CN106947126A - A kind of high intensity bio-compatible chitin nano fiber/Heveatex composite membrane - Google Patents
A kind of high intensity bio-compatible chitin nano fiber/Heveatex composite membrane Download PDFInfo
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- CN106947126A CN106947126A CN201710191084.5A CN201710191084A CN106947126A CN 106947126 A CN106947126 A CN 106947126A CN 201710191084 A CN201710191084 A CN 201710191084A CN 106947126 A CN106947126 A CN 106947126A
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- nano fiber
- chitin
- chitin nano
- heveatex
- composite membrane
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- 229920002101 Chitin Polymers 0.000 title claims abstract description 193
- 239000002121 nanofiber Substances 0.000 title claims abstract description 144
- 239000002131 composite material Substances 0.000 title claims abstract description 86
- 239000012528 membrane Substances 0.000 title claims abstract description 74
- 238000000034 method Methods 0.000 claims abstract description 55
- 239000000463 material Substances 0.000 claims abstract description 49
- 230000001590 oxidative effect Effects 0.000 claims abstract description 13
- 238000001338 self-assembly Methods 0.000 claims abstract description 11
- 238000002360 preparation method Methods 0.000 claims abstract description 10
- 239000000243 solution Substances 0.000 claims description 23
- 239000006185 dispersion Substances 0.000 claims description 21
- 239000003814 drug Substances 0.000 claims description 18
- 230000001172 regenerating effect Effects 0.000 claims description 18
- 239000003513 alkali Substances 0.000 claims description 17
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 15
- XSQUKJJJFZCRTK-UHFFFAOYSA-N Urea Chemical compound NC(N)=O XSQUKJJJFZCRTK-UHFFFAOYSA-N 0.000 claims description 15
- 239000007864 aqueous solution Substances 0.000 claims description 15
- 239000004202 carbamide Substances 0.000 claims description 15
- RRHGJUQNOFWUDK-UHFFFAOYSA-N Isoprene Chemical group CC(=C)C=C RRHGJUQNOFWUDK-UHFFFAOYSA-N 0.000 claims description 12
- KWYUFKZDYYNOTN-UHFFFAOYSA-M Potassium hydroxide Chemical compound [OH-].[K+] KWYUFKZDYYNOTN-UHFFFAOYSA-M 0.000 claims description 12
- 238000010438 heat treatment Methods 0.000 claims description 9
- 239000007788 liquid Substances 0.000 claims description 9
- WMFOQBRAJBCJND-UHFFFAOYSA-M Lithium hydroxide Chemical compound [Li+].[OH-] WMFOQBRAJBCJND-UHFFFAOYSA-M 0.000 claims description 8
- 125000003178 carboxy group Chemical group [H]OC(*)=O 0.000 claims description 8
- 239000007800 oxidant agent Substances 0.000 claims description 8
- 238000000967 suction filtration Methods 0.000 claims description 8
- 239000000835 fiber Substances 0.000 claims description 7
- GDOPTJXRTPNYNR-UHFFFAOYSA-N methyl-cyclopentane Natural products CC1CCCC1 GDOPTJXRTPNYNR-UHFFFAOYSA-N 0.000 claims description 7
- 150000001875 compounds Chemical class 0.000 claims description 6
- 238000004073 vulcanization Methods 0.000 claims description 6
- 239000003153 chemical reaction reagent Substances 0.000 claims description 5
- 240000007594 Oryza sativa Species 0.000 claims description 4
- 235000007164 Oryza sativa Nutrition 0.000 claims description 4
- 239000000203 mixture Substances 0.000 claims description 4
- 238000007254 oxidation reaction Methods 0.000 claims description 4
- 235000009566 rice Nutrition 0.000 claims description 4
- 238000007598 dipping method Methods 0.000 claims description 3
- 238000013007 heat curing Methods 0.000 claims description 3
- 150000002978 peroxides Chemical class 0.000 claims description 3
- 238000004519 manufacturing process Methods 0.000 abstract description 2
- 241000894007 species Species 0.000 description 16
- 239000000843 powder Substances 0.000 description 15
- 239000007787 solid Substances 0.000 description 10
- 238000002156 mixing Methods 0.000 description 6
- 238000003756 stirring Methods 0.000 description 6
- 229920000126 latex Polymers 0.000 description 5
- 239000004816 latex Substances 0.000 description 5
