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CN100462108C - Absorbable periodontal regenerative sheet and its preparing method - Google Patents

Absorbable periodontal regenerative sheet and its preparing method Download PDF

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Publication number
CN100462108C
CN100462108C CNB2005101256887A CN200510125688A CN100462108C CN 100462108 C CN100462108 C CN 100462108C CN B2005101256887 A CNB2005101256887 A CN B2005101256887A CN 200510125688 A CN200510125688 A CN 200510125688A CN 100462108 C CN100462108 C CN 100462108C
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temperature
periodontal
woven
centimetres
minute
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CN1775312A (en
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沈新元
张佩华
郯志清
王文祖
杨庆
陈南梁
赵炯心
李善文
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TIANQING BIOLOGICAL MATERIAL CO Ltd SHANGHAI
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TIANQING BIOLOGICAL MATERIAL CO Ltd SHANGHAI
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Abstract

The present invention discloses an absorbable periodontal regeneration sheet and its preparation method. Said invention adopts a bio-degradable material PGLA as raw material, and utilizes knitting and after-coating process to make the raw material into periodontal regeneration sheet skeleton, its surface is coated with chitin slurry, the mass percentage concentration of chitin coating slurry is 1.0-5.0% and the thickness of said coating layer is 0.01-0.5 mm. The invented PGLA periodontal regeneration sheet can guide the periodontal tissue regeneration, and has good biological compatibility and tissue compatibility.

Description

The preparation method of absorbable periodontal regenerative sheet
One, technical field
The invention relates to a kind of medical material and preparation method thereof, more particularly about a kind of absorbable periodontal regenerative sheet made from the PGLA material and preparation method thereof.
Two, background technology
Bio-medical material is nearly hi tech and new material that grew up in 30 years, is used for diagnosis, reparation, the replacement of human body, organ or promotes its function.Future world is the artificial world, and social population constitutes aging day by day, and artificialization of human organ and tissue is the inevitable course, and the bio-medical material material base of artificial organ and human body substitution material just.Bio-medical material still is each field diagnosis of clinical medicine, the material base of treatment device development and the material base of some important medical skills.Thereby bio-medical material has become the focus of countries in the world research at present, and its growth momentum is just contained.
(periodontal Guided TissueRegeneration GTR) is current up-to-date and state-of-the-art periodontal surgery Therapeutic Method to periodontal guide tissue regeneration technology.This technology is used for the zoopery and the clinical research of periodontal disease therapeutic at first, be used to again promote subsequently osseous tissue reparation, regeneration (promptly induce the osteanagenesis technology, Guide Bone Regeneration, GBR).The bone damaged reparation of quantity not sufficient and other bone, the healing of fracture of its treatment that is applied as periodontal disease, tooth plantation provides a new effective way.Periodontal regenerative sheet is a kind of microporous membrane, and porous surface can make contiguous cell be stretched over easily within the periodontal regenerative sheet, and assurance is organized compound good, reduces crust and grows downwards along root surface.
The total population 1,300,000,000 of China, suffering from the periodontal total number of persons is 65,000,000, accounts for 5% of total population.And the periodontitis pilosity is born in the adult, especially the adult more than 35 years old.The prevalence and the state of an illness can increase or increase the weight of with advancing age, and cause loss of tooth.The prevalence of China adult periodontitis is 50%-60%, and periodontitis has become the first reason of adult's exodontia and old people's absence of tooth.According to investigations, patients with periodontitis mainly concentrates on mid-aged population.At present, the various periodontal treatment technology commonly used and the effect of means are that periodontal is adhering to mostly, are difficult to reach ideal new-attachment of periodontium, and therapeutic effect is unsatisfactory.Periodontal guide tissue regeneration technology and periodontal regenerative sheet have appearred in recent years, for the treatment of periodontitis provides new method and selection.It is predicted that periodontal regenerative sheet still has nearly 49,000,000 number of users only having under the situation of 1% market share, this shows that the development of periodontal regenerative sheet has good economic benefit and social benefit.
