolymer and high density polyethylene(HDPE) intermingling material and preparation method thereof.
Background technology
Ethylene-vinyl alcohol copolymer (EVOH) is a kind of crystalline polymer of chain-like structure, contains great amount of hydroxy group in the molecular chain, makes it have excellent barrier to gas, with polyvinyl dichloride (PVDC) and polyamide (PA) and be called three big barrier resins in the world.The gas barrier property of EVOH is poly 10000 times, is 100 times of PA, and is higher 40 times than PVDC.EVOH not only has excellent gas barrier properties, and its organic chemicals to most of lipid, acids and solvent based also has good barrier.Add its good transparency, glossiness, physical strength, wear resistance and static resistance, make it to be widely used in all kinds of packings, comprise the packing of all food product pack or industrial solvent, chemical pharmacy product and pharmaceuticals.At present, the global annual requirement of EVOH surpasses 90,000 tons, and with the speed increment in every year nearly 10%.But also there are some performance deficiencies in EVOH, and promptly under the humidity condition with higher, barrier property descends, and water absorbability is big, and is more bad than moisture effect with other polymer phases; Compare poor processability, poor toughness with common thermoplastics PP, PE; After being processed into form of film, can producing through repeated deflection and to break and influence barrier property.
Chinese patent CN1050202A discloses a kind of blend composition with the EVOH base that intercepts gas property of thermoformable and/or anti-repeated deflection, and it basic composition is EVOH, PP and compatilizer.Because the shock strength at low temperatures of PP is low, poor toughness is so the application of blend under low temperature condition is subjected to certain restriction.Chinese patent CN101323685A discloses blend film of a kind of EVOH and LLDPE and preparation method thereof, owing to added a certain amount of calcium carbonate masterbatch, and also the content of EVOH is on the low side in the blend, and the barrier property of blend is not good.
Summary of the invention
First purpose of the present invention is at the deficiencies in the prior art part, and a kind of ethylene-vinyl alcohol copolymer and high density polyethylene(HDPE) intermingling material with good toughness and barrier property is provided.
Second purpose of the present invention is to provide the preparation method of this kind intermingling material.
For reaching first purpose, the present invention adopts following technical scheme:
Ethylene-vinyl alcohol copolymer and high density polyethylene(HDPE) intermingling material comprise following components in weight percentage:
Ethylene-vinyl alcohol copolymer 50.0～80.1%
High density polyethylene(HDPE) 10.0～30.0%
Toughner 5.0～15.0%
Compatilizer 4.8～15%
Oxidation inhibitor 0.1～1.0%.
As preferably, the ethene molar content in the described ethylene-vinyl alcohol copolymer generally between 25～50%, more preferably 25～35%.
As preferably, the weight percent of described ethylene-vinyl alcohol copolymer is 60～75%.
As preferably, the melting index of described high density polyethylene(HDPE) under 190 ℃ and 2160 gram loading condictions are 1～50g/min, more preferably 5～10g/min.
As preferably, the weight percent of described high density polyethylene(HDPE) is 12～20%.
As preferably, described toughner is selected from any in metallocene-polyolefin class elastomerics, ethylene-vinyl acetate copolymer, ethene acetate propylene ester copolymer, the terpolymer EP rubber, or their mixtures of at least two kinds.Preferred toughner is for being the metallocene-polyolefin class elastomerics of main ingredient with the ethylene-octene copolymer.
As preferably, described compatilizer is selected from maleic anhydride grafted polyethylene, maleic anhydride graft metallocene polyolefin elastomers, acrylic acid-grafted polyethylene, acrylic acid-grafted metallocene polyolefin elastomers, in glycidyl methacrylate graft polyethylene, the glycidyl methacrylate graft metallocene polyolefin elastomers any, or their mixtures of at least two kinds.Preferred compatilizer is that percentage of grafting is the maleic anhydride grafted polyethylene of 0.5～1.0wt%.
