CN1548168A - Continuous carbon fiber reinforced composite material for bone repair - Google Patents
Continuous carbon fiber reinforced composite material for bone repair Download PDFInfo
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- CN1548168A CN1548168A CNA031170889A CN03117088A CN1548168A CN 1548168 A CN1548168 A CN 1548168A CN A031170889 A CNA031170889 A CN A031170889A CN 03117088 A CN03117088 A CN 03117088A CN 1548168 A CN1548168 A CN 1548168A
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Abstract
The continuous carbon fiber reinforced composite material for bone repair is prepared with continuous carbon fiber, continuous carbon fiber felt or continuous carbon fiber, cloth through soaking in methyl methacrylate monomer or pre-polymer and subsequent extruding or bulk molding. The composite material of the present invention includes methyl methacrylate and carbon fiber, and the carbon fiber content is 20-80 wt%. The composite material may be used as the external fracture fixing material, internal fracture fixing material and bone repairing material. The composite material has the features of light weight, no interference on NMR examination and excellent biocompatibility. It may be implanted inside life body without negative effect on tissue, blood, etc.
Description
Technical field
The present invention relates to a kind of material that is used for bone repair, be specifically related to a kind of carbon fiber and strengthen high molecular material.
Technical background
Along with the aging of society and expanding economy and population, the orthopedic injury patient is more and more, increases and improves the demand and the requirement of bone renovating material are continuous.Traditional fracture inside-fixture and exterior fixation bracket material therefor are mainly medical metal, and it has following deficiency usually: (1) metal material rigidity is big and elasticity is little, and fracture end is produced the stress protection, thereby hinders union of fracture; (2) metal quality is excessive, hinders the recovery of patient activity and health to take exercise; (3) metal pair nuclear magnetic resonance image check (MRI) has interference; (4) in vivo the electrochemistry corrosion may take place; (5) expense is comparatively expensive.
Polymer class can absorb the internal fixation bone material, as " application of solid thing in the orthopaedics adsorbable bone folding " (foreign medical science biomedical engineering fascicle, 1997 20 the 6th phases of volume), " mechanical property of carbon fiber enhancement polylactic acid (C/PLA) composite " (material engineering, 2000 the 5th phases), BostmanO.J Bone Joint Surg (Br) 1987,69B; The PLA of bibliographical informations such as 615-619, PGA, PDLLA etc., though be applied to clinically, its intensity is limited, can only be applied to that part is not born a heavy burden or the low district of bearing a heavy burden, proportion is very little for the whole bone injury patient's of hospital fractures.
Carbon fibre reinforcement has features such as low-density, high strength, good biocompatibility as a kind of advanced composite material (ACM).Clinically at present, carbon fiber strengthens thermoplastic has had following aspect to use: be used for external, comprise illness such as making various splint therapy fracture of maxillary, Phalangeal fracture, fracture of zygomatic bone, deformity of dactyl, and make knee joint-ankle-orthopedic remedy instrument for foot and various support, in order to gain in strength, to reduce weight; Making implants, mainly is tooth implant.Chinese patent CN 1040332A and CN 1179937A have disclosed respectively with carbon fiber enhancing polyether-ketone and have strengthened lucite as materials for use in skull-fixing as double-screw bolt shape internal fixator for cervical vertebrae and carbon fiber.U.S. Pat 6,136038, US5,902,839 have all reported with carbon fiber and have strengthened lucite and other acrylic resin as medical material, but described material is owing to adopting the enhanced reason of short fiber, and all existing insufficient strength, material mechanical performance and skeleton has than defectives such as big-differences.
Summary of the invention
One of technical issues that need to address of the present invention provide and a kind ofly can satisfy medical requirement, have easy to process and have the bone repair continuous carbon fibre reinforced composite that the fracture fixation of enough mechanical strengths is used, have than defective such as big-difference, insufficient strength be big with skeleton with the existing material mechanical performance of technology that overcomes the existing defective of existing metal material and above-mentioned its patent disclosure.
Two of the technical issues that need to address of the present invention are to disclose described preparation methods.
