CN104711702A - Collagen aggregate compound medical fiber with antibacterial/bacteriostatic function - Google Patents
Collagen aggregate compound medical fiber with antibacterial/bacteriostatic function Download PDFInfo
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Abstract
The invention discloses a collagen aggregate compound medical fiber with an antibacterial/bacteriostatic function. The collagen aggregate compound medical fiber is characterized in that collagen aggregate is taken as a raw material, supercritical CO2 is taken as a medium, and epoxy sodium propyl sulfonate or anhydride is taken as a modifying agent, so that acid-soluble collagen aggregate can be obtained; carboxymethyl cellulose is taken as a raw material, and sodium periodate is taken as an oxidizing agent, so that dialdehyde carboxymethyl cellulose can be obtained; the acid-soluble collagen aggregate, the dialdehyde carboxymethyl cellulose and chitin are organically mixed, and the collagen aggregate compound medical fiber can be finally prepared by the technological processes of stirring, standing and defoaming, spinning and the like. The fiber material has good biological performance, biodegradability and biodegradability of the collagen aggregate as well as excellent antibacterial/bacteriostatic activity and anti-inflammation/wound healing promotion function of the chitin; all the performances of the collagen aggregate compound medical fiber are obviously superior to those of the collagen matrix composite fiber material prepared by taking common collagen as a raw material; the collagen aggregate compound medical fiber can be taken as a biological dressing, a hemostatic material, an absorbable suture, a medical face-lifting material, and the like.
Description
Technical field
The present invention relates to a kind of collagen aggregate composite type medical fiber with antibacterial/bacteria resistance function, belong to biomedical materials field.
Background technology
Collagen has been proved to be the splendid bio-medical material of combination property, by collagen group composite material prepared by itself and other natural/synthesis high-molecular biologic medical material organic composite, the focus widely explored of collagen research field and difficult point always, collagen and composite thereof have been made into the different dosage forms such as gel, solution, sponge, granule, fiber and biomembrane, are widely used in the biomedical sectors such as tissue engineering bracket, biological dressing, hemostatic material, suture.Particularly collagen or its composite are become medical function fiber by wet spinning preparation, be subject to researchers especially to pay close attention to widely, also more existing medical fibre launch, the Surgical Absorbable Suture of the commodity of first medical high-tech protein line Co., Ltd as right in Hunan exploitation " good repair pure natural sub-thread collagen sutures " by name, is prepared from by wet spinning animal tendon collagen exactly.In recent years, more there is the report of a large amount of Patents about collagen-based composite medical fiber, but Wei Hua etc. with collagen and shitosan for raw material, organic blended, the collagen-chitin composite medical fiber having been prepared superior performance by wet spinning (but defends China, Zhou Wenchang, Zeng Rui etc. Chinese invention patent. ZL 200410022640.9); Chen Wu bravely waits and has also prepared collagen-polyvinyl composite fibre, and use metal ion and acetal to composite fibre carried out modification (Chen Wuyong, Lin Yunzhou, Ye Guangdou, etc. Chinese invention patent. ZL200510020902.2).But large quantity research shows, also there is following defect in the preparation process of collagen-based composite fibre and properties of product:
1. the spinnability of collagen own is poor, not easily spinning;
2. collagen-based composite fibre mechanical strength is generally poor, and biodegradability is too fast can not meet organism metabolism demand, and its structural stability is also poor simultaneously, is subject to the impact of external environment.
In order to make up above-mentioned defect, the composite fibre that wet spinning is obtained is generally immersed in modification in acetalation bath (main component mostly is formaldehyde, glutaraldehyde) by researcher, cause the biocompatibility of material significantly to decline, and there is potential toxicity, directly affect the application of material.
