CN101121813A - Full-degradation natural fibre/polylactic acid composite material and preparation method thereof - Google Patents
Full-degradation natural fibre/polylactic acid composite material and preparation method thereof Download PDFInfo
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- CN101121813A CN101121813A CNA2007100445062A CN200710044506A CN101121813A CN 101121813 A CN101121813 A CN 101121813A CN A2007100445062 A CNA2007100445062 A CN A2007100445062A CN 200710044506 A CN200710044506 A CN 200710044506A CN 101121813 A CN101121813 A CN 101121813A
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Abstract
The present invention belongs to the technological field of the polymer material, provides and relates to a wholly degradable natural fiber and polylactic composite material and the preparation method. The composite material consists of the surface modified natural fiber and the polylactic acid. The specific preparation steps are: first the natural fiber of a certain long diameter is taken and the natural fiber is soaked in the aqueous solution of the coupling agent for 1 to 100 minutes; then the natural fiber is taken out and dried; thus the surface modified natural fiber can be got. Then the polylactic acid is molded and refined in the two-roller smelting machine at a temperature between 100 and 160 Celsius system; after 1 to 20 minutes, the surface modified natural fiber is added to mix and refine. The mixed products are putinto the mold; the mixed products are compressed and molded in the flat vulcanization machine to make the natural fiber and polylactic composite material. Compared with the pure polylactic acid, the mechanical and thermal performances of the composite material are improved; the composite material can be used in the preparation of the engineering plastics with the demanding conditions. The composite material of the present invention can be wholly degraded in the natural environment after being used and wasted, and the composite material belongs to the environmentally friendly material.
Description
Technical field
The invention belongs to technical field of polymer materials, be specifically related to a kind of full-degradation natural fibre/polylactic acid composite material and preparation method thereof.
Background technology
At present, biodegradated polymer materal seems more and more important in the application aspect biomedical and the environment.Wherein, poly(lactic acid) (PLA) becomes the biodegradated polymer materal that is most widely used because of having degradation property, better biocompatibility, favorable mechanical performance and moulding processability.Poly(lactic acid) plastics, fiber or film are applied in industrial or agricultural and the daily life, can solve " white pollution " problem, satisfy the requirement of environmental protection aspect.Yet PLA matter is hard, toughness is relatively poor, lacks flexibility and elasticity, very easily flexural deformation; Degree of crystallinity is higher, and degradation speed is wayward, does not contain response function group and hydrophilic radical, can not realize the function expansion by chemical reaction.These characteristics of poly(lactic acid) have greatly limited its purposes and result of use, are badly in need of by the method for modification its performance being improved.
Natural fiber have density low, than advantages such as performance height, inexpensive, aboundresources, degradables, natural-fiber composite material enjoys people to pay close attention in recent years, becomes the focus of whole world research.Wherein, flaxen fiber belongs to the high-performance natural vegetable fibre owing to content of cellulose height, intensity height, and many research institutions have carried out the research to the flaxen fiber reinforced composite.Natural fiber is a kind of as natural fiber, and China is the natural main place of production, and output accounts for more than 90% of the world, and natural fiber content of cellulose height, intensity height belong to the high-performance natural vegetable fibre.Can be used as enhancement component and prepare matrix material, improve the performance of poly(lactic acid).
Adopt natural fiber as strongthener, the research domestic and international research of preparation natural fiber reinforced composite has been done many work, and some has had good application in industry.Germany BASF AG adopts the jute reinforced polypropylene compound material to produce the car inside gadget, inhales the standby wheel cover of noise plate, adopts sisal hemp/compound polyurethane material to produce the sedan door trim panel, inhales the noise plate.As strongthener, poly(lactic acid) prepares matrix material as matrix to K.Oksman etc. (Composites science and technology, 2003,63:1317～1324) in twin screw extruder with flax.With pure poly(lactic acid), the mechanical property of matrix material all increases to some extent relatively, and they adopt vanay as softening agent in experiment, have studied softening agent to effect of material performance, the research surface, and the adding of softening agent has obviously improved the erosion-resisting characteristics of material.(Composites science and technology such as David, 2003,63:1287～1296) use jute as enhancement component, poly(lactic acid) adopts pressure sintering to prepare matrix material as matrix, has studied the influence of processing temperature to composite materials property, when processing temperature during at 210 ℃, heating 3min, the tensile strength of matrix material improves 1 times nearly, can reach 100.5MPa.