At present, the report of relevant Biodegradable material periodontal regenerative sheet development situation seldom, the periodontal regenerative sheet of the guiding paradenlal tissue regeneration of Shi Yonging also is limited to some imports such as Johnson Co. clinically, costs an arm and a leg.It is domestic because the Biodegradable material of guiding paradenlal tissue regeneration also exists many problems at aspects such as the degradation property of material, mechanical property, biocompatibility, therefore, the periodontal regenerative sheet of the guiding paradenlal tissue regeneration that carries out with biodegradated polymer materal also fails to be applied clinical so far.
Three, summary of the invention
The objective of the invention is in order to remedy the deficiency of above-mentioned material, and a kind of periodontal regenerative sheet made from the PGLA Biodegradable material is provided.
Second purpose of the present invention provides a kind of knitting technology braiding periodontal regenerative sheet skeleton, has the required peculiar pore structure of periodontal regenerative sheet.
The 3rd purpose of the present invention provides a kind of periodontal regenerative sheet with the chitin slurry coating.
The 4th purpose of the present invention provides a kind of preparation method of using the periodontal regenerative sheet of chitin serosity degradation material coating.
These and other objects of the present invention will further embody and set forth by following detailed description and explanation.
Periodontal regenerative sheet of the present invention, make the periodontal regenerative sheet skeleton with Biodegradable material PGLA by special weaving and back coating process, at periodontal regenerative sheet skeleton surface-coated chitin serosity (biodegradable), the mass percent concentration of chitin coating agent is 1.0-5.0%, and the thickness of coating is the 0.01-0.5 millimeter.
Further, in periodontal regenerative sheet of the present invention, Biodegradable material PGLA (polymeric polyglycolide-polylactide) is formed by the part by weight copolymerization of 75-90:25-10 by GA (Acetic acid, hydroxy-, bimol. cyclic ester) and LA (lactide), described chitin serosity is a chitosan, and the mass percent concentration of coating agent is 1.0-5.0%.
Periodontal regenerative sheet of the present invention can prepare by the following method, comprises the steps:
A, take by weighing and to absorb polymeric polyglycolide-polylactide, be placed on then in the baking oven to descend dry 15-28 hour in 90-120 ℃, under temperature program(me) control, in screw extruder, make temperature and be 200-230 ℃ melt, spray by spinning head through dosing pump, solidify in cabinet, the medium in the cabinet is an air, and temperature is a room temperature;
B, the as-spun fibre that makes is wound on the bobbin, winding speed be 100-250 rice/minute, as-spun fibre on the bobbin is carried out secondary drawing, first order draft temperature is 60-80 ℃, second level draft temperature is 70-90 ℃, and total stretching ratio is 4.0-7.0 times, thermal finalization in baking oven subsequently, temperature is 90-100 ℃, and the time is 3-10 minute;
C, adopt knitting weft-knitted technology to be woven into knitted fabric on the PGLA yarn, wherein, raw material specification is 5-10tex, loop length is 0.2~0.35 centimetre, the underfill coefficient is 20-40, the vertical 60-90 coil of Density/5 centimetres, the horizontal 40-70 coil of Density/5 centimetres.
D, the knitting skeleton fabric compact structure that will be woven into are finalized the design, and setting temperature is 50-70 ℃, and shaping time is 10-15 minute, carry out coating at last, coating agent is the chitin serosity, and concentration is 1.0-5.0% solution, soak time is 30-40 minute, and coating layer thickness is the 0.01-0.5 millimeter.
Further, periodontal regenerative sheet of the present invention can prepare by the following method, comprises the steps:
A, the ratio that takes by weighing in Acetic acid, hydroxy-, bimol. cyclic ester-lactide are the absorbed polymeric polyglycolide-polylactide of 75:25 copolymerization, be placed in the baking oven following dry 24 hours then in 90 ℃, under temperature program(me) control, in screw extruder, make temperature and be 210 ℃ melt, spray by spinning head through dosing pump, solidify in cabinet, the medium in the cabinet is an air, and temperature is a room temperature;
B, the as-spun fibre that makes is wound on the bobbin, winding speed is 200 meters/minute, as-spun fibre on the bobbin is carried out secondary drawing, first order draft temperature is 70 ℃, second level draft temperature is 80 ℃, and total stretching ratio is 5.0 times, thermal finalization in baking oven subsequently, temperature is 100 ℃, and the time is 5 minutes;
C, adopt knitting weft-knitted technology to be woven into knitted fabric on the PGLA yarn, wherein, raw material specification is 5-10tex, loop length is 0.2~0.35 centimetre, the underfill coefficient is 20-40, the vertical 60-90 coil of Density/5 centimetres, the horizontal 40-70 coil of Density/5 centimetres.
