CN105713359A - Method for preparing long natural fiber/polylactic acid-based composite material - Google Patents
Method for preparing long natural fiber/polylactic acid-based composite material Download PDFInfo
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- CN105713359A CN105713359A CN201410704612.9A CN201410704612A CN105713359A CN 105713359 A CN105713359 A CN 105713359A CN 201410704612 A CN201410704612 A CN 201410704612A CN 105713359 A CN105713359 A CN 105713359A
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Abstract
The invention discloses a long natural fiber/polylactic acid-based composite material. The material comprises the following components in parts by weight: 60-100 parts of polylactic acid resin, 0-40 parts of natural fiber, 0.01-5 parts of a heat stabilizer, 0-1 part of an anti-oxidant, 0-2 parts of a nucleating agent, and 0-5 parts of a coupling agent. A production method comprises the following steps: drying a substrate polylactic acid resin, natural fiber, the nucleating agent, the heat stabilizer, and the anti-oxidant under vacuum at the temperature of 50-100 DEG C for 5-24 hours, uniformly mixing the components according to the ratio by a high-speed mixer, introducing the natural fiber into a double screw extruder from a fiber addition port, extruding the material at the temperature of 150-210 DEG C, performing air cooling, granulation, and drying to obtain the uniform natural fiber/polylactic acid-based composite material. The material is easily available, the production process is simple, a blending object contains polylactic acid and natural fiber, the material has the advantages of no toxicity and no odor, no volatility, and degradability; no pollution is generated during production, usage and after-usage, and the material develops polylactic acid usage fields of automobile, electron, home decoration and building material.
Description
Technical field
The invention belongs to the field of polymer composite material in material science, relate to a kind of method utilizing natural fiber to prepare long natural fiber/polylactic acid-base composite material.Polylactic acid-base composite material prepared by the present invention, the problem solving tradition natural fibre reinforced polylactic acid lengthization being low, inorganic filler can not be degradable.The performance controllability that method involved in the present invention is simple to operate, prepare material is strong, it is adaptable to laboratory and enterprise's industrialization produce, and this material is a kind of long natural fiber/polylactic acid-base composite material.
Background technology
Along with the development of macromolecular material, petroleum base macromolecular material is widely used in human lives and work.But these material source non-renewable resources, and be difficult to degrade in natural environment, cause the deterioration of the ecological environment and resource scarcity, do not meet the strategy of human kind sustainable development, bring harm to the mankind.In recent years, Wei the biodegradation material deriving from Renewable resource causes people to note widely.
Polylactic acid is unique with living resources for raw material, by the degradable linear aliphatic adoption ester of chemical synthesis process, it derives from Renewable resource, there is good biocompatibility, degradability, higher hot strength and modulus of compressibility, therefore polylactic acid is considered as the substitute of petroleum-based plastics: be applied to general-purpose plastics field, is of great significance for reducing environmental pollution, save petroleum resources and alleviating global greenhouse effect aspect tool.Petroleum resources shortage and environmental pollution have seriously promoted development and the application of non-petroleum base degradable green high polymer.Polylactic acid is a kind of green thermoplastic polyester integrating biological degradability, Bioabsorbable, there is good mechanical strength, elastic modelling quantity and hot formability, catabolite can penetrate into body metabolism, it is widely used in the fields such as medical treatment, pharmacy, agricultural, packing business, service occupation, it is believed that be the degradable polymer having market potential up to now most.But, identical with other macromolecular materials, impact strength lower limit polylactic acid is in aviation.The application in the field such as electronics, automobile, develops the environmental protection polylactic acid with higher toughness and seems particularly urgent for this.
Summary of the invention
It is an object of the invention to for solve inorganic filler strengthen polylactic acid can not degradable and problem that part natural fibre reinforced polylactic acid lengthization is low.