As preferably, described oxidation inhibitor is Hinered phenols antioxidant or phosphite ester kind antioxidant, or their mixture; Wherein, described Hinered phenols antioxidant comprises four [β-(3, the 5-di-tert-butyl-hydroxy phenyl) propionic acid] pentaerythritol ester, 2,6-di-tert-butyl-4-methy phenol, β-[3, the 5-di-tert-butyl-hydroxy phenyl] propionic acid octadecyl ester, 1,1,3-three [2-methyl-4-hydroxyl-5-tert-butyl-phenyl] butane, β-di-t-butyl-[4-hydroxy phenyl] n-octyl propionate; Described phosphite ester kind antioxidant comprises tricresyl phosphite [2, the 4-di-tert-butyl] ester, Tyox B, thio-2 acid SUNSOFT Q-182S.
For reaching second purpose, the present invention adopts following technical scheme:
The preparation method of ethylene-vinyl alcohol copolymer and high density polyethylene(HDPE) intermingling material as mentioned above, by proportioning ethylene-vinyl alcohol copolymer, high density polyethylene(HDPE), toughner, compatilizer and oxidation inhibitor are joined in the high speed agitator, after high-speed stirring is even material is joined in the forcing machine, through extruding pelletization and dry, promptly obtain ethylene-vinyl alcohol copolymer and high density polyethylene(HDPE) intermingling material.
Ethylene-vinyl alcohol copolymer that obtains by the present invention and high density polyethylene(HDPE) intermingling material compared with prior art have following outstanding advantage and beneficial effect:
1) use the polar monomer grafts to improve the consistency of EVOH and HDPE and elastic body toughening agent, make EVOH be in the layered distribution state in blend, blend had both had the high gas barrier property of EVOH, and the high resistant that has HDPE again is moist.
2) among the present invention owing to used materials such as HDPE on the low side, elastomerics morely, reduced the cost of product effectively.
3) EVOH/HDPE intermingling material good toughness of the present invention, normal temperature and low temperature impact strength have enlarged the range of application of EVOH apparently higher than EVOH.
Embodiment
Further describe the present invention below in conjunction with embodiment.
Ethylene-vinyl alcohol copolymer of the present invention and high density polyethylene(HDPE) intermingling material comprise that weight part is 50.0～80.1% ethylene-vinyl alcohol copolymer, 10.0～30.0% high density polyethylene(HDPE), 5.0～15.0% toughner, 4.8～15% compatilizer and 0.1～1.0% oxidation inhibitor.
Wherein, the ethene molar content in the above-mentioned ethylene-vinyl alcohol copolymer generally between 25～50%, more preferably 25～35%.The preferred weight percent of ethylene-vinyl alcohol copolymer is 60～75%.
Wherein, the above-specified high density polyethylene is 1～50g/min, more preferably 5～10g/min 190 ℃ and the melting index of 2160 grams under the loading condictions.The preferred weight percent of high density polyethylene(HDPE) is 12～20%.
Wherein, above-mentioned toughner is selected from any in metallocene-polyolefin class elastomerics, ethylene-vinyl acetate copolymer, ethene acetate propylene ester copolymer, the terpolymer EP rubber, or their mixtures of at least two kinds.Preferred toughner is for being the metallocene-polyolefin class elastomerics of main ingredient with the ethylene-octene copolymer.
Wherein, above-mentioned compatilizer is selected from maleic anhydride grafted polyethylene, maleic anhydride graft metallocene polyolefin elastomers, acrylic acid-grafted polyethylene, acrylic acid-grafted metallocene polyolefin elastomers, in glycidyl methacrylate graft polyethylene, the glycidyl methacrylate graft metallocene polyolefin elastomers any, or their mixtures of at least two kinds.Preferred compatilizer is that percentage of grafting is the maleic anhydride grafted polyethylene of 0.5～1.0wt%.
Wherein, above-mentioned oxidation inhibitor is Hinered phenols antioxidant or phosphite ester kind antioxidant, or their mixture; Wherein, described Hinered phenols antioxidant comprises four [β-(3, the 5-di-tert-butyl-hydroxy phenyl) propionic acid] pentaerythritol ester, 2,6-di-tert-butyl-4-methy phenol, β-[3, the 5-di-tert-butyl-hydroxy phenyl] propionic acid octadecyl ester, 1,1,3-three [2-methyl-4-hydroxyl-5-tert-butyl-phenyl] butane, β-di-t-butyl-[4-hydroxy phenyl] n-octyl propionate; Described phosphite ester kind antioxidant comprises tricresyl phosphite [2, the 4-di-tert-butyl] ester, Tyox B, thio-2 acid SUNSOFT Q-182S.