D, the knitting skeleton fabric compact structure that will be woven into are finalized the design, and setting temperature is 70 ℃, and shaping time is 10 minutes, carry out coating at last, coating agent is chitin serosity (Biodegradable material), and concentration is 2.0% solution, soak time is 30 minutes, and coating layer thickness is 0.25 millimeter.
What can select is that periodontal regenerative sheet of the present invention can prepare by the following method, comprises the steps:
A, the ratio that takes by weighing in Acetic acid, hydroxy-, bimol. cyclic ester-lactide are the absorbed polymeric polyglycolide-polylactide of 80:20 copolymerization, be placed in the baking oven following dry 24 hours then in 100 ℃, under temperature program(me) control, in screw extruder, make temperature and be 225 ℃ melt, spray by spinning head through dosing pump, solidify in cabinet, the medium in the cabinet is an air, and temperature is a room temperature;
B, the as-spun fibre that makes is wound on the bobbin, winding speed is 250 meters/minute, as-spun fibre on the bobbin is carried out secondary drawing, first order draft temperature is 75 ℃, second level draft temperature is 85 ℃, and total stretching ratio is 6.0 times, thermal finalization in baking oven subsequently, temperature is 100 ℃, and the time is 4 minutes;
C, adopt knitting weft-knitted technology to be woven into knitted fabric on the PGLA yarn, wherein, raw material specification is 5-10tex, loop length is 0.2~0.35 centimetre, the underfill coefficient is 20-40, the vertical 60-90 coil of Density/5 centimetres, the horizontal 40-70 coil of Density/5 centimetres.
D, the knitting skeleton fabric compact structure that will be woven into are finalized the design, and setting temperature is 50 ℃, and shaping time is 15 minutes, carries out coating at last, and coating agent is the chitin serosity, and concentration is 3.0% solution, and soak time is 35 minutes, and coating layer thickness is 0.35 millimeter.
Be preferably, periodontal regenerative sheet of the present invention can prepare by the following method, comprises the steps:
A, the ratio that takes by weighing in Acetic acid, hydroxy-, bimol. cyclic ester-lactide are the absorbed polymeric polyglycolide-polylactide of 90:10 copolymerization, be placed in the baking oven following dry 24 hours then in 100 ℃, under temperature program(me) control, in screw extruder, make temperature and be 220 ℃ melt, spray by spinning head through dosing pump, solidify in cabinet, the medium in the cabinet is an air, and temperature is a room temperature;
B, the as-spun fibre that makes is wound on the bobbin, winding speed is 250 meters/minute, as-spun fibre on the bobbin is carried out secondary drawing, first order draft temperature is 80 ℃, second level draft temperature is 90 ℃, and total stretching ratio is 7.0 times, thermal finalization in baking oven subsequently, temperature is 100 ℃, and the time is 4 minutes;
C, adopt knitting weft-knitted technology to be woven into knitted fabric on the PGLA yarn, wherein, raw material specification is 5-10tex, loop length is 0.2~0.35 centimetre, the underfill coefficient is 20-40, the vertical 60-90 coil of Density/5 centimetres, the horizontal 40-70 coil of Density/5 centimetres.
D, the knitting skeleton fabric compact structure that will be woven into are finalized the design, and setting temperature is 70 ℃, and shaping time is 10 minutes, carries out coating at last, and coating agent is the chitin serosity, and concentration is 4.0% solution, and soak time is 40 minutes, and coating layer thickness is 0.5 millimeter.
In the present invention, the braiding apparatus of periodontal regenerative sheet is commercially available medical braider, adopts knitting weft-knitted technology to be woven into knitted fabric on the PGLA yarn, and its fabric parameter is as shown in table 1:
Table 1
Raw material specification (tex) Density (vertical/horizontal stroke) (coil/5 centimetre) Loop length (centimetre) The underfill coefficient
Periodontal regenerative sheet 5~10 60~90/40~70 0.2~0.35 20~40
Identical knitting weft-knitted method is all adopted in the development of different model periodontal regenerative sheet, but adopts different technological parameters.