Three of the technical issues that need to address of the present invention are to disclose described material is used material with material or fracture internal fixation as external fixation of fracture application.
Technical conceive of the present invention is such:
The present invention obtains the enhanced carbon fibre composite of continuous fiber or felt or cloth by pultrude process or body pouring technology then by continuous carbon fibre or carbon fiber felt or cloth dipping methyl methacrylate (being called for short PMMA, down together) monomer or its performed polymer.
Because the present invention adopts continuous fiber to strengthen methyl methacrylate, so carbon fiber exists with continuous state in the material, in the bone repair goods that made by material of the present invention, the two ends of 95%～100% (quantity percentage ratio) carbon fiber are positioned at product surface 0～0.5mm place.
The enhanced carbon fibre composite of continuous fiber of the present invention or felt or cloth comprises methyl methacrylate and carbon fiber, and wherein, the content of carbon fiber is 20%～80% by weight percentage, and preferred content is 40%～70%.
The carbon fiber of being addressed comprises continuous tow, fiber cloth or fiber felt.
In order to overcome the fragility of PMMA material, reduce the softening temperature of material, composite also comprises the acrylic ester monomer polymer that has flexible chain, the monomer of being addressed comprises one or more in (methyl) butyl acrylate, (methyl) Hexyl 2-propenoate, (methyl) Isooctyl acrylate monomer or (methyl) dodecylacrylate etc., and the amount of adding is 5～30% of a composite gross weight.
Material of the present invention adopts pultrusion method or body pouring procedure to be prepared, and pultrusion method comprises the steps:
(1) under 60～90 ℃ temperature, 0.02～0.3% of the adding monomer weight high-temperature initiator in methyl methacrylate, as azodiisobutyronitrile or dibenzoyl peroxide etc., polymerization obtains the performed polymer that viscosity is the methyl methacrylate of 0.1～3.5Pa.S, the preferred addition of high-temperature initiator is 0.04～0.1%, impregnation liquid of the present invention has lower viscosity, lower viscosity can improve the wellability of fiber, thereby improves the performance of the effect raising fiber between fiber and resin matrix;
(2) in the performed polymer that obtains, add radical initiator; the radical initiator of being addressed comprises di-isopropyl peroxydicarbonate; dibenzoyl peroxide or N; N '-dimethylaniline etc.; addition is 0.01～3% of an amount of monomer; polyreaction can be carried out below the monomer boiling point fast and stably; as required; can in performed polymer, add the acrylic ester monomer that has flexible chain and carry out copolymerization; the monomer of being addressed comprises (methyl) butyl acrylate; (methyl) Hexyl 2-propenoate; in (methyl) Isooctyl acrylate monomer or (methyl) dodecylacrylate etc. one or more, the content of adding is 5～30% of composite gross weight.Flood with continuous tow, fiber cloth, fiber felt traction and by above-mentioned performed polymer with traction machine, and (the polymerizing curable chamber is a tubular conduit to enter the polymerizing curable chamber, the front and rear part temperature difference of passage) first polymeric segment is carried out polymerization, polymerization temperature is 60～100 ℃, polymerization time is 2～30 minutes, the holdup time of fiber in the polymerizing curable chamber can be regulated by the hauling speed of adjusting traction machine, and general hauling speed is 0.15～1.2m/min.
The continuous fiber that is stained with the PMMA resin that (3) will obtain is drawn in the heat treatment section of polymerizing curable chamber and is heat-treated, the temperature of heat treatment section is 110～140 ℃, by the time be 2-20 minute, make that the polymerization of PMMA is complete, obtain the enhanced PMMA resin material of continuous fiber.
(4) the enhanced PMMA resin material of continuous fiber is pulled through the typing of typing die head, die head temperature is 160～220 ℃, obtains the enhanced composite material of polymethyl methacrylate of continuous carbon fibre.
According to the present invention, the fiber of being addressed can carry out surface treatment earlier, and general used inorganic agent is a silane coupler, as methyl allyl acyloxypropyl trimethoxysilane (KH-570), vinyltrimethoxy silane etc.