Embodiment 1:
The intermingling material components based on weight percentage is calculated: EVOH 50%, HDPE 25%, metallocene polyolefin elastomers is the ENGAGE820010% of LG-DOW company, the maleic anhydride graft metallocene polyolefin elastomers AR-114.8% that Guangzhou Lu Shan novel material limited-liability company produces, oxidation inhibitor four [β-(3, the 5-di-tert-butyl-hydroxy phenyl) propionic acid] pentaerythritol ester 0.2%.Above-mentioned each component except that oxidation inhibitor, is joined in the high-speed mixer and to mix 5 minutes, add again and join in the twin screw extruder after oxidation inhibitor mixes, after extruding pelletization and drying, obtain described blend of the present invention.Wherein the diameter of twin screw extruder is 35mm, and length-to-diameter ratio is 40, and temperature is set: a district～five districts are respectively 150 ℃, 180 ℃, 190 ℃, 200 ℃, 205 ℃, and die head temperature is 200 ℃, and the forcing machine rotating speed is 350rpm.
Embodiment 2:
The intermingling material components based on weight percentage is calculated: EVOH 75%, HDPE 10%, and EVA 10%, the maleic anhydride graft metallocene polyolefin elastomers AR-14.8% that Guangzhou Lu Shan novel material limited-liability company produces, 2,6 di tert butyl 4 methyl phenol 0.2%.The preparation method of intermingling material is with embodiment 1.
Embodiment 3:
The components based on weight percentage of intermingling material is calculated: EVOH 80.1%, HDPE 10%, the metallocene polyolefin elastomers DF7405% of Mitsui company, the maleic anhydride grafted polyethylene HR-14.8% that Guangzhou Lu Shan novel material limited-liability company produces, 2,6 di tert butyl 4 methyl phenol 0.1%.The preparation method of intermingling material is with embodiment 1.
Embodiment 4:
The intermingling material components based on weight percentage is calculated: EVOH 70%, HDPE 15%, metallocene polyolefin elastomers is the ENGAGE820010% of LG-DOW company, the maleic anhydride graft metallocene polyolefin elastomers 4.8% that Guangzhou Lu Shan novel material limited-liability company produces, oxidation inhibitor four [β-(3, the 5-di-tert-butyl-hydroxy phenyl) propionic acid] pentaerythritol ester 0.2%.The preparation method of intermingling material is with embodiment 1.
Embodiment 5:
The intermingling material components based on weight percentage is calculated: EVOH 70%, HDPE 15%, and EVA 10%, the maleic anhydride graft metallocene polyolefin elastomers AR-14.8% that Guangzhou Lu Shan novel material limited-liability company produces, 2,6 di tert butyl 4 methyl phenol 0.2%.The preparation method of intermingling material is with embodiment 1.
Embodiment 6:
The components based on weight percentage of intermingling material is calculated: EVOH 60%, HDPE 20%, the metallocene polyolefin elastomers DF74010% of Mitsui company, the maleic anhydride grafted polyethylene HR-19.8% that Guangzhou Lu Shan novel material limited-liability company produces, 2,6 di tert butyl 4 methyl phenol 0.2%.The preparation method of intermingling material is with embodiment 1.
Embodiment 7:
The intermingling material components based on weight percentage is calculated: EVOH 60%, HDPE 20%, and EVA 10%, the maleic anhydride grafted polyethylene HR-19.8% that Guangzhou Lu Shan novel material limited-liability company produces, oxidation inhibitor four [β-(3, the 5-di-tert-butyl-hydroxy phenyl) propionic acid] pentaerythritol ester 0.2%.The preparation method of intermingling material is with embodiment 1.