The regeneration synchronised of the degradation cycle of periodontal regenerative sheet of the present invention and periodontal tissue can guide contiguous cell to be stretched within the periodontal regenerative sheet, and assurance is organized compound good, and the good biocompatibility of this material.
Periodontal regenerative sheet of the present invention has passed through the medical apparatus and instruments quality supervision and test center check of Beijing University of National Drug Administration, reaches 95.45% through the clinical experimental study clinical effective rate, good biocompatibility, and safety is stable.
All raw materials of Shi Yonging comprise chitin Biodegradable material (chitin serosity) in the present invention, can buy from market.
In the present invention, refer in particular to as non-, all must be measured, percentage ratio is unit of weight.
Below further specify the present invention by specific embodiment, but embodiment only be used for the explanation, can not limit the scope of the invention.
Four, specific implementation method
Embodiment 1
Take by weighing and to absorb polymeric polyglycolide-polylactide (ratio of Acetic acid, hydroxy-, bimol. cyclic ester-lactide is 75:25), be placed in the baking oven following dry 24 hours then in 90 ℃, under temperature program(me) control, in screw extruder, make temperature and be 210 ℃ melt, spray by spinning head through dosing pump, solidify in cabinet, the medium in the cabinet is an air, and temperature is a room temperature; The as-spun fibre that makes is wound on the bobbin, winding speed is 200 meters/minute, as-spun fibre on the bobbin is carried out secondary drawing, first order draft temperature is 70 ℃, second level draft temperature is 80 ℃, and total stretching ratio is 5.0 times, thermal finalization in baking oven subsequently, temperature is 100 ℃, and the time is 5 minutes; Adopt knitting weft-knitted technology to be woven into knitted fabric on the PGLA yarn, wherein, raw material specification is 7tex, and loop length is 0.28 centimetre, and the underfill coefficient is 30, vertical 70 coils of Density/5 centimetres, horizontal 55 coils of Density/5 centimetres.The knitting skeleton fabric compact structure that is woven into is finalized the design, setting temperature is 70 ℃, shaping time is 10 minutes, carry out coating at last, coating agent is the chitin Biodegradable material, and concentration is 2.0% solution, and soak time is 30 minutes, coating layer thickness is 0.25 millimeter, obtains periodontal regenerative sheet.
Embodiment 2
Take by weighing and to absorb polymeric polyglycolide-polylactide (ratio of Acetic acid, hydroxy-, bimol. cyclic ester-lactide is 80:20), be placed in the baking oven following dry 24 hours then in 100 ℃, under temperature program(me) control, in screw extruder, make temperature and be 225 ℃ melt, spray by spinning head through dosing pump, solidify in cabinet, the medium in the cabinet is an air, and temperature is a room temperature; The as-spun fibre that makes is wound on the bobbin, winding speed is 250 meters/minute, as-spun fibre on the bobbin is carried out secondary drawing, first order draft temperature is 80 ℃, second level draft temperature is 90 ℃, and total stretching ratio is 6.5 times, thermal finalization in baking oven subsequently, temperature is 100 ℃, and the time is 5 minutes; Adopt knitting weft-knitted technology to be woven into knitted fabric on the PGLA yarn, wherein, raw material specification is 8tex, and loop length is 0.30 centimetre, and the underfill coefficient is 25, vertical 80 coils of Density/5 centimetres, horizontal 60 coils of Density/5 centimetres.The knitting skeleton fabric compact structure that is woven into is finalized the design, setting temperature is 50 ℃, shaping time is 15 minutes, carry out coating at last, coating agent is chitin serosity (chitosan, Tianqing Biological Material Co., Ltd., Shanghai produces), concentration is 3.0% solution, soak time is 35 minutes, and coating layer thickness is 0.35 millimeter, obtains periodontal regenerative sheet.
