WO2007137378A2 - Process of confection of polyamide compounds with natural fibers and compounds of polyamides with natural fibers - Google Patents

Process of confection of polyamide compounds with natural fibers and compounds of polyamides with natural fibers Download PDF

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Publication number
WO2007137378A2
WO2007137378A2 PCT/BR2007/000122 BR2007000122W WO2007137378A2 WO 2007137378 A2 WO2007137378 A2 WO 2007137378A2 BR 2007000122 W BR2007000122 W BR 2007000122W WO 2007137378 A2 WO2007137378 A2 WO 2007137378A2
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Prior art keywords
natural fibers
polyamide
fibers
fact
compounds
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PCT/BR2007/000122
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French (fr)
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WO2007137378A3 (en
Inventor
Marco Aurélio DE PAOLI
Karen Kely Godoi Fermoselli
Márcia Aparecida DA SILVA SPINACÉ
Paulo Aparecido Dos Santos
João Carlos GIRIOLI
Original Assignee
Sabic Innovative Plastics South América - Indústria De Comércio De Plásticos Ltda.
Universidade Estadual De Campinas - Unicamp
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Application filed by Sabic Innovative Plastics South América - Indústria De Comércio De Plásticos Ltda., Universidade Estadual De Campinas - Unicamp filed Critical Sabic Innovative Plastics South América - Indústria De Comércio De Plásticos Ltda.
Priority to JP2009511308A priority Critical patent/JP2009537671A/en
Priority to US12/302,135 priority patent/US8066934B2/en
Priority to CN2007800191416A priority patent/CN101563403B/en
Priority to EP07719290A priority patent/EP2021403A2/en
Publication of WO2007137378A2 publication Critical patent/WO2007137378A2/en
Publication of WO2007137378A3 publication Critical patent/WO2007137378A3/en
Priority to US13/291,368 priority patent/US20120053268A1/en

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    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L77/00—Compositions of polyamides obtained by reactions forming a carboxylic amide link in the main chain; Compositions of derivatives of such polymers
    • 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
    • B29C45/00—Injection moulding, i.e. forcing the required volume of moulding material through a nozzle into a closed mould; Apparatus therefor
    • B29C45/0005—Injection moulding, i.e. forcing the required volume of moulding material through a nozzle into a closed mould; Apparatus therefor using fibre reinforcements
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
    • C08J5/00—Manufacture of articles or shaped materials containing macromolecular substances
    • C08J5/04—Reinforcing macromolecular compounds with loose or coherent fibrous material
    • C08J5/045—Reinforcing macromolecular compounds with loose or coherent fibrous material with vegetable or animal fibrous material
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K7/00—Use of ingredients characterised by shape
    • C08K7/02—Fibres or whiskers
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L77/00—Compositions of polyamides obtained by reactions forming a carboxylic amide link in the main chain; Compositions of derivatives of such polymers
    • C08L77/02—Polyamides derived from omega-amino carboxylic acids or from lactams thereof
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
    • C08J2377/00—Characterised by the use of polyamides obtained by reactions forming a carboxylic amide link in the main chain; Derivatives of such polymers
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
    • C08J2377/00—Characterised by the use of polyamides obtained by reactions forming a carboxylic amide link in the main chain; Derivatives of such polymers
    • C08J2377/02—Polyamides derived from omega-amino carboxylic acids or from lactams thereof