At home, universities and colleges such as Zhongshan University, the National University of Defense technology are also studied natural plant fibre and the compound of unsaturated polyester and urethane, break through though obtained some at material mechanical performance, resistance toheat etc., its maximum shortcoming is that it can not degrade fully.Donghua University had once applied for " a kind of preparation method of natural fibre reinforced polylactic acid composite material " in 2005, this patent is mentioned and is adopted poly(lactic acid) and polycaprolactone as matrix, natural fiber is as enhancement component, adopt in-situ polymerization to prepare matrix material, this patent shortcoming is to carry out large-scale industrial production.Develop a kind of degradation material that mechanical property and thermal characteristics are had relatively high expectations that can be used for of excellent performance, and it is simple to design a kind of technology, the preparation method who is fit to suitability for industrialized production is a problem demanding prompt solution.
Summary of the invention
The purpose of this invention is to provide a kind of full-degradation natural fibre/polylactic acid composite material and preparation method thereof with mechanical property and thermal characteristics preferably.
Full-degradation natural fibre/polylactic acid composite material provided by the invention is made up of natural fiber, poly(lactic acid) and coupling agent, and the weight percent of its component is as follows:
Natural fiber 20～79wt%
Poly(lactic acid) 20～79wt%
Coupling agent 1～5wt%.
Among the present invention, described natural fiber can adopt short restriction of natural fiber or natural macrofiber.As in ramee, flax fiber, sisal fibers, jute fibre, hemp fibre or the bamboo fibers etc. one or more.
Among the present invention, the length-to-diameter ratio of described natural fiber is 5～100.
Among the present invention, the weight-average molecular weight of described poly(lactic acid) is 1 * 10
5～3 * 10
5
Among the present invention, described coupling agent is a silane coupling agent.Comprise KH-550 (γ-An Bingjisanyiyangjiguiwan), KH-560 (γ-(2,3-epoxy third oxygen) propyl trimethoxy silicane), KH-570 (γ-(methacryloxy) propyl trimethoxy silicane), KH-590 (γ-thiopropyl Trimethoxy silane), A-143 (γ-r-chloropropyl trimethoxyl silane), A-150 (vinyl trichloro silane), A-151 (vinyltriethoxysilane), A-171 (vinyltrimethoxy silane) or A-172[vinyl three ('beta '-methoxy oxyethyl group) silane] etc.
The present invention also proposes the preparation method of full-degradation natural fibre/polylactic acid composite material, by the surface modification to natural fiber, improves natural fiber and poly(lactic acid) interface combination degree.First preparation modified natural fiber carries out this natural fiber and poly(lactic acid) compoundly then, obtains natural fibre reinforced polylactic acid composite material.Concrete steps are as follows:
(1) by proportioning raw materials, get length-to-diameter ratio and be 5～100 natural fiber, impregnated in concentration and be in 0.01wt%～10wt% coupling agent aqueous solution after 1～100 minute, take out, 50～150 ℃ dry 2～30 hours down, obtain surface-treated natural fiber;
(2) poly(lactic acid) is plasticated in two roller mills, plasticating temperature is 100～160 ℃, and the time of plasticating is 1～20 minute;
(3) natural fiber that obtains in the step (1) is joined carry out in the product of step (2) gained mixing, melting temperature is 100～170 ℃, mixing time is 1～20 minute, need when mixing material is cut, to guarantee that mixing of materials is even, wherein natural fiber weight accounts for 1～80% of matrix material gross weight;
(4) material that step (3) is obtained is put into mould, compression molding, and the control mold temperature is 150～200 ℃, and the time is 1～20 minute, and pressure is 5～15MPa, promptly obtains desired product.
The invention has the advantages that:
(1) it is compound to select for use degradable natural fiber and poly(lactic acid) to carry out, and the goods of gained have excellent biological degradability, can effectively solve " white pollution ", satisfy environmental requirement.