With the intermingling material particle that obtains in the foregoing description, after the blowing film forming, test barrier, the result is as follows:
| Performance | Unit | ??EVOH | Example 1 | Example 2 | Example 3 | Example 4 | Example 5 | Example 6 | Example 7 |
| OTR oxygen transmission rate | ?cm 3/m 2·24hr·atm | ??1.2 | ??1.51 | ??1.32 | ??1.27 | ??1.28 | ??1.27 | ??1.35 | ??1.39 |
| The dimethylbenzene rate of permeation | ?g/100in 2/24hr | ??0.07 | ??0.09 | ??0.08 | ??0.07 | ??0.07 | ??0.08 | ??0.08 | ??0.08 |
| The trichloromethane rate of permeation | ?g/100in 2/24hr | ??0.13 | ??0.22 | ??0.20 | ??0.17 | ??0.17 | ??0.20 | ??0.22 | ??0.20 |
| Shock strength (23 ℃) | ?J/m | ??10 | ??88 | ??81 | ??73 | ??80 | ??76 | ??88 | ??80 |
| Shock strength (5 ℃) | ?J/m | ??/ | ??46 | ??40 | ??35 | ??40 | ??39 | ??46 | ??42 |
Wherein, the ethylene content of EVOH is 32%.During the OTR oxygen transmission rate test, film thickness=15 μ m.
Dimethylbenzene and trichloromethane rate of permeation test condition: 20 ℃, 65%RH, film thickness=20 μ m.
This shows that the barrier property of blend is very nearly the same with pure EVOH, but the shock strength under normal temperature and low-temperature condition significantly improves, and shows that blend has better toughness than EVOH.
Claims (10)
1. ethylene-vinyl alcohol copolymer and high density polyethylene(HDPE) intermingling material is characterized in that, comprise following components in weight percentage:
Ethylene-vinyl alcohol copolymer 50.0～80.1%
High density polyethylene(HDPE) 10.0～30.0%
Toughner 5.0～15.0%
Compatilizer 4.8～15%
Oxidation inhibitor 0.1～1.0%.
2. intermingling material according to claim 1 is characterized in that, the ethene molar content in the described ethylene-vinyl alcohol copolymer is 25～35%.
3. intermingling material according to claim 1 is characterized in that, the weight percent of described ethylene-vinyl alcohol copolymer is 60～75%.
4. intermingling material according to claim 1 is characterized in that, the melting index of described high density polyethylene(HDPE) is 5～10g/min.
5. intermingling material according to claim 1 is characterized in that, the weight percent of described high density polyethylene(HDPE) is 12～20%.
6. intermingling material according to claim 1, it is characterized in that, described toughner is selected from any in metallocene-polyolefin class elastomerics, ethylene-vinyl acetate copolymer, ethene acetate propylene ester copolymer, the terpolymer EP rubber, or their mixtures of at least two kinds.
7. intermingling material according to claim 1, it is characterized in that, described compatilizer is selected from maleic anhydride grafted polyethylene, maleic anhydride graft metallocene polyolefin elastomers, acrylic acid-grafted polyethylene, acrylic acid-grafted metallocene polyolefin elastomers, in glycidyl methacrylate graft polyethylene, the glycidyl methacrylate graft metallocene polyolefin elastomers any, or their mixtures of at least two kinds.
8. intermingling material according to claim 7 is characterized in that, described compatilizer is that percentage of grafting is the maleic anhydride grafted polyethylene of 0.5～1.0wt%.
9. intermingling material according to claim 1 is characterized in that, described oxidation inhibitor is Hinered phenols antioxidant or phosphite ester kind antioxidant, or their mixture; Wherein, described Hinered phenols antioxidant comprises four [β-(3, the 5-di-tert-butyl-hydroxy phenyl) propionic acid] pentaerythritol ester, 2,6-di-tert-butyl-4-methy phenol, β-[3, the 5-di-tert-butyl-hydroxy phenyl] propionic acid octadecyl ester, 1,1,3-three [2-methyl-4-hydroxyl-5-tert-butyl-phenyl] butane, β-di-t-butyl-[4-hydroxy phenyl] n-octyl propionate; Described phosphite ester kind antioxidant comprises tricresyl phosphite [2, the 4-di-tert-butyl] ester, Tyox B, thio-2 acid SUNSOFT Q-182S.