Realizing the object of the invention technical solution is: polylactic acid/natural fiber enhancing modified method, by polylactic resin, natural fiber, nucleator, heat stabilizer, antioxidant vacuum drying also mixes by ratio row, make the matrix moisture content of dried blend lower than 50ppm, then adopt the method melt extruded that blend is injection molded into master body, it is characterized in that the fusing point of matrix polylactic acid is between 150～200 DEG C, the consumption of natural fiber accounts for the 0～45% of blend matrix consumption, melt extrudes temperature 180～205 DEG C.
Component and the components by weight percent number proportioning of a kind of long natural fiber/polylactic acid-base composite material be: polylactic acid 60～100 parts, 0～40 part of natural fiber, heat stabilizer 0.01～5 part；0～1 part of antioxidant；Nucleator 0～2 part；Coupling agent 0～5 part.
The number-average molecular weight of described polylactic acid is 12～200,000
Described natural fiber is selected from one or more in hemp, flax fiber, bamboo hemp fibre, tossa and sisal fiber, and the addition of natural fiber is the 0～40% of gross mass.
Described heat stabilizer is selected from one or more of four [3-(3,5-di-t-butyl) propanoic acid] tetramethylolmethane, three (2,4-di-tert-butyl-phenyl) phosphite esters and (2,4-di-tert-butyl-phenyl) pentaerythritol diphosphites.
Described antioxidant be selected from four [β-(3,5-di-tert-butyl-hydroxy phenyl) propanoic acid] tetramethylolmethane, (3,5-di-tert-butyl-hydroxy phenyl) propanoic acid octadecyl ester or,β-One or more of phenyl (3,5-di-t-butyl-4-hydroxyl) the positive octadecanol ester of propanoic acid.
Described nucleator be selected from modified extrafine talc powder, replace dibenzal sorbitol class, two (4-t-butyl-benzoic acid) aluminium hydroxide one or more.
Described coupling agent is selected from 2-(3,4-epoxycyclohexyl) ethyl trimethoxy silane, 3-aminopropyl triethoxysilane, 3-glycidyl ether oxygen propyl dimethoxysilane or 3-glycidyl ether oxygen propyl trimethoxy silicane one or more.
Detailed description of the invention
Embodiment one
Polylactic acid 80 parts
Tossa 20 parts
Four [3-(3,5-di-t-butyl) propanoic acid] tetramethylolmethane 2 parts
[β-(3,5-di-tert-butyl-hydroxy phenyl) propanoic acid] tetramethylolmethane 0.5 part
Replace dibenzal sorbitol class 0.6 part
3-glycidyl ether oxygen propyl dimethoxysilane 1 part
First it is placed in vacuum drying oven by polylactic resin, natural fiber, heat stabilizer, antioxidant, nucleator, coupling agent 60 DEG C of vacuum dryings 5 hours, and then removal moisture, dried blend is placed on high-speed mixer mix 5～8 minutes, the material mixed is joined in double screw extruder by hopper, through melt blending extrusion, air knife cool drying, pelletize, homogenizing, wherein barrel temperature is set to: leading portion 180 DEG C, 190 DEG C of stage casing, back segment 200 DEG C, screw slenderness ratio 35, head temperature 195 DEG C.