- 230000002787 reinforcement Effects 0.000 description 5
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 5
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 4
- 238000013019 agitation Methods 0.000 description 4
- 238000000502 dialysis Methods 0.000 description 4
- 238000005516 engineering process Methods 0.000 description 4
- 239000002070 nanowire Substances 0.000 description 4
- 230000000052 comparative effect Effects 0.000 description 3
- SUKJFIGYRHOWBL-UHFFFAOYSA-N sodium hypochlorite Chemical compound [Na+].Cl[O-] SUKJFIGYRHOWBL-UHFFFAOYSA-N 0.000 description 3
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 description 2
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical class OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 description 2
- 208000037656 Respiratory Sounds Diseases 0.000 description 2
- XLOMVQKBTHCTTD-UHFFFAOYSA-N Zinc monoxide Chemical compound [Zn]=O XLOMVQKBTHCTTD-UHFFFAOYSA-N 0.000 description 2
- 230000002378 acidificating effect Effects 0.000 description 2
- ROOXNKNUYICQNP-UHFFFAOYSA-N ammonium peroxydisulfate Substances [NH4+].[NH4+].[O-]S(=O)(=O)OOS([O-])(=O)=O ROOXNKNUYICQNP-UHFFFAOYSA-N 0.000 description 2
- VAZSKTXWXKYQJF-UHFFFAOYSA-N ammonium persulfate Chemical compound [NH4+].[NH4+].[O-]S(=O)OOS([O-])=O VAZSKTXWXKYQJF-UHFFFAOYSA-N 0.000 description 2
- 229910001870 ammonium persulfate Inorganic materials 0.000 description 2
- 239000003519 biomedical and dental material Substances 0.000 description 2
- 230000001276 controlling effect Effects 0.000 description 2
- 239000002086 nanomaterial Substances 0.000 description 2
- JHJLBTNAGRQEKS-UHFFFAOYSA-M sodium bromide Chemical compound [Na+].[Br-] JHJLBTNAGRQEKS-UHFFFAOYSA-M 0.000 description 2
- 239000000725 suspension Substances 0.000 description 2
- 238000005406 washing Methods 0.000 description 2
- 241000238421 Arthropoda Species 0.000 description 1
- 241000195493 Cryptophyta Species 0.000 description 1
- 241000196324 Embryophyta Species 0.000 description 1
- 241000233866 Fungi Species 0.000 description 1
- 240000002853 Nelumbo nucifera Species 0.000 description 1
- 235000006508 Nelumbo nucifera Nutrition 0.000 description 1
- 235000006510 Nelumbo pentapetala Nutrition 0.000 description 1
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 description 1
- 239000005864 Sulphur Substances 0.000 description 1
- 238000009825 accumulation Methods 0.000 description 1
- 125000000218 acetic acid group Chemical group C(C)(=O)* 0.000 description 1
- 238000005903 acid hydrolysis reaction Methods 0.000 description 1
- 238000010306 acid treatment Methods 0.000 description 1
- 125000003277 amino group Chemical group 0.000 description 1
- 229910021529 ammonia Inorganic materials 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000006065 biodegradation reaction Methods 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 238000004061 bleaching Methods 0.000 description 1
- 210000000988 bone and bone Anatomy 0.000 description 1
- 159000000007 calcium salts Chemical class 0.000 description 1
- 238000006555 catalytic reaction Methods 0.000 description 1
- 210000000170 cell membrane Anatomy 0.000 description 1
- 229920002678 cellulose Polymers 0.000 description 1
- 239000001913 cellulose Substances 0.000 description 1
- 238000005119 centrifugation Methods 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 231100000135 cytotoxicity Toxicity 0.000 description 1
- 230000003013 cytotoxicity Effects 0.000 description 1
- 231100000263 cytotoxicity test Toxicity 0.000 description 1
- 230000006196 deacetylation Effects 0.000 description 1
- 238000003381 deacetylation reaction Methods 0.000 description 1
- 230000003247 decreasing effect Effects 0.000 description 1
- 230000035614 depigmentation Effects 0.000 description 1
- 238000004090 dissolution Methods 0.000 description 1
- 238000001035 drying Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 238000005189 flocculation Methods 0.000 description 1
- 230000016615 flocculation Effects 0.000 description 1
- 239000003292 glue Substances 0.000 description 1