Inventing resulting composite can carry out pelletizing by Len req, as extruding intermedium, carries out the blend extrusion molding with other polymer.Like this through the fiber of resin-coating, can keep former length and further do not cut off and obtain long fine reinforced composite materials.Also can design difform mould, that pultrusion goes out is bar-shaped, the composite of sheet material, profile shapes or other shapes.Final products comprise bar, sheet material, profile shapes or pellet etc.According to the requirement of product, make fixed support or blade plate and intramedullary needle by machine tooling.
The body pouring procedure is similar with general pouring technology, and the present invention repeats no more.
Continuous carbon fibre reinforced composite of the present invention can be used as external fixation of fracture with material or fracture internal fixation with material or skeleton patching material, as the external fixation of fracture support etc., can be as fracture internal fixation material, as making intramedullary needle or blade plate etc.Material of the present invention has light weight, to characteristics such as nuclear magnetic resonance image check is noiseless.
Thermoplastic composites such as continuous carbon fibre reinforced PMMA of the present invention or other acrylic resin have following characteristics: (1) substrate PMMA resin and the enhanced carbon fiber that is used for all have excellent biological compatibility; (2) can to meet or exceed with steel be the metal material of representative to its intensity index; (3) its elastic modelling quantity is sent out cortical bone near human body, helps the normal healing of fracture site; (4) good anti-fatigue performance is arranged; (5) in light weight, be about same intensity steel weight 1/4th in addition lower; (6) noiseless to MRI (nuclear magnetic resonance, NMR); (7) with low cost, can standardization, stabilisation production.Therefore the continuous carbon fibre reinforced PMMA composite utmost point of the present invention is hopeful to replace to a certain extent metal to become the implants and the exterior fixation bracket material of fixing fracture usefulness.
The inventive method can prepare two dimension, three-dimensional reinforced composite materials such as fiber cloth, fiber felt, has overcome the problem that preceding method cann't be solved, i.e. the dipping problem of fiber cloth, fiber felt etc.
Forming method can pass through the accurately machined manufacturing process of lathe, also can be by the method for mould heat pressure molding.Two kinds of methods all have processing characteristics simple to operation.
Material of the present invention is through biological toxicity evidence, and this material all meets national standard.Have extraordinary biocompatibility, bio-tissue, blood, cerebrospinal fluid are had no adverse reaction no rejection in the long-term implantable bioartificial body.
Description of drawings
Fig. 1 prepares the pultrude process flow chart of continuous fiber intensified response type thermoplastic resin for the present invention.
The specific embodiment
Referring to Fig. 1, the pultrusion preparation method of composite comprises the steps:
Fibre bundle is drawn under the traction of traction machine (8) from creel (1); flood through impregnation chamber (2); impregnated fiber enters first section prepolymerization section (3) of polymerizing curable chamber; the temperature of this section is controlled at 60～100 ℃; material after the pre-polymerization enters second section heat treatment section (4); the temperature of this section is controlled at 110～140 ℃; so that make the unconverted monomer polymerization complete; after this by shaper (5); the temperature of mould is controlled at 160～220 ℃; then by cooling section (6) cooling, then as requested by pelleter (7) pelletizing.
In 90 ℃ water-bath, at the azodiisobutyronitrile of 0.045 part of 40 parts of methyl methacrylates adding, polymerization obtains the performed polymer of methyl methacrylate.The di-isopropyl peroxydicarbonate that in performed polymer, adds 0.3 part, with 0.015 part of azodiisobutyronitrile, be 90 ℃ at polymerization temperature, heat treatment temperature is 140 ℃, the typing die head temperature obtains 60 parts of enhanced composite material of polymethyl methacrylate of continuous carbon fibre by pultrusion under 200 ℃.According to the requirement of product, make fixed support or blade plate and intramedullary needle by machine tooling.Concrete toxicity test result sees Table 1.Mechanical mechanics property sees Table 2 and 3.