(2) Zhi Bei matrix material is than pure poly(lactic acid), and mechanical property and thermal characteristics all increase, and can be used for the harsh relatively engineering plastics field of preparation condition requirement.
(3) adopt coupling agent that natural fiber is carried out surface modification, improved the combination degree between natural fiber and poly(lactic acid), thereby improved performance of composites.
(4) preparation method is simple, is suitable for carrying out suitability for industrialized production.
Embodiment
Embodiment 1
1, getting length-to-diameter ratio is 5 ramee 100g, impregnated in 200g concentration and be in 0.01% silane resin acceptor kh-550 (γ-An Bingjisanyiyangjiguiwan) aqueous solution after 1 minute, take out, 50 ℃ dry 1 hour down, obtain surface-treated ramee.
2, poly(lactic acid) 400g is plasticated under 100 ℃ in two roller mills, the time of plasticating is 1 minute.
3, add the ramee that obtains in the step 1, carry out mixingly, melting temperature is 100 ℃, and mixing time is 1 minute, needs when mixing cut material, to guarantee that mixing of materials is even.
4, the material that step 3 is obtained is put into mould, compression molding in vulcanizing press.The temperature of compression molding is 150 ℃, and the time is 1 minute, and pressure is 5MPa, obtains ramee/lactic acid composite material.
Embodiment 2
1, getting length-to-diameter ratio is 15 jute fibre 200g, impregnated in 400g concentration and be in 1% silane coupling agent KH-560 (γ-(2, the 3-epoxy third oxygen) propyl trimethoxy silicane) aqueous solution after 10 minutes, take out, drying is 10 hours under 100 ℃, obtains surface-treated jute fibre.
2, poly(lactic acid) 200g is plasticated under 120 ℃ in two roller mills, the time of plasticating is 5 minutes.
3, add the jute fibre that obtains in the step 1, carry out mixingly, melting temperature is 130 ℃, and mixing time is 10 minutes, needs when mixing cut material, to guarantee that mixing of materials is even.
4, the material that step 3 is obtained is put into mould, compression molding in vulcanizing press.The temperature of compression molding is 160 ℃, and the time is 5 minutes, and pressure is 8MPa, obtains jute fibre/lactic acid composite material.
Embodiment 3
1, getting length-to-diameter ratio is 40 sisal fibers 400g, impregnated in 300g concentration and be in 5% silane coupling agent H-570 (γ-(methacryloxy) propyl trimethoxy silicane) aqueous solution after 20 minutes, take out, drying is 5 hours under 80 ℃, obtains surface-treated natural fiber.
2, poly(lactic acid) 100g is plasticated under 130 ℃ in two roller mills, the time of plasticating is 10 minutes.
3, add the sisal fibers that obtains in the step 1, carry out mixingly, melting temperature is 140 ℃, and mixing time is 15 minutes, needs when mixing cut material, to guarantee that mixing of materials is even.
4, the material that step 3 is obtained is put into mould, compression molding in vulcanizing press.The temperature of compression molding is 170 ℃, and the time is 10 minutes, and pressure is 10MPa, obtains sisal fibers/lactic acid composite material.
Embodiment 4
1, getting length-to-diameter ratio is 80 bamboo fibers 200g, is immersed in 200g concentration and is in 7% silane coupling agent KH-590 (γ-thiopropyl Trimethoxy silane) aqueous solution after 60 minutes, take out, 130 ℃ dry 20 hours down, obtain surface-treated bamboo fibers.
2, poly(lactic acid) 300g is plasticated under 150 ℃ in two roller mills, the time of plasticating is 15 minutes.
3, add the bamboo fibers that obtains in the step 1, carry out mixingly, melting temperature is 150 ℃, and mixing time is 17 minutes, needs when mixing cut material, to guarantee that mixing of materials is even.
4, the material that step 3 is obtained is put into mould, compression molding in vulcanizing press.The temperature of compression molding is 180 ℃, and the time is 15 minutes, and pressure is 12MPa, obtains bamboo fibers/lactic acid composite material.