Embodiment 3
Take by weighing and to absorb polymeric polyglycolide-polylactide (ratio of Acetic acid, hydroxy-, bimol. cyclic ester-lactide is 85:15), be placed in the baking oven following dry 24 hours then in 100 ℃, under temperature program(me) control, in screw extruder, make temperature and be 210 ℃ melt, spray by spinning head through dosing pump, solidify in cabinet, the medium in the cabinet is an air, and temperature is a room temperature; The as-spun fibre that makes is wound on the bobbin, winding speed is 100 meters/minute, as-spun fibre on the bobbin is carried out secondary drawing, first order draft temperature is 75 ℃, second level draft temperature is 85 ℃, and total stretching ratio is 6.0 times, thermal finalization in baking oven subsequently, temperature is 100 ℃, and the time is 5 minutes; Adopt knitting weft-knitted technology to be woven into knitted fabric on the PGLA yarn, wherein, raw material specification is 6tex, and loop length is 0.22 centimetre, and the underfill coefficient is 23, vertical 65 coils of Density/5 centimetres, horizontal 45 coils of Density/5 centimetres.The knitting skeleton fabric compact structure that is woven into is finalized the design, and setting temperature is 70 ℃, and shaping time is 10 minutes, carry out coating at last, coating agent is a chitosan, and concentration is 3.5% solution, soak time is 30 minutes, and coating layer thickness is 0.3 millimeter, obtains periodontal regenerative sheet.
Embodiment 4
Take by weighing and to absorb polymeric polyglycolide-polylactide (ratio of Acetic acid, hydroxy-, bimol. cyclic ester-lactide is 90:10), be placed in the baking oven following dry 24 hours then in 100 ℃, under temperature program(me) control, in screw extruder, make temperature and be 215 ℃ melt, spray by spinning head through dosing pump, solidify in cabinet, the medium in the cabinet is an air, and temperature is a room temperature; The as-spun fibre that makes is wound on the bobbin, winding speed is 200 meters/minute, as-spun fibre on the bobbin is carried out secondary drawing, first order draft temperature is 80 ℃, second level draft temperature is 90 ℃, and total stretching ratio is 3.5 times, thermal finalization in baking oven subsequently, temperature is 100 ℃, and the time is 5 minutes; Adopt knitting weft-knitted technology to be woven into knitted fabric on the PGLA yarn, wherein, raw material specification is 9tex, and loop length is 0.32 centimetre, and the underfill coefficient is 38, vertical 85 coils of Density/5 centimetres, horizontal 65 coils of Density/5 centimetres.The knitting skeleton fabric compact structure that is woven into is finalized the design, and setting temperature is 60 ℃, and shaping time is 13 minutes, carry out coating at last, coating agent is a chitosan, and concentration is 3.0% solution, soak time is 40 minutes, and coating layer thickness is 0.35 millimeter, obtains periodontal regenerative sheet.
Embodiment 5
Take by weighing and to absorb polymeric polyglycolide-polylactide (ratio of Acetic acid, hydroxy-, bimol. cyclic ester-lactide is 80:20), be placed in the baking oven following dry 24 hours then in 100 ℃, under temperature program(me) control, in screw extruder, make temperature and be 220 ℃ melt, spray by spinning head through dosing pump, solidify in cabinet, the medium in the cabinet is an air, and temperature is a room temperature; The as-spun fibre that makes is wound on the bobbin, winding speed is 250 meters/minute, as-spun fibre on the bobbin is carried out secondary drawing, first order draft temperature is 75 ℃, second level draft temperature is 85 ℃, and total stretching ratio is 6.5 times, thermal finalization in baking oven subsequently, temperature is 100 ℃, and the time is 5 minutes; Adopt knitting weft-knitted technology to be woven into knitted fabric on the PGLA yarn, wherein, raw material specification is 5-10tex, loop length is 0.2~0.35 centimetre, the underfill coefficient is 20-40, the vertical 60-90 coil of Density/5 centimetres, the horizontal 40-70 coil of Density/5 centimetres.The knitting skeleton fabric compact structure that is woven into is finalized the design, and setting temperature is 70 ℃, and shaping time is 10 minutes, carry out coating at last, coating agent is the chitin serosity, and concentration is 3.0% solution, soak time is 40 minutes, and coating layer thickness is 0.4 millimeter, obtains periodontal regenerative sheet.