- 238000005470 impregnation Methods 0.000 description 1
- 229920002521 macromolecule Polymers 0.000 description 1
- 229920001206 natural gum Polymers 0.000 description 1
- 229920005615 natural polymer Polymers 0.000 description 1
- 229920006173 natural rubber latex Polymers 0.000 description 1
- 230000007935 neutral effect Effects 0.000 description 1
- 231100001083 no cytotoxicity Toxicity 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- JRKICGRDRMAZLK-UHFFFAOYSA-L peroxydisulfate Chemical compound [O-]S(=O)(=O)OOS([O-])(=O)=O JRKICGRDRMAZLK-UHFFFAOYSA-L 0.000 description 1
- 239000003208 petroleum Substances 0.000 description 1
- UMPKMCDVBZFQOK-UHFFFAOYSA-N potassium;iron(3+);oxygen(2-) Chemical compound [O-2].[O-2].[K+].[Fe+3] UMPKMCDVBZFQOK-UHFFFAOYSA-N 0.000 description 1
- 239000000047 product Substances 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 230000001105 regulatory effect Effects 0.000 description 1
- 230000003014 reinforcing effect Effects 0.000 description 1
- 238000002791 soaking Methods 0.000 description 1
- JBJWASZNUJCEKT-UHFFFAOYSA-M sodium;hydroxide;hydrate Chemical compound O.[OH-].[Na+] JBJWASZNUJCEKT-UHFFFAOYSA-M 0.000 description 1
- 239000006228 supernatant Substances 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
- 238000002604 ultrasonography Methods 0.000 description 1
- 239000011787 zinc oxide Substances 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L7/00—Compositions of natural rubber
- C08L7/02—Latex
-
- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61F—FILTERS IMPLANTABLE INTO BLOOD VESSELS; PROSTHESES; DEVICES PROVIDING PATENCY TO, OR PREVENTING COLLAPSING OF, TUBULAR STRUCTURES OF THE BODY, e.g. STENTS; ORTHOPAEDIC, NURSING OR CONTRACEPTIVE DEVICES; FOMENTATION; TREATMENT OR PROTECTION OF EYES OR EARS; BANDAGES, DRESSINGS OR ABSORBENT PADS; FIRST-AID KITS
- A61F6/00—Contraceptive devices; Pessaries; Applicators therefor
-
- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61L—METHODS OR APPARATUS FOR STERILISING MATERIALS OR OBJECTS IN GENERAL; DISINFECTION, STERILISATION OR DEODORISATION OF AIR; CHEMICAL ASPECTS OF BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES; MATERIALS FOR BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES
- A61L31/00—Materials for other surgical articles, e.g. stents, stent-grafts, shunts, surgical drapes, guide wires, materials for adhesion prevention, occluding devices, surgical gloves, tissue fixation devices
- A61L31/12—Composite materials, i.e. containing one material dispersed in a matrix of the same or different material
- A61L31/125—Composite materials, i.e. containing one material dispersed in a matrix of the same or different material having a macromolecular matrix
- A61L31/129—Composite materials, i.e. containing one material dispersed in a matrix of the same or different material having a macromolecular matrix containing macromolecular fillers
-
- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61L—METHODS OR APPARATUS FOR STERILISING MATERIALS OR OBJECTS IN GENERAL; DISINFECTION, STERILISATION OR DEODORISATION OF AIR; CHEMICAL ASPECTS OF BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES; MATERIALS FOR BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES
- A61L31/00—Materials for other surgical articles, e.g. stents, stent-grafts, shunts, surgical drapes, guide wires, materials for adhesion prevention, occluding devices, surgical gloves, tissue fixation devices
- A61L31/14—Materials characterised by their function or physical properties, e.g. injectable or lubricating compositions, shape-memory materials, surface modified materials
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08B—POLYSACCHARIDES; DERIVATIVES THEREOF
- C08B37/00—Preparation of polysaccharides not provided for in groups C08B1/00 - C08B35/00; Derivatives thereof
- C08B37/0006—Homoglycans, i.e. polysaccharides having a main chain consisting of one single sugar, e.g. colominic acid