Definitions

  • the present Patent Invention has the objective of obtainment, by means of extrusion/injection, a polyamide compound, such as polyamide-6, reinforced with natural fibers.
  • one of the objectives of the present patent is to replace the fibers of inorganic materials, such as, for example, fiberglass, with fibers from organic materials, such as, for example, Curaua fiber in polyamide compounds.
  • Curaua An example of this type of plant is the Curaua (Ananas erectofolius of the species L.B. Smith), which was considered as the ideal substitute of fiberglass for some applications, as it presents a lesser density, cost and abrasiveness on the processing equipment, when compared with fiberglass.
  • Curaua An example of this type of plant is the Curaua (Ananas erectofolius of the species L.B. Smith), which was considered as the ideal substitute of fiberglass for some applications, as it presents a lesser density, cost and abrasiveness on the processing equipment, when compared with fiberglass.
  • the present invention establishes the fact of using a natural fiber to obtain a compound with mechanical properties similar to the one obtained from inorganic loads by means of a continuous process such as extrusion and molding by injection process.
  • the process treated herein allows the obtainment, by means of injection, of finished products with precise and complex dimensional features.
  • the natural fiber of preference is the natural fiber of Curaua, which presents properties similar to that of fiberglass.
  • the fact of the compound with the natural fiber of Curaua presenting suitable mechanical properties combined with a lesser density than the compound with inorganic load is interesting to the automotive industry as manufactured vehicles with lighter parts consume less fuel.
  • the compound in question can also be employed in the civil construction industry.
  • Figures 1A and 1B illustrate an example of finished product, such product being a part of the automobile industry, molded by injection using the compound of polyamides with natural fibers treated herein.
  • the aspect and finishing of the part and its performance demonstrate that it is possible to manufacture a finished product by injection molding using natural fiber as reinforcement.
  • the present patent invention presents two objectives, namely the process of production of the polyamide compounds with natural fibers and the genuine polyamide compounds with natural fibers.
  • the natural fibers, in the forms of A or B, are ground in a cutting (knives) mill until obtainment of mean length between 0.1 to 15 mm;
  • the natural fibers, already ground, are superficially treated with cold plasma of O 2 or N 2 , in a quartz reactor; 1.3) The fibers are treated between an interval of 30 minutes up to 2 hours in a solution of 10% in mass of NaOH (solution with pH approximately equal to 5.0), washed once with water from main water supply, and once with distilled water (w/ pH value about equal to 6.0); and 1.4) Subsequently, the fibers are dried in a kiln at 100° C for 2 hours.
  • the quantity of fibers used is from 10 to 50% in ground fiber mass in relation to the mass of the polymeric matrixes used.
  • the treatment method of natural fiber that produces the compound with better performance is the treatment with oxygen plasma.
  • the polymeric matrixes used are: polyamide-6 without any modification and or polyamide-6 containing about 1 to 10% in poly(ethylene- co-propylene-co-diene) elastomer mass functionalized with anhydrous maleic (EPDM-g-AM).