10. the preparation method of ethylene-vinyl alcohol copolymer and high density polyethylene(HDPE) intermingling material according to claim 1, it is characterized in that, by proportioning ethylene-vinyl alcohol copolymer, high density polyethylene(HDPE), toughner, compatilizer and oxidation inhibitor are joined in the high speed agitator, after high-speed stirring is even material is joined in the forcing machine, through extruding pelletization and dry, promptly obtain ethylene-vinyl alcohol copolymer and high density polyethylene(HDPE) intermingling material.
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| CN104448477A (en) * | 2014-11-19 | 2015-03-25 | 河南联塑实业有限公司 | High-oxygen-resistant PE gas pipe material and application thereof to high-oxygen-resistant PE gas pipe |
| CN107298782A (en) * | 2017-06-28 | 2017-10-27 | 天津海晶塑料制品有限公司 | A kind of polyethylene with good gas barrier property and preparation method thereof |
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| CN108329564A (en) * | 2018-02-12 | 2018-07-27 | 贵州凯科特材料有限公司 | A kind of high-barrier polythene material and preparation method thereof |
| CN109895351A (en) * | 2019-03-14 | 2019-06-18 | 泉州市信贵机械设备有限公司 | The preparation method of the multilayer materials of high barrier |
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| CN111499960A (en) * | 2020-05-08 | 2020-08-07 | 四川省宏源防水工程有限公司 | Preparation and application of high-resilience EPO (erythropoietin) high polymer material and waterproof board for gas tunnel |
| CN112297277A (en) * | 2020-09-15 | 2021-02-02 | 南京林业大学 | Preparation method of bamboo nanofiber/polyethylene multilayer composite gas barrier material |
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- 2009-12-22 CN CN200910214042A patent/CN101735537A/en active Pending
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| CN104448477A (en) * | 2014-11-19 | 2015-03-25 | 河南联塑实业有限公司 | High-oxygen-resistant PE gas pipe material and application thereof to high-oxygen-resistant PE gas pipe |
| JPWO2018062126A1 (en) * | 2016-09-30 | 2019-07-11 | 株式会社フジシールインターナショナル | Spout with pouch |
| CN108264867A (en) * | 2016-12-30 | 2018-07-10 | 上海邦中新材料有限公司 | A kind of binding resin with barrier property and its preparation method and application |
| CN107298782A (en) * | 2017-06-28 | 2017-10-27 | 天津海晶塑料制品有限公司 | A kind of polyethylene with good gas barrier property and preparation method thereof |
| CN107400275A (en) * | 2017-07-14 | 2017-11-28 | 成都新柯力化工科技有限公司 | A kind of high-barrier composite plastic that can be directly blow molded and preparation method |
| CN108329564A (en) * | 2018-02-12 | 2018-07-27 | 贵州凯科特材料有限公司 | A kind of high-barrier polythene material and preparation method thereof |
| JP2019214695A (en) * | 2018-06-08 | 2019-12-19 | 日本クロージャー株式会社 | Injection molding |
| WO2019235222A1 (en) * | 2018-06-08 | 2019-12-12 | 日本クロージャー株式会社 | Resin composition for injection molding |
| US11459450B2 (en) | 2018-06-08 | 2022-10-04 | Nippon Closures Co., Ltd. | Resin composition for injection forming |
| CN109895351A (en) * | 2019-03-14 | 2019-06-18 | 泉州市信贵机械设备有限公司 | The preparation method of the multilayer materials of high barrier |
| CN111499960A (en) * | 2020-05-08 | 2020-08-07 | 四川省宏源防水工程有限公司 | Preparation and application of high-resilience EPO (erythropoietin) high polymer material and waterproof board for gas tunnel |
| CN112297277A (en) * | 2020-09-15 | 2021-02-02 | 南京林业大学 | Preparation method of bamboo nanofiber/polyethylene multilayer composite gas barrier material |
| CN116063764A (en) * | 2021-11-01 | 2023-05-05 | 中国石油化工股份有限公司 | Polyethylene composition, preparation method thereof and packaging product |
| CN116063764B (en) * | 2021-11-01 | 2024-03-26 | 中国石油化工股份有限公司 | Polyethylene composition, preparation method thereof and packaging product |
| WO2023125007A1 (en) * | 2021-12-31 | 2023-07-06 | 广东太力科技集团股份有限公司 | High-barrier thermoplastic elastomer, preparation method therefor and use thereof |
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Open date: 20100616 |