Claims (3)

1, a kind of preparation method of absorbable periodontal regenerative sheet is characterized in that comprising the steps:
A, the ratio that takes by weighing in Acetic acid, hydroxy-, bimol. cyclic ester-lactide are the absorbed polymeric polyglycolide-polylactide of 75:25 copolymerization, be placed on then in the baking oven to descend dry 15-28 hour in 90-120 ℃, under temperature program(me) control, in screw extruder, make temperature and be 200-230 ℃ melt, spray by spinning head through dosing pump, solidify in cabinet, the medium in the cabinet is an air, and temperature is a room temperature;
B, the as-spun fibre that makes is wound on the bobbin, winding speed be 100-250 rice/minute, as-spun fibre on the bobbin is carried out secondary drawing, first order draft temperature is 60-80 ℃, second level draft temperature is 70-90 ℃, and total stretching ratio is 4.0-7.0 times, thermal finalization in baking oven subsequently, temperature is 90-100 ℃, and the time is 3-10 minute;
C, adopt knitting weft-knitted technology to be woven into knitted fabric on the PGLA yarn, wherein, raw material specification is 5-10tex, loop length is 0.2~0.35 centimetre, the underfill coefficient is 20-40, the vertical 60-90 coil of Density/5 centimetres, the horizontal 40-70 coil of Density/5 centimetres;
D, the knitting skeleton fabric compact structure that will be woven into are finalized the design, and setting temperature is 50-70 ℃, and shaping time is 10-15 minute, carry out coating at last, coating agent is the chitin serosity, and concentration is 1.0-5.0% solution, soak time is 30-40 minute, and coating layer thickness is the 0.01-0.5 millimeter.
2, a kind of preparation method of absorbable periodontal regenerative sheet is characterized in that comprising the steps:
A, the ratio that takes by weighing in Acetic acid, hydroxy-, bimol. cyclic ester-lactide are the absorbed polymeric polyglycolide-polylactide of 80:20 copolymerization, be placed in the baking oven following dry 24 hours then in 100 ℃, under temperature program(me) control, in screw extruder, make temperature and be 225 ℃ melt, spray by spinning head through dosing pump, solidify in cabinet, the medium in the cabinet is an air, and temperature is a room temperature;
B, the as-spun fibre that makes is wound on the bobbin, winding speed is 250 meters/minute, as-spun fibre on the bobbin is carried out secondary drawing, first order draft temperature is 75 ℃, second level draft temperature is 85 ℃, and total stretching ratio is 6.0 times, thermal finalization in baking oven subsequently, temperature is 100 ℃, and the time is 4 minutes;
C, adopt knitting weft-knitted technology to be woven into knitted fabric on the PGLA yarn, wherein, raw material specification is 5-10tex, loop length is 0.2~0.35 centimetre, the underfill coefficient is 20-40, the vertical 60-90 coil of Density/5 centimetres, the horizontal 40-70 coil of Density/5 centimetres;
D, the knitting skeleton fabric compact structure that will be woven into are finalized the design, and setting temperature is 50 ℃, and shaping time is 15 minutes, carries out coating at last, and coating agent is the chitin serosity, and concentration is 3.0% solution, and soak time is 35 minutes, and coating layer thickness is 0.35 millimeter.
3, according to the preparation method of claims 1 or 2 described absorbable periodontal regenerative sheets, the internal layer that it is characterized in that periodontal regenerative sheet is knitting skeleton fabric, has the required pore structure of periodontal regenerative sheet.
CNB2005101256887A 2005-12-05 2005-12-05 Absorbable periodontal regenerative sheet and its preparing method Expired - Fee Related CN100462108C (en)

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* Cited by examiner, † Cited by third party
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GB0715376D0 (en) * 2007-08-07 2007-09-19 Smith & Nephew Coating

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US6420027B2 (en) * 1999-03-15 2002-07-16 Takasago International Corporation Biodegradable complex fiber and method for producing the same
CN1398643A (en) * 2002-08-12 2003-02-26 天津大学 Prepn process of multi-component hybridized 3D woven myotendinous rack material

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