  • the compound are picked off and molded by injection using temperature profile between 200 and 260° C
  • the polyamide compounds with natural fibers are: The compounds obtained from the process detailed above, for the purpose of testing, injected, and from such injection obtained the trial bodies.
  • the obtained trial bodies were used in traction, flexion, shock, thermal distortion temperature (HDT) and density essays.
  • the trial bodies were characterized using ASTM standards by means of traction trials (ASTM D 638-02), flexion (ASTM D 790-02), impact (ASTM D 256-02), HDT (ASTM D 648-98c) and density (ASTM D 792-00).
  • the values of the mechanical properties and HDT described below refer to the 3 compounds with 80 wt % of polyamide-6 and 20 wt% of Curaua fiber, talc or fiberglass, respectively.
  • the tension values at maximum force ( ⁇ max.) and the Young module under traction (E), obtained were 80 ( ⁇ 1), 73 ( ⁇ 1 ), 101 ( ⁇ 1 ) MPa; and 5.1 ( ⁇ 0.4), 6.7 ( ⁇ 0.6) and 6.5 ( ⁇ 0.5) GPa, respectively.
  • the values of resistance to shock, such as Izod with indentation for three compounds described above were: 9 ( ⁇ 1), 9 ( ⁇ 2) and 7 ( ⁇ 1) J m "1 , respectively, and for shock resistance measures without indentation were of 35 ( ⁇ 2), 58 ( ⁇ 3) and 32 ( ⁇ 4) J rrf 1 , respectively.
  • the values measured for tension at maximum force were: 116 ( ⁇ 2), 114 ( ⁇ 2), 160 ( ⁇ 5) MPa, respectively.
  • the values measured for the Young model under flexion were: 3.7 ( ⁇ 0.1), 4.4 ( ⁇ 0.1), and 5.0 ( ⁇ 0.1) GPa, respectively.
  • the HDT values using 1.82 MPa tension for these compounds were: 186 ( ⁇ 10), 110 ( ⁇ 4), and 194 ( ⁇ 1 ) ° C, respectively; and using 0.45 MPa tension, were: 217 ( ⁇ 1), 206 ( ⁇ 4), and 214 ( ⁇ 1) ° C, respectively.
  • the densities obtained for these three compounds were: 1.18 ( ⁇ 0.01 ), 1.27 ( ⁇ 0.01) and 1.27 ( ⁇ 0.01 ) g cm '3 , respectively.
  • the treatment method of the Curaua fiber, which produces the compound with the best performance is the treatment with oxygen plasma. However, the compound prepared with the Curaua fiber without treatment and polyamide-6 without pre-drying presents performance comparable to that of polyamide-6 loaded with talc.
  • the sweep optical and electronic micrographies showed a good distribution, dispersion and adhesion of the fiber matrix.
  • Figures 1A and 1B show the finished product molded by injection, using the raw material described in this technical report.
  • the aspect and finishing of the parts reinforced with the Curaua fiber are superior to those of parts produced with polyamide-6, reinforced with fiberglass.
  • the performance of the part in standard trials of the automobile industry reveals that it is possible to manufacture a finished product by injection molding using natural fibers as reinforcement.
  • This fiber is a raw material of renewable and biodegradable source for application in the automobile, civil construction industry, etc.
  • the description above of the present invention was presented with the purpose of illustrating and describing. In addition, the description is not intended to limit the invention to the manner by which its reveled herein. Consequently, variations and modifications compatible with the above teachings and the ability or knowledge of the relevant technique, are within the scope of the present invention.