As everyone knows, in organizer, the existing way of collagen is the aggregation of the higher level structure having collagen, collagen aggregate directly obtains from collagen tissue body, for the mixture of collagenous fibres and fibre bundle, be collagen by laterally to assemble and side direction assembles the supermolecule three-dimensional net structure body of automatic self assembly.Visible, collagen aggregate is more close to the form of collagen in organizer, therefore many performances such as spinnability, mechanics mechanical performance, biologically active, biodegradability, structural stability of collagen aggregate are better than common collagen all significantly, and thus it be more suitable for the raw material as wet spinning.But the collagen Conventional solvents such as collagen aggregate is water insoluble, diluted acid, therefore the present invention is by epoxy propanesulfonate or acid anhydrides to its modification, increases the hydrophilic radical of collagen aggregate, makes it become acid-soluble, be more convenient for the subsequent applications of material.Carboxymethyl cellulose is the cellulose kind that in the world today, the scope of application is the widest, consumption is maximum, food, pharmaceuticals industry are widely used in, by the dialdehyde carboxymethyl cellulose that oxidation reaction makes its strand exposure aldehyde radical be prepared into, it fully remains the good performance of carboxymethyl cellulose itself, equally there is hypotoxicity, and can with the amino generation schiff base reaction of tropocollagen molecule and produce effectively crosslinked effect, can be used as the bion crosslinking agent of collagen, the acetalation bath that current collagen-based composite fibre uses can be substituted completely.Chitin antibacterial/bacteriostatic activity is stronger, itself and collagen aggregate, dialdehyde carboxymethyl cellulose is blended, give full play to the synergy of storeroom, can obtain by wet spinning the collagen aggregate composite type medical fiber that combination property is superior, have antibacterial/bacteria resistance function.
Summary of the invention
A kind of collagen aggregate composite type medical fiber with antibacterial/bacteriostasis efficacy provided for the deficiencies in the prior art is provided.This fibrous material should be a kind ofly both had the premium properties such as good physical and mechanical properties, suitable biodegradability, biologically active and biocompatibility, can effectively stop blooding fast again, the bio-medical material of antibacterial/antibacterial, wound healing and reparation.
For achieving the above object, the present invention adopts following technical scheme:
(1) preparation of acid-soluble collagen aggregate: the collagen aggregate getting 1 ~ 2 weight portion, grinder is ground, be ground into floccule, then the pH being impregnated in 1 ~ 20 parts by volume is in the cushioning liquid of 9.0 ~ 11.5, be stir 5 ~ 10h under the condition of 4 ~ 10 DEG C in temperature, above-mentioned collagen aggregate is taken out from solution, drain, then again by the epoxy propanesulfonate of above-mentioned collagen aggregate and 0.05 ~ 0.2 weight portion or acid anhydrides impouring simultaneously supercritical carbon dioxide reactor, it is 30 DEG C ~ 45 DEG C in temperature, pressure is react 2 ~ 48 h under the condition of 8 ~ 15Mpa, the collagen aggregate after being cross-linked is taken out after terminating, it is successively immersed in PBS buffer solution and deionized water and repeatedly cleans 5 ~ 10h, acid-soluble collagen aggregate is made in final freeze drying,
(2) preparation of dialdehyde carboxymethyl cellulose sodium: be in the Acetic acid-sodium acetate buffer solution impouring simultaneously reactor of 3.0 ~ 5.0 by the pH of the sodium carboxymethylcellulose of 1 ~ 2 weight portion and 20 ~ 50 parts by volume, stirred at ambient temperature is to clarification, then the sodium metaperiodate of 0.5 ~ 2 weight portion is dissolved in the above-mentioned buffer solution of 1 ~ 4 parts by volume, and in slow impouring reactor, be stirring reaction 48 ~ 72h under the condition of 25 DEG C ~ 35 DEG C in temperature, reaction terminating agent polyethylene glycol 0.1 ~ 1 parts by volume is added after question response terminates, after slow stirring 0.5 ~ 1h, then the sodium chloride of 2 ~ 5 weight portions and the acetone of 30 ~ 100 parts by volume is added to reactor, leave standstill and make Precipitation, removing supernatant, final through centrifugal, washing, dialysis, freeze drying prepares dialdehyde carboxymethyl cellulose sodium,