Embodiment two
Polylactic acid 80 parts
Tossa 20 parts
Three (2,4-di-tert-butyl-phenyl) phosphite ester 2 parts
[β-(3,5-di-tert-butyl-hydroxy phenyl) propanoic acid] tetramethylolmethane 0.5 part
Replace dibenzal sorbitol class 0.6 part
3-glycidyl ether oxygen propyl dimethoxysilane 1 part
Process conditions are embodiment one such as
Embodiment three
Polylactic acid 75 parts
Hemp 25 parts
Four [3-(3,5-di-t-butyl) propanoic acid] tetramethylolmethane 2 parts
[β-(3,5-di-tert-butyl-hydroxy phenyl) propanoic acid] tetramethylolmethane 0.5 part
Replace dibenzal sorbitol class 0.6 part
3-glycidyl ether oxygen propyl dimethoxysilane 1 part
Process conditions are embodiment one such as
Embodiment four
Polylactic acid 75 parts
Hemp 25 parts
Four [3-(3,5-di-t-butyl) propanoic acid] tetramethylolmethane 2 parts
(2,4-di-tert-butyl-phenyl) pentaerythritol diphosphites 0.5 part
Replace dibenzal sorbitol class 0.6 part
3-glycidyl ether oxygen propyl dimethoxysilane 1 part
Process conditions are embodiment one such as
Embodiment five
Polylactic acid 70 parts
Sisal fiber 30 parts
Four [3-(3,5-di-t-butyl) propanoic acid] tetramethylolmethane 2 parts
[β-(3,5-di-tert-butyl-hydroxy phenyl) propanoic acid] tetramethylolmethane 0.5 part
Replace dibenzal sorbitol class 0.6 part
3-glycidyl ether oxygen propyl dimethoxysilane 1 part
Process conditions are embodiment one such as
Embodiment six
Polylactic acid 70 parts
Sisal fiber 30 parts
Four [3-(3,5-di-t-butyl) propanoic acid] tetramethylolmethane 2 parts
[β-(3,5-di-tert-butyl-hydroxy phenyl) propanoic acid] tetramethylolmethane 0.5 part
Modified extrafine talc powder 0.6 part
3-glycidyl ether oxygen propyl dimethoxysilane 1 part
Process conditions are embodiment one such as
Embodiment seven
Polylactic acid 85 parts
Bamboo hemp fibre 15 parts
Four [3-(3,5-di-t-butyl) propanoic acid] tetramethylolmethane 2 parts
[β-(3,5-di-tert-butyl-hydroxy phenyl) propanoic acid] tetramethylolmethane 0.5 part
Replace dibenzal sorbitol class 0.6 part
3-glycidyl ether oxygen propyl dimethoxysilane 1 part
Process conditions are embodiment one such as
Embodiment eight
Polylactic acid 85 parts
Bamboo hemp fibre 15 parts
Four [3-(3,5-di-t-butyl) propanoic acid] tetramethylolmethane 2 parts
[β-(3,5-di-tert-butyl-hydroxy phenyl) propanoic acid] tetramethylolmethane 0.5 part
Replace dibenzal sorbitol class 0.6 part
3-aminopropyl triethoxysilane 1 part
Process conditions are embodiment one such as
The performance test results
| Test event | Embodiment one | Embodiment two | Embodiment three | Embodiment four | Embodiment five | Embodiment six | Embodiment seven | Embodiment eight |
| Hot strength (Mpa) | 79 | 76 | 73 | 74 | 69 | 72 | 73 | 72 |
| Bending strength (Mpa) | 112 | 109 | 105 | 109 | 99 | 103 | 94 | 95 |
| Vicat temperature (DEG C) | 89 | 87 | 109 | 114 | 85 | 89 | 115 | 112 |
Claims (8)
1. prepare long natural fiber/polylactic acid-base composite material method for one kind, it is by adding natural fiber, nucleator, heat stabilizer, antioxidant and polylactic acid blend, what better solve tradition natural fiber polydactyl acid can not grow jumping, material matrix can not be degradable etc. a difficult problem.
2. the long natural fiber/polylactic acid-base composite material told according to patent requirements 1, the molecular weight of its PLA resin matrix is chosen for 12 × 104Polylactic resin, account for the 60～100% of oeverall quality.
3., according to the long natural fiber/polylactic acid-base composite material of patent requirements 1, natural fiber is selected from one or more in hemp, flax fiber, bamboo hemp fibre, tossa and sisal fiber.
4. according to the long natural fiber/polylactic acid-base composite material of patent requirements 1, nucleator is selected from modified extrafine talc powder, replaces dibenzal sorbitol class, one or more of two (4-t-butyl-benzoic acid) aluminium hydroxide.