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  • Chemical & Material Sciences (AREA)
  • Health & Medical Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Medicinal Chemistry (AREA)
  • Polymers & Plastics (AREA)
  • Organic Chemistry (AREA)
  • Engineering & Computer Science (AREA)
  • Manufacturing & Machinery (AREA)
  • Materials Engineering (AREA)
  • Mechanical Engineering (AREA)
  • Compositions Of Macromolecular Compounds (AREA)
  • Reinforced Plastic Materials (AREA)
  • Injection Moulding Of Plastics Or The Like (AREA)
  • Treatments For Attaching Organic Compounds To Fibrous Goods (AREA)
  • Chemical Or Physical Treatment Of Fibers (AREA)

Abstract

The present invention relates to a process of production of polyamide compounds with natural fibers and polyamide compounds with natural fibers, establishes the fact of using natural fiber to obtain a compound with mechanical properties close to the one obtained with inorganic loads by means of continuous process with extrusion and molding by injection process; the processes presented allows the obtainment, by means of injection, of finished products with precise dimensional and complex features; the fact that the compound with natural Curauá fiber presenting suitable mechanical properties combined to a lesser density than the compound with inorganic load is interesting to the automotive industry as vehicles manufactured with lighter parts consume less fuel.

Description

Title: "PROCESS OF CONFECTION OF POLYAMIDE COMPOUNDS WITH NATURAL FIBERS AND COMPOUNDS OF POLYAMIDES WITH NATURAL FIBERS"
The present Patent Invention has the objective of obtainment, by means of extrusion/injection, a polyamide compound, such as polyamide-6, reinforced with natural fibers.
Therefore, one of the objectives of the present patent is to replace the fibers of inorganic materials, such as, for example, fiberglass, with fibers from organic materials, such as, for example, Curaua fiber in polyamide compounds.
FUNDAMENTS OF THE INVENTION
The use of synthetic fibers as a reinforcement in polymers has been made by the industry in order to obtain materials with better mechanical performance. However, they have high abrasive power, resulting in wear in equipment used for the processing, in addition to the fact that they are not degradable by exposure to the environment.
There is a growing interest in the use of natural fibers as reinforcement in compounds with thermoplastic matrixes [M. Palabiyik, S. Bahadur. Wear, 253 (2002) 369-376.}, [J. J. Rajesh, J. Bijwe, U.S. Tewari. Journal of Materials Science 36 (2001) 351-356.], [S. -H. Wu, F. -Y. Wang, C. -C. M. Ma, W. -C. Chang, C. -T, Kuo, H. -C. Kuan, W. -J. Chen. Materials Letters 49 (2001) 327-333.], [A. G. Pedroso, L. H. I. Mei, J.A.M. Agnelli, D.S. Rosa. Polymer Testing, 18 (1999) 211-215.], [A.G. Pedroso, LH.I. Mei, J. A. M. Agnelli, D.S. Rosa. Polymer Testing, 21 (2002) 229-232.], [S.V. Joshi, LT. Dr- zal, A. K. Mohanty, S. Arora.], [M.A. Silva Spinace, K.K.G. Fermoselli, M.-A. De Paoli, PPS 2004 Americas Regional Meeting, 2004 Proceedings, Floria- nόpolis, S.C., Brazil, 48-49.] and [A. L., Leao R. Rowell, N. Tavares, Sci. Te- chnol. Polym. Adv. Mater, (1998) 756.].
This interest is due to its low cost and some advantages such as: they are atoxic, obtained from renewable sources, are recyclable, biodegradable, have low density, good mechanical properties and low attrition on processing equipment when compared to inorganic fibers. In addi- tion, the production of inorganic fibers, such as fiberglass for instance, requires large amounts of power, increasing its impact on the environment. However, the hydrophilic nature of natural fibers influences in the properties of a- dhesion due to the weak interfacial interactions between the fiber and the polymeric matrix, affecting the mechanical properties of the compound. A way of improving the adhesion of the fiber with the polymeric matrix is by means of modification of the fiber surface by physical and or chemical methods, or by using coupling agents. Currently, different natural fibers have been studied for the obtainment of these compounds. Among them stands out the fiber extracted from plants belonging to the family of the bromeliace- ous, which are found in the Amazon region. These species do not require soils of high fertility and can be planted in sandy texture soils, but with a high level of organic matter.