(3) preparation of the compound spinning mother liquor of collagen aggregate: by the acid-soluble collagen aggregate stirring and dissolving of 1 ~ 2 weight portion in the acetum of 0.1 ~ 0.5mol/L of 100 ~ 200 parts by volume, the dialdehyde carboxymethyl cellulose sodium of 0.1 ~ 0.5 weight portion is added in above-mentioned solution, stir 10 ~ 24h at 4 ~ 10 DEG C, obtain composite spinning mother liquor A; Again by the acetum of same for the chitin of 1 ~ 2 weight portion stirring and dissolving at 0.1 ~ 0.5mol/L of 100 ~ 200 parts by volume, obtain composite spinning mother liquor B; Be finally that 4 ~ 6:6 ~ 4 are blended by above-mentioned composite spinning mother liquor A and composite spinning mother liquor B according to volume ratio, be stir 5 ~ 12h under the condition of 4 ~ 10 DEG C in temperature, standing and defoaming, obtains wet spinning mother liquor;
(4) preparation of collagen aggregate composite type medical fiber: adopt wet-spinning frame, be that the saturated mixed solution of the sodium sulphate of 5 ~ 9:1 ~ 5 and sodium chloride is for solidification liquid with mass ratio, silk is sprayed under 35 ~ 55 DEG C of setting temperatures and 0.05 ~ 0.3Mpa nitrogen pressure condition, under suitable tractive force effect, coagulation forming obtains crude fibre, then is 6 ~ 30KGy/h through the desalination of graded ethanol substep, washing repeatedly, 100 ~ 150 DEG C of hot-stretchs sizing (hot-stretch rate is 90% ~ 150%), dosage
60gamma-rays sterilization, formed package that Co produces, obtain collagen aggregate composite type medical fiber.
In above-mentioned preparation method, the source animal skin of the collagen aggregate in step (1) or tendon are ecology, can trace to the source; In step (2), sodium carboxymethylcellulose, epoxy propanesulfonate, acid anhydrides are commercially available, and wherein the carboxymethyl content of sodium carboxymethylcellulose is 65% ~ 85%; The diameter of the collagen aggregate composite type medical fiber in step (4) can adjust according to the conversion of technological parameter; The present invention's wet-spinning frame used is that Shanxi Inst. of Coal Chemistry, Chinese Academy of Sciences produces.
The key performance with the collagen aggregate composite type medical fiber of antibacterial/bacteria resistance function should meet following requirement:
Outward appearance: white or micro-yellow fibrous thing;
Content of beary metal :≤10 μ g/g (m/m);
Line density: 1 ~ 20 dtex;
Fracture strength: 1 ~ 8 cN/dtex;
Elongation at break: 15% ~ 50%;
Cytotoxicity: cell-cytotoxic reaction is not more than 1 grade;
Sterility test: aseptic;
Sensitization test (STT): without delayed type hypersensitivity, DTH;
Intradermal reaction is tested: primary SI PII<0.4.
Compared with prior art, tool has the following advantages this technology:
(1) different from the collagen-based composite fibre had been reported, the present invention with collagen aggregate for raw material, by epoxy propanesulfonate or the more hydrophilic radicals of anhydride modified introducing, prepare acid-soluble collagen aggregate, using acid-soluble collagen aggregate as the base material of wet spinning, compared with common collagen, there is structural form more close to collagen in organizer in its structure, therefore its spinnability, mechanics mechanical performance, biodegradability, biologically active etc. are more excellent;
(2) the present invention's homemade dialdehyde carboxymethyl cellulose sodium has very high chemical reactivity, can occur effectively crosslinked with collagen aggregate, the properties of collagen aggregate is improved further, himself biocompatibility, anthemorrhagic performances etc. are also comparatively superior, can not have an impact to the biologically active of collagen aggregates, there is not potential toxicity, (main component mostly is formaldehyde can to substitute the acetalation bath that current collagen-based composite fibre uses completely, glutaraldehyde, the biocompatibility of material can be caused significantly to decline, and there is potential toxicity, the direct application affecting material), and dialdehyde carboxymethyl cellulose sodium production cost is low, be convenient to large-scale promotion use, it is a kind of excellent Biological cross-linker of collagen,
(3) at supercritical CO
2in fluid condition, chemical crosslinking is carried out to collagen aggregate, early stage can be used as chemical reaction medium, later stage can be used as again the solvent of residual, unreacted epoxy propanesulfonate or acid anhydrides extraction, and the method efficient stable, environmental protection, be conducive to ensureing the biocompatibility of material.
