CN101200579A - Natural fibre reinforced polylactic acid composite material and method for making same - Google Patents
Natural fibre reinforced polylactic acid composite material and method for making same Download PDFInfo
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- CN101200579A CN101200579A CNA2007101716606A CN200710171660A CN101200579A CN 101200579 A CN101200579 A CN 101200579A CN A2007101716606 A CNA2007101716606 A CN A2007101716606A CN 200710171660 A CN200710171660 A CN 200710171660A CN 101200579 A CN101200579 A CN 101200579A
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
- B29C—SHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
- B29C48/00—Extrusion moulding, i.e. expressing the moulding material through a die or nozzle which imparts the desired form; Apparatus therefor
- B29C48/25—Component parts, details or accessories; Auxiliary operations
- B29C48/36—Means for plasticising or homogenising the moulding material or forcing it through the nozzle or die
- B29C48/395—Means for plasticising or homogenising the moulding material or forcing it through the nozzle or die using screws surrounded by a cooperating barrel, e.g. single screw extruders
- B29C48/40—Means for plasticising or homogenising the moulding material or forcing it through the nozzle or die using screws surrounded by a cooperating barrel, e.g. single screw extruders using two or more parallel screws or at least two parallel non-intermeshing screws, e.g. twin screw extruders
Abstract
The present invention belongs to the macromolecular material technical field and concretely relates to natural fibre enhanced polylactic acid composite material and a preparation method thereof. The composite material consists of graft modified polylactic acid and the natural fibre. A concrete preparation step is that a polylactic acid matrix is processed for the graft modification, so as to improve the interface combined degree of the natural fibre and the polylactic acid matrix. Firstly, the polylactic acid is processed for the graft reaction with maleic anhydride under the action of an initiator to prepare the graft modified polylactic acid matrix; then the modified polylactic acid and the natural fibre are compounded to obtain biological full-degraded natural fibre enhanced polylactic acid composite material. Compared with pure polylactic acid, the mechanical performance and the thermal performance of the composite material are all improved, and the composite material can be used for preparing the project plastic with rigorous condition requirement. The composite material of the present invention can be degraded completely in the natural environment after being used and wasted and belongs to environmental friendly material.
Description
Technical field
The invention belongs to technical field of polymer materials, be specifically related to a kind of natural fibre reinforced 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.Kobe Steel Ltd mentions in the patent 01109452.4 of calendar year 2001 and adopts natural fiber as fortifying fibre, prepared fiber reinforced thermoplastic resin sheets with the dipping extrusion molding, the shortcoming of this method is that fiber and interlaminar resin combination degree are bad, thereby has influenced performance of composites.After mentioning natural fiber in the patent 200610037894.7 of Toray Fiber Research Institute (China) Co., Ltd. and adopting natural fiber, melt extrude granulation with poly(lactic acid), oxidation inhibitor, nucleator, lubricant with coupling agent treatment.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, must find and bestly improve method between fiber and matrix, 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 object of the present invention is to provide a kind of natural fibre reinforced polylactic acid composite material and preparation method thereof with better mechanical property and thermal characteristics.
The natural fibre reinforced polylactic acid composite material that the present invention proposes is made up of natural fiber, poly(lactic acid), initiator and maleic anhydride, and the weight percent of its component is as follows:
Weight percentages of components wt%
Natural fiber 10～89.8
Poly(lactic acid) 10～89.8
Initiator 0.1～2
Maleic anhydride 0.1～10,
Its total amount satisfies 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 initiator is peroxide initiator or azo-initiator.
Among the present invention; described peroxide initiator is benzoyl peroxide, peroxidation two (2; the 4-dichloro-benzoyl), in diacetyl peroxide, dioctanoyl peroxide or dilauroyl peroxide etc. any, described azo-initiator is Diisopropyl azodicarboxylate or 2,2'-Azobis(2,4-dimethylvaleronitrile).
Among the present invention, described natural fiber in short restriction of natural fiber or the natural macrofiber any.
Among the present invention, described natural fiber be 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.
The present invention proposes the preparation method of natural fibre reinforced polylactic acid composite material, and concrete steps are:
(1) with poly(lactic acid) and natural fiber 30～120 ℃ of following vacuum-dryings 1～24 hour, to remove moisture;
(2) with poly(lactic acid), maleic anhydride and initiator according to the weight ratio uniform mixing, in twin screw extruder, react then, product is through cooling, pelletizing, oven dry, screw speed is 10～250rpm, 150～200 ℃ of extrusion temperatures of reaction.
(3) polydactyl acid that step (2) is obtained and the natural fiber in the step (1) successively add and carry out Compound Machining in the twin screw extruder, and screw speed is 50～250rpm, and extrusion temperature is 150～180 ℃, obtains desired product.