An example of this type of plant is the Curaua (Ananas erectofolius of the species L.B. Smith), which was considered as the ideal substitute of fiberglass for some applications, as it presents a lesser density, cost and abrasiveness on the processing equipment, when compared with fiberglass. BRIEF DESCRIPTION OF THE INVENTION Based on the state of the art, and aimed at optimizing it, the present patent of Invention was developed.
The present invention establishes the fact of using a natural fiber to obtain a compound with mechanical properties similar to the one obtained from inorganic loads by means of a continuous process such as extrusion and molding by injection process.
The process treated herein allows the obtainment, by means of injection, of finished products with precise and complex dimensional features. The natural fiber of preference is the natural fiber of Curaua, which presents properties similar to that of fiberglass. The fact of the compound with the natural fiber of Curaua presenting suitable mechanical properties combined with a lesser density than the compound with inorganic load is interesting to the automotive industry as manufactured vehicles with lighter parts consume less fuel.
The compound in question can also be employed in the civil construction industry.
BRIEF DESCRIPTION OF THE FIGURES The preset patent of invention shall be described in detail based on the figures listed below, namely:
Figures 1A and 1B illustrate an example of finished product, such product being a part of the automobile industry, molded by injection using the compound of polyamides with natural fibers treated herein. The aspect and finishing of the part and its performance demonstrate that it is possible to manufacture a finished product by injection molding using natural fiber as reinforcement.
DETAILED DESCRIPTION OF THE INVENTION
As described above, the present patent invention presents two objectives, namely the process of production of the polyamide compounds with natural fibers and the genuine polyamide compounds with natural fibers.
• The production process of the compounds of polyamides with natural fibers
For the confection of the polyamide compounds, preferably polyamide-6, with natural fibers, preferably the fiber of Curaua, it is
^ployed: Natural fibers in bulk form, i.e. without washing, drying and superficial treatment; and
(B) Dry natural fibers for 1 ,5 hours at 100° C in a conventional kiln without superficial treatment. The process of confection of polyamide compounds with natural fibers involves the following stages:
1 ) Preparation of natural fibers. This stage establishes the following sub-stages:
1.1) The natural fibers, in the forms of A or B, are ground in a cutting (knives) mill until obtainment of mean length between 0.1 to 15 mm;
1.2) The natural fibers, already ground, are superficially treated with cold plasma of O2 or N2, in a quartz reactor; 1.3) The fibers are treated between an interval of 30 minutes up to 2 hours in a solution of 10% in mass of NaOH (solution with pH approximately equal to 5.0), washed once with water from main water supply, and once with distilled water (w/ pH value about equal to 6.0); and 1.4) Subsequently, the fibers are dried in a kiln at 100° C for 2 hours.
2. Confection of polyamide compounds with natural fibers. This stage establishes the following sub-stages: 2.1 ) Separate the quantity of natural fibers to be used;
2.2 Homogenize the natural fibers prepared beforehand with the polymeric matrixes; and extrude the compound obtained in sub-stage 2.2.
It is important to mention that the quantity of fibers used is from 10 to 50% in ground fiber mass in relation to the mass of the polymeric matrixes used.
The treatment method of natural fiber that produces the compound with better performance is the treatment with oxygen plasma.
The polymeric matrixes used are: polyamide-6 without any modification and or polyamide-6 containing about 1 to 10% in poly(ethylene- co-propylene-co-diene) elastomer mass functionalized with anhydrous maleic (EPDM-g-AM). The extrusion of the compound obtained in the sub-stage 2.2 should occur in extrusion equipment of single-worm thread type (L/D = 30, D = 32 mm), double-worm thread (L/D = 13, D= 29 mm, co-rotatory, interpenetrating, worm thread with segmented shape), using rotation between 50 to 300 rpm, and temperature profile between 200 and 250° C. After the extrusion the compound are picked off and molded by injection using temperature profile between 200 and 260° C The polyamide compounds with natural fibers. The compounds obtained from the process detailed above, for the purpose of testing, injected, and from such injection obtained the trial bodies.