Detailed description of the invention
Below by enforcement, the present invention is specifically described; what be necessary to herein means out is that the present embodiment is only used to further illustrate the present invention; and limiting the scope of the invention can not be interpreted as, the person skilled in the art in this field can make nonessential improvement and adjustment according to the content of foregoing invention.
Embodiment 1
(1) preparation of acid-soluble collagen aggregate: the collagen aggregate getting 1 weight portion, grinder is ground, be ground into floccule, then the pH being impregnated in 1 parts by volume is in the cushioning liquid of 9.0, be stir 5h under the condition of 4 DEG C in temperature, above-mentioned collagen aggregate is taken out from solution, drain, then again by the epoxy propanesulfonate of above-mentioned collagen aggregate and 0.05 weight portion impouring simultaneously supercritical carbon dioxide reactor, it is 30 DEG C in temperature, pressure is react 2h under the condition of 8Mpa, the collagen aggregate after being cross-linked is taken out after terminating, it is successively immersed in PBS buffer solution and deionized water and repeatedly cleans 5h, acid-soluble collagen aggregate is made in final freeze drying,
(2) preparation of dialdehyde carboxymethyl cellulose sodium: be in the Acetic acid-sodium acetate buffer solution impouring simultaneously reactor of 3.0 by the pH of the sodium carboxymethylcellulose of 1 weight portion and 20 parts by volume, stirred at ambient temperature is to clarification, then the sodium metaperiodate of 0.5 weight portion is dissolved in the above-mentioned buffer solution of 1 parts by volume, and in slow impouring reactor, be stirring reaction 48h under the condition of 25 DEG C in temperature, reaction terminating agent polyethylene glycol 0.1 parts by volume is added after question response terminates, after slow stirring 0.5h, then the sodium chloride of 2 weight portions and the acetone of 30 parts by volume is added to reactor, leave standstill and make Precipitation, removing supernatant, final through centrifugal, washing, dialysis, freeze drying prepares dialdehyde carboxymethyl cellulose sodium,
(3) preparation of the compound spinning mother liquor of collagen aggregate: by the acid-soluble collagen aggregate stirring and dissolving of 1 weight portion in the acetum of the 0.5mol/L of 100 parts by volume, the dialdehyde carboxymethyl cellulose sodium of 0.1 weight portion is added in above-mentioned solution, stir 10h at 4 DEG C, obtain composite spinning mother liquor A; Again by the acetum of same for the chitin of 1 weight portion stirring and dissolving at the 0.5mol/L of 100 parts by volume, obtain composite spinning mother liquor B; Be finally that 4:6 is blended by above-mentioned composite spinning mother liquor A and composite spinning mother liquor B according to volume ratio, be stir 5h, standing and defoaming under the condition of 4 DEG C in temperature, obtain wet spinning mother liquor;
(4) preparation of collagen aggregate composite type medical fiber: employing wet-spinning frame, take mass ratio as the sodium sulphate of 5:5 and the saturated mixed solution of sodium chloride be solidification liquid, silk is sprayed under 35 DEG C of setting temperatures and 0.05Mpa nitrogen pressure condition, under suitable tractive force effect, coagulation forming obtains crude fibre, then is 6KGy/h through the desalination of graded ethanol substep, washing repeatedly, 100 DEG C of hot-stretchs sizing (hot-stretch rate is 90%), dosage
60gamma-rays sterilization, formed package that Co produces, obtain collagen aggregate composite type medical fiber.