The graft modification of the present invention by the poly(lactic acid) matrix is carried out is to improve the interface combination degree of natural fiber and poly(lactic acid) matrix.The poly(lactic acid) of preparation graft modification earlier matrix carries out polydactyl acid and natural fiber compoundly then, obtains the fully bio-degradable natural fibre reinforced polylactic acid composite material.
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) poly(lactic acid) is carried out 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
Further specify the present invention below by embodiment.
Embodiment 1
1. be that 15 ramee is 45 ℃ of following vacuum-dryings 10 hours, to remove moisture with poly(lactic acid) and length-to-diameter ratio.
With poly(lactic acid), maleic anhydride and benzoyl peroxide according to certain ratio uniform mixing, in twin screw extruder, react then, product through the cooling, pelletizing, the oven dry.Wherein the add-on of maleic anhydride is 3wt%, and the dosage of benzoyl peroxide is 4wt%, and screw speed is 50rpm, 150 ℃ of reaction extrusion temperatures.
3. polydactyl acid that step 2 is obtained and the ramee in the step 1 successively add and carry out Compound Machining in the twin screw extruder, and wherein the weight ratio of poly(lactic acid) and ramee is 1: 9, and screw speed is 50～250rpm, and extrusion temperature is 150 ℃.Obtain ramee/lactic acid composite material.
Embodiment 2
1. be that 5 jute fibre is 30 ℃ of following vacuum-dryings 1 hour, to remove moisture with poly(lactic acid) and length-to-diameter ratio.
With poly(lactic acid), maleic anhydride and initiator peroxidation two (2,4 dichloro benzene formyl) according to certain ratio uniform mixing, in twin screw extruder, react then, product through the cooling, pelletizing, the oven dry.Wherein the add-on of maleic anhydride is 0.1wt%, and the dosage of peroxidation two (2,4 dichloro benzene formyl) is 0.1wt%, and screw speed is 10rpm, 150 ℃ of reaction extrusion temperatures.
3. polydactyl acid that step 2 is obtained and the jute fibre in the step 1 successively add and carry out Compound Machining in the twin screw extruder, wherein the weight ratio of poly(lactic acid) and jute fibre is 2: 9, screw speed is 50rpm, and extrusion temperature is 150 ℃, obtains jute fibre/lactic acid composite material.
Embodiment 3
1. be that 100 flax fiber is 120 ℃ of following vacuum-dryings 24 hours, to remove moisture with poly(lactic acid) and length-to-diameter ratio.
With poly(lactic acid), maleic anhydride and initiator diacetyl peroxide according to certain ratio uniform mixing, in twin screw extruder, react then, product through the cooling, pelletizing, the oven dry.Wherein the add-on of maleic anhydride is 10wt%, and the dosage of initiator is 2wt%, and screw speed is 250rpm, 200 ℃ of reaction extrusion temperatures.
3. polydactyl acid that step 2 is obtained and the flax fiber in the step 1 successively add and carry out Compound Machining in the twin screw extruder, wherein the weight ratio of poly(lactic acid) and flax fiber is 9: 1, screw speed is 250rpm, and extrusion temperature is 180 ℃, obtains flax fiber/lactic acid composite material.
Embodiment 4
1. be that 50 bamboo fibers is 80 ℃ of following vacuum-dryings 12 hours, to remove moisture with poly(lactic acid) and length-to-diameter ratio.
With poly(lactic acid), maleic anhydride and initiator dioctanoyl peroxide according to certain ratio uniform mixing, in twin screw extruder, react then, product through the cooling, pelletizing, the oven dry.Wherein the add-on of maleic anhydride is 5wt%, and the dosage of initiator dioctanoyl peroxide is 1.5wt%, and screw speed is 120rpm, 180 ℃ of reaction extrusion temperatures.
3. polydactyl acid that step 2 is obtained and the bamboo fibers in the step 1 successively add and carry out Compound Machining in the twin screw extruder, wherein the weight ratio of poly(lactic acid) and bamboo fibers is 4: 1, screw speed is 150rpm, and extrusion temperature is 170 ℃, obtains bamboo fibers/lactic acid composite material.
Embodiment 5
1. be that 20 sisal fibers is 60 ℃ of following vacuum-dryings 4 hours, to remove moisture with poly(lactic acid) and length-to-diameter ratio.
With poly(lactic acid), maleic anhydride dilauroyl peroxide and initiator according to certain ratio uniform mixing, in twin screw extruder, react then, product through the cooling, pelletizing, the oven dry.Wherein the add-on of maleic anhydride is 3wt%, and the dosage of initiator dilauroyl peroxide is 0.3wt%, and screw speed is 200rpm, 180 ℃ of reaction extrusion temperatures.