The obtained trial bodies were used in traction, flexion, shock, thermal distortion temperature (HDT) and density essays. The trial bodies were characterized using ASTM standards by means of traction trials (ASTM D 638-02), flexion (ASTM D 790-02), impact (ASTM D 256-02), HDT (ASTM D 648-98c) and density (ASTM D 792-00).
The results of the traction mechanical trials for the compounds revealed that the addition of natural fibers, treated or not, acts as reinforcement to polyamide-6, as the addition (20 wt %) promotes an increase of up to 300% in the module under traction and 80% in tension in maximum force.
The values of the mechanical properties and HDT described below refer to the 3 compounds with 80 wt % of polyamide-6 and 20 wt% of Curaua fiber, talc or fiberglass, respectively. The tension values at maximum force (σmax.) and the Young module under traction (E), obtained were 80 (± 1), 73 (± 1 ), 101 (± 1 ) MPa; and 5.1 (± 0.4), 6.7 (± 0.6) and 6.5 (± 0.5) GPa, respectively. The values of resistance to shock, such as Izod with indentation for three compounds described above were: 9 (± 1), 9 (± 2) and 7 (± 1) J m"1, respectively, and for shock resistance measures without indentation were of 35 (± 2), 58 (± 3) and 32 (± 4) J rrf1, respectively. The values measured for tension at maximum force were: 116 (± 2), 114 (± 2), 160 (± 5) MPa, respectively. The values measured for the Young model under flexion were: 3.7 (± 0.1), 4.4 (± 0.1), and 5.0 (± 0.1) GPa, respectively. The HDT values using 1.82 MPa tension for these compounds were: 186 (± 10), 110 (± 4), and 194 (± 1 ) ° C, respectively; and using 0.45 MPa tension, were: 217 (± 1), 206 (± 4), and 214 (± 1) ° C, respectively. The densities obtained for these three compounds were: 1.18 (± 0.01 ), 1.27 (± 0.01) and 1.27 (± 0.01 ) g cm'3, respectively. The treatment method of the Curaua fiber, which produces the compound with the best performance is the treatment with oxygen plasma. However, the compound prepared with the Curaua fiber without treatment and polyamide-6 without pre-drying presents performance comparable to that of polyamide-6 loaded with talc. For the compounds prepared with treated Curaua fiber, the performance results are above the one of the respective compounds using talc as load and the specific mechanical properties are comparable to the one of compounds containing fiber glass. Both the values of resistance to shock and to HDT are similar to the compounds containing fiberglass.
The sweep optical and electronic micrographies showed a good distribution, dispersion and adhesion of the fiber matrix. The analysis of the intrinsic viscosity of the polyamide-6, of polyamide-6 with stabilizing additives, and without fibers processed and injected, and of the injected trial bodies of compounds with 20 wt % of Curaua fiber, were: η = 96.59 (± 0.23), η = 98.02 (± 0.66) and η = 97.47 (± 3.03) ml_ g-1 , respectively. Therefore, it was verified that there is no matrix degradation of the polyamide-6 during the processing with or without Curaua fiber. To evaluate the finishing and appearance, a part was injected using a mold provided by a parts company, which is used for producing polyamide parts reinforced with fiberglass, as shown in figures 1 A and 1 B.
Figures 1A and 1B show the finished product molded by injection, using the raw material described in this technical report. The aspect and finishing of the parts reinforced with the Curaua fiber are superior to those of parts produced with polyamide-6, reinforced with fiberglass. The performance of the part in standard trials of the automobile industry reveals that it is possible to manufacture a finished product by injection molding using natural fibers as reinforcement. This fiber is a raw material of renewable and biodegradable source for application in the automobile, civil construction industry, etcThe description above of the present invention was presented with the purpose of illustrating and describing. In addition, the description is not intended to limit the invention to the manner by which its reveled herein. Consequently, variations and modifications compatible with the above teachings and the ability or knowledge of the relevant technique, are within the scope of the present invention.
The modalities described above are aimed at providing a better explanation of the known modes for the practice of the invention and allow the technicians of the area to use the invention in such, or other modalities, and with the modifications necessary by the specific applications, or uses of the present invention. It is the purpose of the present invention to include all of its modifications and variations within the scope described in the report.