Table 1 bone repair is tested with continuous carbon fibre reinforced composite toxicity
| Test event | Technical standard | Test result |
| Cell toxicity test | GB/T16886.5-1997 | Cytotoxicity is 0 grade |
| Hemolytic test | GB/T16175-1996 | No haemolysis |
| Sensitization test (STT) | GB/T16886.10-2000 | No sensitization |
| Ames test | GB/T16886.3-1997 | Histidine defect type Salmonella typhimurium there is not mutagenicity |
| Micronucleus test | GB/T16886.3-1997 | Do not bring out the increase of the many micronucleus in erythrocytes of mouse bone marrow cells |
| External chromosomal aberration test | GB/T16886.3-1997 | Chromosome to the CHL cell does not have mutagenesis |
The mechanical mechanics property of table 2 product of the present invention and common metal implant and human tibia relatively
| This material | The fine polysulfones that strengthens of carbon | Rustless steel | Titanium alloy | The Co-Cr-Mo alloy | Human tibia | |
| Hot strength (MPa) | ??561 | ????458 | ??690 | ????793 | ????448 | ????170 |
| Stretch modulus (GPa) | ??104 | ????- | ??210 | ????110 | ????210 | ????18 |
| Compressive strength (MPa) | ??342 | ????308 | ??- | ????- | ????- | ????- |
| Modulus of compressibility (GPa) | ??157 | ????- | ??- | ????- | ????- | ????- |
| Bending strength (MPa) | ??716 | ????579 | ??- | ????- | ????- | ????- |
| Bending modulus (GPa) | ??43 | ????- | ??- | ????- | ????- | ????- |
| Shear strength (MPa) | ??58 | ????47 | ??- | ????- | ????- | ????- |
| Poisson's ratio μ | ??0.314 | ????0.318 | ??- | ????- | ????- | ????- |
| Extend δ (%) | ??18.2 | ????- | ??12 | ????10 | ????18 | ????6.5 |
Embodiment 2
Ten layers of carbon cloth are overlayed in the fixed mould, add the performed polymer of methyl methacrylate, performed polymer is to add 0.1 part azodiisobutyronitrile to form in 80 ℃ of prepolymerizations in 40 parts of methyl methacrylates and 20 parts of butyl methacrylates.About 20 minutes of evacuation to be to remove bubble, then mould is placed on polyase 13 sky in 50 ℃ the water-bath, handles 3 hours for 80 ℃ then, handled 2 hours at 120 ℃, cooling and demolding obtains 40 parts of enhanced composite material of polymethyl methacrylate of carbon fiber cloth, is pressed into materials for use in skull-fixing by mold hot.
In 95 ℃ water-bath, in 30 parts of methyl methacrylates and 10 parts of butyl methacrylates, add 0.06 part azodiisobutyronitrile, polymerization obtains the performed polymer of methyl methacrylate.Di-isopropyl peroxydicarbonate and 0.02 part of azodiisobutyronitrile of in performed polymer, adding 0.1 part, at polymerization temperature is 90 ℃, heat treatment temperature is 140 ℃, and the typing die head temperature obtains 60 parts of enhanced composite material of polymethyl methacrylate of continuous carbon fibre by pultrusion under 200 ℃.According to the requirement of product, make fixed support or blade plate, intramedullary needle or skeleton patching material by machine tooling.
Ten layers of carbon cloth are overlayed in the fixed mould, the performed polymer that adds methyl methacrylate, performed polymer are to add 0.1 part di-isopropyl peroxydicarbonate and 0.1 part dibenzoyl peroxide forms in 80 ℃ of prepolymerizations in 50 parts of methyl methacrylates and 20 parts of butyl acrylate.About 20 minutes of evacuation is to remove bubble, then mould was placed in 50 ℃ the water-bath polymerization 4 days, handled 3 hours for 80 ℃ then, handled 2.5 hours at 120 ℃, cooling and demolding, obtain 50 parts of enhanced composite material of polymethyl methacrylate of carbon fiber cloth, be pressed into blade plate or skeleton patching material by mold hot.
In 90 ℃ water-bath, at the azodiisobutyronitrile of 0.05 part of 40 parts of methyl methacrylates adding, polymerization obtains the performed polymer of methyl methacrylate.The di-isopropyl peroxydicarbonate that adds 0.02 part in performed polymer is 90 ℃ at polymerization temperature, and heat treatment temperature is 140 ℃, and the typing die head temperature obtains 78 parts of enhanced composite material of polymethyl methacrylate of continuous carbon fibre by pultrusion under 200 ℃.According to the requirement of product, make fixed support or blade plate and intramedullary needle by machine tooling.