3. polydactyl acid that step 2 is obtained and the sisal fibers in the step 1 successively add and carry out Compound Machining in the twin screw extruder, wherein the weight ratio of poly(lactic acid) and natural fiber is 5: 5, screw speed is 150rpm, and extrusion temperature is 170 ℃, obtains sisal fibers/lactic acid composite material.
Embodiment 6
1. be that 40 ramee and jute fibre are 70 ℃ of following vacuum-dryings 14 hours, to remove moisture with poly(lactic acid) and length-to-diameter ratio.
With poly(lactic acid), maleic anhydride and initiator Diisopropyl azodicarboxylate according to certain ratio uniform mixing, in twin screw extruder, react then, product through the cooling, pelletizing, the oven dry.Wherein the add-on of maleic anhydride is 0.9wt%, and the dosage of initiator Diisopropyl azodicarboxylate is 2wt%, and screw speed is 90rpm, 170 ℃ of reaction extrusion temperatures.
3. polydactyl acid that step 2 is obtained and the ramee in the step 1 and jute fibre assorted fibre successively add and carry out Compound Machining in the twin screw extruder, wherein the weight ratio of poly(lactic acid) and assorted fibre is 4: 6, screw speed is 160rpm, extrusion temperature is 180 ℃, obtains ramie jute assorted fibre/lactic acid composite material.
Embodiment 7
1. be that 85 sisal fibers and bamboo fibers are 850 ℃ of following vacuum-dryings 7 hours, to remove moisture with poly(lactic acid) and length-to-diameter ratio.
With poly(lactic acid), maleic anhydride and initiator 2,2'-Azobis(2,4-dimethylvaleronitrile) according to certain ratio uniform mixing, in twin screw extruder, react then, product through the cooling, pelletizing, the oven dry.Wherein the add-on of maleic anhydride is 4wt%, and the dosage of initiator is 1.5wt%, and screw speed is 100rpm, 190 ℃ of reaction extrusion temperatures.
3. polydactyl acid that step 2 is obtained and the sisal fibers in the step 1 and bamboo fibers assorted fibre successively add and carry out Compound Machining in the twin screw extruder, wherein the weight ratio of poly(lactic acid) and sisal fibers and bamboo fibers assorted fibre is 7: 3, screw speed is 200rpm, extrusion temperature is 170 ℃, obtains sisal hemp bamboo assorted fibre/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 (8)
1. a natural fibre reinforced polylactic acid composite material is characterized in that being made up of natural fiber, poly(lactic acid), initiator and maleic anhydride, and the weight percent of its component is as follows:
Weight percentages of components wt%
Natural fiber 10～89.8
Poly(lactic acid) 10～89.8
Initiator 0.1～2
Maleic anhydride 0.1～10,
Its total amount satisfies 100%.
2. natural fibre reinforced 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
3. natural fibre reinforced polylactic acid composite material according to claim 1 is characterized in that described initiator is peroxide initiator or azo-initiator.
4. natural fibre reinforced polylactic acid composite material according to claim 3; it is characterized in that described peroxide initiator is benzoyl peroxide, peroxidation two (2; the 4-dichloro-benzoyl), in diacetyl peroxide, dioctanoyl peroxide or the dilauroyl peroxide any, described azo-initiator is Diisopropyl azodicarboxylate or 2,2'-Azobis(2,4-dimethylvaleronitrile).
5. natural fibre reinforced polylactic acid composite material according to claim 1, it is characterized in that described natural fiber in short restriction of natural fiber or the natural macrofiber any.
6. natural fibre reinforced polylactic acid composite material according to claim 1 is characterized in that described natural fiber is one to several in ramee, flax fiber, sisal fibers, jute fibre, hemp fibre or the bamboo fibers.
7. natural fibre reinforced polylactic acid composite material according to claim 1, the length-to-diameter ratio that it is characterized in that described natural fiber is 5～100.
8. the preparation method of a natural fibre reinforced polylactic acid composite material as claimed in claim 1 is characterized in that concrete steps are:
(1) with poly(lactic acid) and natural fiber 30～120 ℃ of following vacuum-dryings 1～24 hour, to remove moisture;
(2) with poly(lactic acid), maleic anhydride and initiator according to the weight ratio uniform mixing, in twin screw extruder, react then, product is through cooling, pelletizing, oven dry, screw speed is 10～250rpm, 150～200 ℃ of extrusion temperatures of reaction.
(3) polydactyl acid that step (2) is obtained and the natural fiber in the step (1) successively add and carry out Compound Machining in the twin screw extruder, and screw speed is 50～250rpm, and extrusion temperature is 150～180 ℃, obtains desired product.
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