Embodiment 2
(1) preparation of acid-soluble collagen aggregate: the collagen aggregate getting 1.5 weight portions, grinder is ground, be ground into floccule, then the pH being impregnated in 15 parts by volume is in the cushioning liquid of 10.5, be stir 8h under the condition of 5 DEG C in temperature, in toilet, above-mentioned collagen aggregate is taken out from solution, drain, then again by the succinyl oxide of above-mentioned collagen aggregate and 0.1 weight portion impouring simultaneously supercritical carbon dioxide reactor, it is 35 DEG C in temperature, pressure is react 12 h under the condition of 10Mpa, the collagen aggregate after being cross-linked is taken out after terminating, it is successively immersed in PBS buffer solution and deionized water and repeatedly cleans 8h, acid-soluble collagen aggregate is made in final freeze drying,
(2) preparation of dialdehyde carboxymethyl cellulose sodium: be in the Acetic acid-sodium acetate buffer solution impouring simultaneously reactor of 4.0 by the pH of the sodium carboxymethylcellulose of 1.5 weight portions and 30 parts by volume, stirred at ambient temperature is to clarification, then the sodium metaperiodate of 1 weight portion is dissolved in the above-mentioned buffer solution of 2 parts by volume, and in slow impouring reactor, be stirring reaction 60h under the condition of 30 DEG C in temperature, reaction terminating agent polyethylene glycol 0.5 parts by volume is added after question response terminates, after slow stirring 40min, then the sodium chloride of 3 weight portions and the acetone of 50 parts by volume is added to reactor, leave standstill and make Precipitation, removing supernatant, final through centrifugal, washing, dialysis, freeze drying prepares dialdehyde carboxymethyl cellulose sodium,
(3) preparation of the compound spinning mother liquor of collagen aggregate: by the acid-soluble collagen aggregate stirring and dissolving of 1.5 weight portions in the acetum of the 0.2mol/L of 150 parts by volume, the dialdehyde carboxymethyl cellulose sodium of 0.2 weight portion is added in above-mentioned solution, be stir 15h under the condition of 6 DEG C in temperature, obtain composite spinning mother liquor A; Again by the acetum of same for the chitin of 1.5 weight portions stirring and dissolving at the 0.2mol/L of 150 parts by volume, obtain composite spinning mother liquor B; Be finally that 5:5 is blended by above-mentioned composite spinning mother liquor A and composite spinning mother liquor B according to volume ratio, be stir 8h, standing and defoaming under the condition of 6 DEG C in temperature, obtain wet spinning mother liquor;
(4) preparation of collagen aggregate composite type medical fiber: adopt wet-spinning frame, take mass ratio as the sodium sulphate of 6:4 and the saturated mixed solution of sodium chloride be solidification liquid, silk is sprayed under 45 DEG C of setting temperatures and 0.2Mpa nitrogen pressure condition, under suitable tractive force effect, coagulation forming obtains crude fibre, then is 15KGy/h through the desalination of graded ethanol substep, washing repeatedly, 120 DEG C of hot-stretchs sizing (hot-stretch rate is 120%), dosage
60gamma-rays sterilization, formed package that Co produces, obtain collagen aggregate composite type medical fiber.
Embodiment 3
(1) preparation of acid-soluble collagen aggregate: the collagen aggregate getting 2 weight portions, grinder is ground, be ground into floccule, then the pH being impregnated in 20 parts by volume is in the cushioning liquid of 11.5, be stir 10h under the condition of 10 DEG C in temperature, above-mentioned collagen aggregate is taken out from solution, drain, then again by the epoxy propanesulfonate of above-mentioned collagen aggregate and 0.2 weight portion impouring simultaneously supercritical carbon dioxide reactor, it is 45 DEG C in temperature, pressure is react 48 h under the condition of 15Mpa, the collagen aggregate after being cross-linked is taken out after terminating, it is successively immersed in PBS buffer solution and deionized water and repeatedly cleans 10h, acid-soluble collagen aggregate is made in final freeze drying,