Claims

1. "PROCESS OF PRODUCTION OF POLYAMIDE COMPOUNDS WITH NATURAL FIBERS", characterized by the fact of its using: (A) natural fibers in the bulk form and (B) natural fibers dried for 1 ,5 hour at 100° C in conventional kiln without superficial treatment; the process of production of the polyamide compounds with natural fibers involves the following stages:
(1) preparation of natural fibers and
(2) production of polyamide compounds with natural fibers; the stage (1 ) establishes the following sub-stages:
(1.1 ) natural fibers, in the form A as well as B, are ground in a cutting (knives)'mill until obtaining the mean length of 0.1 to 15 mm;
(1.2) the natural fibers, already ground, are superficially treated with cold plasma of O2 or N2 in a quartz reactor; (1.3) the fibers are treated in a solution of 10% in NaOH mass, washed once in water from the main water supply, and once with distilled water; and
(1.4) subsequently, the fibers are dried in a kiln at 100 0C for 2 hours; stage (2) establishes the following sub-stages: (2.1 ) separate the amount of natural fibers to be used;
(2.2) homogenize the natural fibers prepared in advance with the polymeric matrixes; and
(2.3) extrude the compound obtained in sub-stage (2.2).
2. "PROCESS OF PRODUCTION OF POLYAMIDE COM- POUNDS WITH NATURAL FIBERS", according to claim 1 , characterized by the fact that in sub-stage (1.2) the quartz reactor has an RF source of 13.56 MHz, power of 30 W, and pressure of 4 x 10"2 Torr for 15 min; In the sub- stage (1.3), the fibers are treated for a period of 30 min to 2 hours, the solution of 10% in NaOH mass has a pH close to 5.0 and the distilled water has a pH close to 6.
3. "PROCESS OF PRODUCTION OF POLYAMIDE COMPOUNDS WITH NATURAL FIBERS", according to claims 1 , characterized by the fact that the amount of fibers used is of 10 to 50% in ground fiber mass in relation to the mass of the polymeric matrixes used.
4. "PROCESS OF PRODUCTION OF POLYAMIDE COMPOUNDS WITH NATURAL FIBERS", according to claim 1 , characterized by the fact that the polyamide compounds are preferably polyamide-6 and the natural fibers are preferably Curaua fibers.
5. "PROCESS OF PRODUCTION OF POLYAMIDE COMPOUNDS WITH NATURAL FIBERS", according to claims 1 and 4, characterized by the fact that the polyamide matrixes used are: polyamide-6 without any modification, and polyamide-6 containing about 1 to 10% in poly (ethyle- ne-co-propylene-co-diene) elastomer mass, functionalized with anhydrous maleic.
6. "PROCESS OF PRODUCTION OF POLYAMIDE COMPOUNDS WITH NATURAL FIBERS", according to claim 1 , characterized by the fact that the extrusion of the compound obtained in sub-stage (2.2) should take place in extrusion equipment of single- or double-worm thread, using from 50 to 300 rpm and temperature profile of 200 to 250 0C.
7. "POLYAMIDE COMPOUNDS WITH NATURAL FIBERS", establishes a compound formed by 80 wt % of polyamide-6 and 20 wt % of Cu- raua fiber, characterized by the fact of having a density of about 1.18 g cm"3.
8. "POLYAMIDE COMPOUNDS WITH NATURAL FIBERS", characterized by the fact of having an increase of 300% in the module under traction and 80% in tension in maximum force.
9. "POLYAMIDE COMPOUNDS WITH NATURAL FIBERS", cha- racterized by the fact of being applicable in the automobile and civil construction industries.
PCT/BR2007/000122 2006-05-25 2007-05-24 Process of confection of polyamide compounds with natural fibers and compounds of polyamides with natural fibers WO2007137378A2 (en)

Priority Applications (5)

Application Number Priority Date Filing Date Title
JP2009511308A JP2009537671A (en) 2006-05-25 2007-05-24 Formulation of polyamide blends with natural fibers and blends of polyamides with natural fibers
US12/302,135 US8066934B2 (en) 2006-05-25 2007-05-24 Process of confection of polyamide compounds with natural fibers and compounds of polyamides with natural fibers
CN2007800191416A CN101563403B (en) 2006-05-25 2007-05-24 Process of preparation of polyamide compounds with natural fibers and compounds of polyamides with natural fibers
EP07719290A EP2021403A2 (en) 2006-05-25 2007-05-24 Process of confection of polyamide compounds with natural fibers and compounds of polyamides with natural fibers
US13/291,368 US20120053268A1 (en) 2006-05-25 2011-11-08 Process of confection of polyamide compounds with natural fibers and compounds of polyamides with natural fibers

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
BRPI0602097A BRPI0602097B1 (en) 2006-05-25 2006-05-25 process for making natural fiber polyamide composites and natural fiber polyamide composites
BRPI0602097-6 2006-05-25

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US12/302,135 A-371-Of-International US8066934B2 (en) 2006-05-25 2007-05-24 Process of confection of polyamide compounds with natural fibers and compounds of polyamides with natural fibers
US13/291,368 Division US20120053268A1 (en) 2006-05-25 2011-11-08 Process of confection of polyamide compounds with natural fibers and compounds of polyamides with natural fibers

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WO2007137378A3 WO2007137378A3 (en) 2008-05-02

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US9821606B2 (en) 2011-02-03 2017-11-21 Compagnie Generale Des Etablissements Michelin Composite reinforcer sheathed with a layer of polymer that is self-adhesive to rubber
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