Table 3 bone repair material is formed and the performance table
| |
Embodiment 2 | |
|
|
||
| Component (weight portion) | Carbon fiber | ?????60 | ????40 | ????60 | ????50 | ????78 |
| Methyl methacrylate | ?????40 | ????40 | ????30 | ????40 | ????25 | |
| Azodiisobutyronitrile | ?????0.06 | ????0.1 | ????0.08 | ????0.05 | ||
| Dibenzoyl peroxide | ????0.1 | |||||
| Di-isopropyl peroxydicarbonate | ?????0.3 | ????0.3 | ????0.1 | ????0.2 | ||
| Butyl methacrylate | ????20 | ????10 | ||||
| Butyl acrylate | ????10 | |||||
| Test event | Hot strength MPa | ?????561 | ????423 | ????520 | ????500 | ????589 |
| Bending strength MPa | ?????716 | ????552 | ????603 | ????571 | ????575 | |
| Shear strength MPa | ?????58 | ????50 | ????53 | ????51 | ????45 | |
| Bending modulus GPa | ?????45 | ????38 | ????40 | ????41 | ????42 | |
Claims (9)
1. bone repair continuous carbon fibre reinforced composite, its component comprises methyl methacrylate and carbon fiber, it is characterized in that, be positioned at product surface 0～0.5mm place by the two ends of 95%～100% (quantity percent) carbon fiber in its bone repair goods of making.
2. continuous carbon fibre reinforced composite according to claim 1 is characterized in that, the content of carbon fiber is 20%～80% by weight percentage.
3. continuous carbon fibre reinforced composite according to claim 1 is characterized in that, the content of carbon fiber is 40%～70% by weight percentage.
4. continuous carbon fibre reinforced composite according to claim 1 is characterized in that, composite also comprises the acrylic ester monomer polymer that has flexible chain, and the content of adding is 5%～30% of composite gross weight.
5. according to each described continuous carbon fibre reinforced composite of claim 1～4, it is characterized in that the carbon fiber of being addressed comprises continuous tow, fiber cloth or fiber felt.
6. according to the preparation method of each described continuous carbon fibre reinforced composite of claim 1～5, it is characterized in that, comprise the steps:
(1) under 60～90 ℃ temperature, in methyl methacrylate, add high-temperature initiator, polymerization obtains the performed polymer of methyl methacrylate;
(2) in the performed polymer of the methyl methacrylate that obtains, add radical initiator, and carbon fiber is flooded by performed polymer, carbon fibres is heated, carry out polymerization, polymerization temperature is 80～95 ℃, and the time is 2～30 minutes, obtains the compositions of continuous fiber and PMMA resin;
(3) continuous fiber that obtained and the compositions of PMMA resin are heat-treated, temperature is 110～140 ℃, and the time is 2-20 minute;
(4) the enhanced PMMA resin of the continuous fiber behind the heat treatment is pulled through 160～220 ℃ typing die head, obtains the enhanced composite material of polymethyl methacrylate of continuous carbon fibre.
7. the preparation method of continuous carbon fibre reinforced composite according to claim 6 is characterized in that, fiber carries out surface treatment with silane coupler earlier.
8. according to the preparation method of claim 6 or 7 described continuous carbon fibre reinforced composites, it is characterized in that, in performed polymer, add the acrylic ester monomer that has flexible chain and carry out copolymerization, the monomer of being addressed comprises one or more in (methyl) butyl acrylate, (methyl) Hexyl 2-propenoate, (methyl) Isooctyl acrylate monomer or (methyl) dodecylacrylate etc., and the content of adding is 5～30% of composite gross weight.
Each described continuous carbon fibre reinforced composite of claim 1～6 as external fixation of fracture with material or fracture internal fixation with the application of material or skeleton patching material.