5. according to the long natural fiber/polylactic acid-base composite material of patent requirements 1, heat stabilizer is selected from four [3-(3,5-di-t-butyl) propanoic acid] tetramethylolmethane, three (2,4-di-tert-butyl-phenyl) one or more of phosphite ester and double; two (2,4-di-tert-butyl-phenyl) pentaerythritol diphosphites.
6. according to the long natural fiber/polylactic acid-base composite material of patent requirements 1, antioxidant be selected from four [β-(3,5-di-tert-butyl-hydroxy phenyl) propanoic acid] tetramethylolmethane, (3,5-di-tert-butyl-hydroxy phenyl) propanoic acid octadecyl ester or,β-One or more of phenyl (3,5-di-t-butyl-4-hydroxyl) the positive octadecanol ester of propanoic acid.
7. according to the long natural fiber/polylactic acid-base composite material of patent requirements 1, coupling agent is selected from 2-(3,4-epoxycyclohexyl) ethyl trimethoxy silane, 3-aminopropyl triethoxysilane, 3-glycidyl ether oxygen propyl dimethoxysilane or 3-glycidyl ether oxygen propyl trimethoxy silicane.
8. the long natural fiber according to patent requirements 1/polylactic acid based complex method, its feature with comprise the following steps: by proportioning by polylactic acid, nucleator, heat stabilizer, 50～100 DEG C of vacuum drying 5～24h of antioxidant, mixed 3～5 minutes by high-speed mixer, then pass through double screw extruder, natural fiber is added by glass fiber opening, the temperature of double screw extruder is set to a district: 170～180 DEG C, 2nd district: 175～185 DEG C, 3rd district: 180～190 DEG C, 4th district: 180～200 DEG C, 5th district: 185～195 DEG C, 6th district: 190～200 DEG C, 7th district: 195～205 DEG C, 8th district: 200～210 DEG C, 9th district: 200～210 DEG C, tenth district: 200～210 DEG C, head: 195～205 DEG C, engine speed 150～350rpm, subsidiary engine rotating speed 7～15rmp.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110218427A (en) * | 2019-06-28 | 2019-09-10 | 王新华 | A kind of high strength easy-to-degrade antibacterial environment protection poly-lactic acid material |
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| CN101003667A (en) * | 2006-01-20 | 2007-07-25 | 东丽纤维研究所（中国）有限公司 | Composite material of poly lactic acid / natural faric, and production method |
| CN101020781A (en) * | 2007-04-02 | 2007-08-22 | 中国科学院长春应用化学研究所 | Heat resistant polylactic acid-base composite material and its prepn process |
| CN101200581A (en) * | 2006-12-13 | 2008-06-18 | 第一毛织株式会社 | Natural fiber-reinforced polylatic acid-based resin composition |
| CN103509317A (en) * | 2012-06-28 | 2014-01-15 | 上海杰事杰新材料(集团)股份有限公司 | Natural fiber/polylactic acid composite material and preparation method thereof |
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- 2014-11-30 CN CN201410704612.9A patent/CN105713359A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101003667A (en) * | 2006-01-20 | 2007-07-25 | 东丽纤维研究所（中国）有限公司 | Composite material of poly lactic acid / natural faric, and production method |
| CN101200581A (en) * | 2006-12-13 | 2008-06-18 | 第一毛织株式会社 | Natural fiber-reinforced polylatic acid-based resin composition |
| CN101020781A (en) * | 2007-04-02 | 2007-08-22 | 中国科学院长春应用化学研究所 | Heat resistant polylactic acid-base composite material and its prepn process |
| CN103509317A (en) * | 2012-06-28 | 2014-01-15 | 上海杰事杰新材料(集团)股份有限公司 | Natural fiber/polylactic acid composite material and preparation method thereof |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110218427A (en) * | 2019-06-28 | 2019-09-10 | 王新华 | A kind of high strength easy-to-degrade antibacterial environment protection poly-lactic acid material |
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