(2) preparation of dialdehyde carboxymethyl cellulose sodium: be in the Acetic acid-sodium acetate buffer solution impouring simultaneously reactor of 5.0 by the pH of the sodium carboxymethylcellulose of 2 weight portions and 50 parts by volume, stirred at ambient temperature is to clarification, then the sodium metaperiodate of 2 weight portions is dissolved in the above-mentioned buffer solution of 4 parts by volume, and, in slow impouring reactor, be stirring reaction 72h under the condition of 35 DEG C in temperature, reaction terminating agent polyethylene glycol 1 parts by volume is added after question response terminates, after slow stirring 1h, then the sodium chloride of 5 weight portions and the acetone of 100 parts by volume is added to reactor, leave standstill and make Precipitation, removing supernatant, final through centrifugal, washing, dialysis, freeze drying prepares dialdehyde carboxymethyl cellulose sodium,
(3) preparation of the compound spinning mother liquor of collagen aggregate: by the acid-soluble collagen aggregate stirring and dissolving of 2 weight portions in the acetum of the 0.1mol/L of 200 parts by volume, the dialdehyde carboxymethyl cellulose sodium of 0.5 weight portion is added in above-mentioned solution, be stir 24h under the condition of 10 DEG C in temperature, obtain composite spinning mother liquor A; Again by the acetum of same for the chitin of 2 weight portions stirring and dissolving at the 0.1mol/L of 200 parts by volume, obtain composite spinning mother liquor B; Be finally that 6:4 is blended by above-mentioned composite spinning mother liquor A and composite spinning mother liquor B according to volume ratio, be stir 12h, standing and defoaming under the condition of 10 DEG C in temperature, obtain final spinning mother liquor;
(4) preparation of collagen aggregate composite type medical fiber: adopt wet-spinning frame, take mass ratio as the sodium sulphate of 9:1 and the saturated mixed solution of sodium chloride be solidification liquid, silk is sprayed under 55 DEG C of setting temperatures and 0.3Mpa nitrogen pressure condition, under suitable tractive force effect, coagulation forming obtains crude fibre, then is 30KGy/h through the desalination of graded ethanol substep, washing repeatedly, 150 DEG C of hot-stretchs sizing (hot-stretch rate is 150%), dosage
60gamma-rays sterilization, formed package that Co produces, obtain collagen aggregate composite type medical fiber.
Claims (5)
1. have the collagen aggregate composite type medical fiber of antibacterial/bacteria resistance function, consist predominantly of acid-soluble collagen aggregate, dialdehyde carboxymethyl cellulose sodium and chitin three kinds of bio-medical raw material, its Key Performance Indicator is as follows:
Outward appearance: white or micro-yellow fibrous thing;
Content of beary metal :≤10 μ g/g (m/m);
Line density: 1 ~ 20 dtex;
Fracture strength: 1 ~ 8 cN/dtex;
Elongation at break: 15% ~ 50%;
Cytotoxicity: cell-cytotoxic reaction is not more than 1 grade;
Sterility test: aseptic;
Sensitization test (STT): without delayed type hypersensitivity, DTH;
Intradermal reaction is tested: primary SI PII<0.4.
2. have the collagen aggregate composite type medical fiber of antibacterial/bacteria resistance function described in claim 1, it is characterized in that, preparation method comprises the steps:
(1) preparation of acid-soluble collagen aggregate: the collagen aggregate getting 1 ~ 2 weight portion, grinder is ground, be ground into floccule, then the pH being impregnated in 1 ~ 20 parts by volume is in the cushioning liquid of 9.0 ~ 11.5, be stir 5 ~ 10h under the condition of 4 ~ 10 DEG C in temperature, above-mentioned collagen aggregate is taken out from solution, drain, then again by the epoxy propanesulfonate of above-mentioned collagen aggregate and 0.05 ~ 0.2 weight portion or acid anhydrides impouring simultaneously supercritical carbon dioxide reactor, it is 30 DEG C ~ 45 DEG C in temperature, pressure is react 2 ~ 48 h under the condition of 8 ~ 15Mpa, the collagen aggregate after being cross-linked is taken out after terminating, it is successively immersed in PBS buffer solution and deionized water and repeatedly cleans 5 ~ 10h, acid-soluble collagen aggregate is made in final freeze drying,