Embodiment 5
1, getting length-to-diameter ratio is 100 flax fiber 300g, being immersed in 250g concentration is 10% silane coupling A-172[vinyl three ('beta '-methoxy oxyethyl group) silane] in the aqueous solution after 100 minutes, take out, drying is 30 hours under 150 ℃, obtains surface-treated natural fiber.
2, poly(lactic acid) 200g is plasticated under 160 ℃ in two roller mills, after 20 minutes.
3, add the flax fiber that obtains in the step 1, carry out mixingly, melting temperature is 170 ℃, and mixing time is 20 minutes, needs when mixing cut material, to guarantee that mixing of materials is even.
4, the material that step 3 is obtained is put into mould, compression molding in vulcanizing press.The temperature of compression molding is 200 ℃, and the time is 20 minutes, and pressure is 15MPa, obtains flax fiber/lactic acid composite material.
The above-mentioned description to embodiment is can understand and apply the invention for ease of those skilled in the art.The person skilled in the art obviously can easily make various modifications to these embodiment, and needn't pass through performing creative labour being applied in the General Principle of this explanation among other embodiment.Therefore, the invention is not restricted to the embodiment here, those skilled in the art should be within protection scope of the present invention for improvement and modification that the present invention makes according to announcement of the present invention.
Claims (7)
1. a full-degradation natural fibre/polylactic acid composite material is characterized in that being made up of natural fiber, poly(lactic acid) and coupling agent, and the weight percent of its component is as follows:
Natural fiber 20～79wt%
Poly(lactic acid) 20～79wt%
Coupling agent 1～5wt%.
2. full-degradation natural fibre/polylactic acid composite material according to claim 1 is characterized in that described natural fiber is an one to multiple kind in ramee, flax fiber, sisal fibers, jute fibre, hemp fibre or the bamboo fibers.
3. full-degradation natural fibre/polylactic acid composite material according to claim 1 and 2, the length-to-diameter ratio that it is characterized in that described natural fiber is 5～100.
4. full-degradation natural fibre/polylactic acid composite material according to claim 1, the weight-average molecular weight that it is characterized in that described poly(lactic acid) is 1 * 10
5～3 * 10
5
5. full-degradation natural fibre/polylactic acid composite material according to claim 1 is characterized in that described coupling agent is a silane coupling agent.
6. full-degradation natural fibre/polylactic acid composite material according to claim 5, it is characterized in that described silane coupling agent is γ-An Bingjisanyiyangjiguiwan, γ-(2,3-epoxy third oxygen) propyl trimethoxy silicane), γ-(methacryloxy) propyl trimethoxy silicane), in γ-thiopropyl Trimethoxy silane, γ-r-chloropropyl trimethoxyl silane, vinyl trichloro silane, vinyltriethoxysilane, vinyltrimethoxy silane or vinyl three ('beta '-methoxy oxyethyl group) silane any.
7. the preparation method of a natural fiber/polylactic acid composite material as claimed in claim 1 is characterized in that concrete steps are as follows:
(1) by proportioning raw materials, get length-to-diameter ratio and be 5～100 natural fiber, impregnated in concentration and be in 0.01wt%～10wt% coupling agent aqueous solution after 1～100 minute, take out, 50～150 ℃ dry 2～30 hours down, obtain surface-treated natural fiber;
(2) poly(lactic acid) is plasticated in two roller mills, plasticating temperature is 100～160 ℃, and the time of plasticating is 1～20 minute;
(3) the surface-treated natural fiber that step (1) is obtained joins in the product of step (2) gained, carry out mixing, melting temperature is 100～170 ℃, mixing time is 1～20 minute, when mixing material is cut, wherein natural fiber weight accounts for 1～80% of matrix material gross weight;
(4) material that step (3) is obtained is put into mould, compression molding, and the temperature of compression molding is 150～200 ℃, and the time is 1～20 minute, and pressure is 5～15MPa, promptly obtains desired product.
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| CN101906219A (en) * | 2010-06-25 | 2010-12-08 | 中国林业科学研究院木材工业研究所 | Completely biodegradable bamboo microstructure unit and polylactic acid biomass composite and preparation method thereof |
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