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| CNA031170889A CN1548168A (en) | 2003-05-22 | 2003-05-22 | Continuous carbon fiber reinforced composite material for bone repair |
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| CN102783997A (en) * | 2012-08-17 | 2012-11-21 | 刘建 | Portable fracture external fixing rack |
| WO2013056845A2 (en) | 2011-10-21 | 2013-04-25 | Arkema France | Composite material via in-situ polymerization of thermoplastic (meth) acrylic resins and its use |
| CN105153612A (en) * | 2015-08-31 | 2015-12-16 | 苏州莱特复合材料有限公司 | Composite material for orthopedic braces and preparation method of composite material |
| CN106084606A (en) * | 2016-05-30 | 2016-11-09 | 敖然 | Continuous fiber reinforced thermoplastic composite material and preparation method thereof |
| CN108815573A (en) * | 2018-07-16 | 2018-11-16 | 江苏千汇轻量化技术研究院有限公司 | Artificial Bones and joints made of a kind of application thermoplasticity carbon fiber resin matrix composite |
| CN110835807A (en) * | 2019-11-29 | 2020-02-25 | 吉林大学 | Carbon fiber reinforced polyether-ether-ketone fiber composite material and preparation method and application thereof |
| CN113476651A (en) * | 2021-07-12 | 2021-10-08 | 南通美韦德生命科学有限公司 | Antibacterial resin for bone fixation |
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2003
- 2003-05-22 CN CNA031170889A patent/CN1548168A/en active Pending
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| JP2018076510A (en) * | 2011-10-21 | 2018-05-17 | アルケマ フランス | Composite material of thermoplastic (meth)acrylic resin obtained by in situ polymerization, and use of the same |
| FR2981652A1 (en) * | 2011-10-21 | 2013-04-26 | Arkema France | COMPOSITIONS VIA IN-SITU POLYMERIZATION OF METHACRYLIC THERMOPLASTIC RESINS |
| EP2985135A1 (en) | 2011-10-21 | 2016-02-17 | Arkema France | Composite material via in-situ polymerization of thermoplastic (meth) acrylic resins and its use |
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| JP2014530928A (en) * | 2011-10-21 | 2014-11-20 | アルケマ フランス | Composite materials of thermoplastic (meth) acrylic resin obtained by in situ polymerization and their use |
| US10711117B2 (en) | 2011-10-21 | 2020-07-14 | Arkema France | Composite material via in-situ polymerization of thermoplastic (meth)acrylic resins and its use |
| US20180009968A1 (en) * | 2011-10-21 | 2018-01-11 | Arkema France | Composite material via in-situ polymerization of thermoplastic (meth)acrylic resins and its use |
| WO2013056845A2 (en) | 2011-10-21 | 2013-04-25 | Arkema France | Composite material via in-situ polymerization of thermoplastic (meth) acrylic resins and its use |
| WO2013056845A3 (en) * | 2011-10-21 | 2013-07-11 | Arkema France | Composite material via in-situ polymerization of thermoplastic (meth) acrylic resins and its use |
| CN102783997A (en) * | 2012-08-17 | 2012-11-21 | 刘建 | Portable fracture external fixing rack |
| CN102783997B (en) * | 2012-08-17 | 2014-07-16 | 刘建 | Portable fracture external fixing rack |
| CN105153612A (en) * | 2015-08-31 | 2015-12-16 | 苏州莱特复合材料有限公司 | Composite material for orthopedic braces and preparation method of composite material |
| CN106084606A (en) * | 2016-05-30 | 2016-11-09 | 敖然 | Continuous fiber reinforced thermoplastic composite material and preparation method thereof |
| CN108815573A (en) * | 2018-07-16 | 2018-11-16 | 江苏千汇轻量化技术研究院有限公司 | Artificial Bones and joints made of a kind of application thermoplasticity carbon fiber resin matrix composite |
| CN110835807A (en) * | 2019-11-29 | 2020-02-25 | 吉林大学 | Carbon fiber reinforced polyether-ether-ketone fiber composite material and preparation method and application thereof |
| CN113476651A (en) * | 2021-07-12 | 2021-10-08 | 南通美韦德生命科学有限公司 | Antibacterial resin for bone fixation |
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