(2) preparation of dialdehyde carboxymethyl cellulose sodium: be in the Acetic acid-sodium acetate buffer solution impouring simultaneously reactor of 3.0 ~ 5.0 by the pH of the sodium carboxymethylcellulose of 1 ~ 2 weight portion and 20 ~ 50 parts by volume, stirred at ambient temperature is to clarification, then the sodium metaperiodate of 0.5 ~ 2 weight portion is dissolved in the above-mentioned buffer solution of 1 ~ 4 parts by volume, and in slow impouring reactor, be stirring reaction 48 ~ 72h under the condition of 25 DEG C ~ 35 DEG C in temperature, reaction terminating agent polyethylene glycol 0.1 ~ 1 parts by volume is added after question response terminates, after slow stirring 0.5 ~ 1h, then the sodium chloride of 2 ~ 5 weight portions and the acetone of 30 ~ 100 parts by volume is added to reactor, leave standstill and make Precipitation, removing supernatant, final through centrifugal, washing, dialysis, freeze drying prepares dialdehyde carboxymethyl cellulose sodium,
(3) preparation of the compound spinning mother liquor of collagen aggregate: by the acid-soluble collagen aggregate stirring and dissolving of 1 ~ 2 weight portion in the acetum of 0.1 ~ 0.5mol/L of 100 ~ 200 parts by volume, the dialdehyde carboxymethyl cellulose sodium of 0.1 ~ 0.5 weight portion is added in above-mentioned solution, stir 10 ~ 24h at 4 ~ 10 DEG C, obtain composite spinning mother liquor A; Again by the acetum of same for the chitin of 1 ~ 2 weight portion stirring and dissolving at 0.1 ~ 0.5mol/L of 100 ~ 200 parts by volume, obtain composite spinning mother liquor B; Be finally that 4 ~ 6:6 ~ 4 are blended by above-mentioned composite spinning mother liquor A and composite spinning mother liquor B according to volume ratio, be stir 5 ~ 12h under the condition of 4 ~ 10 DEG C in temperature, standing and defoaming, obtains wet spinning mother liquor;
(4) preparation of collagen aggregate composite type medical fiber: adopt wet-spinning frame, be that the saturated mixed solution of the sodium sulphate of 5 ~ 9:1 ~ 5 and sodium chloride is for solidification liquid with mass ratio, silk is sprayed under 35 ~ 55 DEG C of setting temperatures and 0.05 ~ 0.3Mpa nitrogen pressure condition, under suitable tractive force effect, coagulation forming obtains crude fibre, then is 6 ~ 30KGy/h through the desalination of graded ethanol substep, washing repeatedly, 100 ~ 150 DEG C of hot-stretchs sizing (hot-stretch rate is 90% ~ 150%), dosage
60gamma-rays sterilization, formed package that Co produces, obtain collagen aggregate composite type medical fiber.
3. there is described in claim 2 the collagen aggregate composite type medical fiber of antibacterial/bacteria resistance function, it is characterized in that described acid anhydrides can be any one in acetic anhydride and succinyl oxide.
4. there is described in claim 2 the collagen aggregate composite type medical fiber of antibacterial/bacteria resistance function, it is characterized in that described collagen aggregate is the multi-layer aggregation of common collagen, is extract to obtain from any one pigskin, pig tendon, ox-hide, beef tendon, donkey hide, mouse skin or mouse tail tendon.
5. preparation process according to claim 2 is all complete in clean worker-house, and the cleanliness factor in clean worker-house is respectively ten thousand grades and hundred grades.
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| CN108210985A (en) * | 2018-01-22 | 2018-06-29 | 陕西科技大学 | A kind of high-strength medical hydrogel based on human-like collagen and preparation method thereof |
| CN111501121A (en) * | 2019-01-31 | 2020-08-07 | 华北水利水电大学 | Method for preparing collagen fiber by wet spinning |
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| CN110499541B (en) * | 2019-07-18 | 2021-09-14 | 福建农林大学 | High-strength bionic fiber based on collagen liquid crystal in-situ self-assembly and preparation method thereof |
| CN112624631A (en) * | 2020-12-17 | 2021-04-09 | 四川轻化工大学 | Inducing method of glass fiber polypropylene interface transverse crystal structure |
| CN115068667A (en) * | 2022-07-20 | 2022-09-20 | 青岛大学 | Bioactive nano hemostatic sponge and preparation method and application thereof |
| CN115094629A (en) * | 2022-08-26 | 2022-09-23 | 江苏亨瑞生物医药科技有限公司 | Recombinant collagen modified cellulose fiber and preparation method thereof |
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