- C08B37/0024—Homoglycans, i.e. polysaccharides having a main chain consisting of one single sugar, e.g. colominic acid beta-D-Glucans; (beta-1,3)-D-Glucans, e.g. paramylon, coriolan, sclerotan, pachyman, callose, scleroglucan, schizophyllan, laminaran, lentinan or curdlan; (beta-1,6)-D-Glucans, e.g. pustulan; (beta-1,4)-D-Glucans; (beta-1,3)(beta-1,4)-D-Glucans, e.g. lichenan; Derivatives thereof
- C08B37/0027—2-Acetamido-2-deoxy-beta-glucans; Derivatives thereof
- C08B37/003—Chitin, i.e. 2-acetamido-2-deoxy-(beta-1,4)-D-glucan or N-acetyl-beta-1,4-D-glucosamine; Chitosan, i.e. deacetylated product of chitin or (beta-1,4)-D-glucosamine; Derivatives 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
- C08J5/00—Manufacture of articles or shaped materials containing macromolecular substances
- C08J5/18—Manufacture of films or sheets
-
- 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
- C08J2307/00—Characterised by the use of natural rubber
- C08J2307/02—Latex
-
- 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
- C08J2405/00—Characterised by the use of polysaccharides or of their derivatives not provided for in groups C08J2401/00 or C08J2403/00
- C08J2405/08—Chitin; Chondroitin sulfate; Hyaluronic acid; Derivatives thereof
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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
- C08L2203/00—Applications
- C08L2203/16—Applications used for films
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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
- C08L2205/00—Polymer mixtures characterised by other features
- C08L2205/14—Polymer mixtures characterised by other features containing polymeric additives characterised by shape
- C08L2205/16—Fibres; Fibrils
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- Chemical Kinetics & Catalysis (AREA)
- Vascular Medicine (AREA)
- Polymers & Plastics (AREA)
- Heart & Thoracic Surgery (AREA)
- Animal Behavior & Ethology (AREA)
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- Veterinary Medicine (AREA)
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- Manufacturing & Machinery (AREA)
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- Composite Materials (AREA)
- Molecular Biology (AREA)
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- Materials For Medical Uses (AREA)
- Manufacture Of Macromolecular Shaped Articles (AREA)
Abstract
The invention discloses a kind of high intensity bio-compatible chitin nano fiber/Heveatex composite membrane and preparation method thereof.Negatively charged and weakly alkaline chitin nano fiber is prepared respectively using oxidizing process and self-assembly method, and chitin nano fiber and Heveatex composite membrane-forming are obtained into chitin nano fiber/Heveatex composite membrane.Chitin nano fiber prepared by the present invention/Heveatex composite membrane can significantly improve the mechanical property of Heveatex, and with good biocompatibility, it is easy to mass production, expand application of the Heveatex in biomedical materials field.
Description
【Technical field】
The present invention relates to a kind of high intensity bio-compatible chitin nano fiber/Heveatex composite membrane, belong to natural height
Molecule, biomedical materials field.
【Background technology】
Heveatex has high resiliency, good film forming, and glued membrane is imbued with pliability, is widely used in the day of people
Often in life.However, the modulus of Heveatex glued membrane is smaller and biocompatibility is poor, in the application of biomedical materials field
It is very restricted.Therefore, the reinforcement of Heveatex and Study on biocompatibility for expand its application have it is important
Meaning.Inorganic nano material reinforcement Heveatex has difficult scattered, technological process complexity and can not changed to a certain extent
The shortcoming (CN105694130A, CN101307193A and CN101381483A) of kind Heveatex biocompatibility.Synthesize high score
Sub- modified natural rubber latex is then easily caused latex system viscosity and drastically raised, and destroys the stability of latex, and reinforcing effect is poor, and
And synthesis macromolecule is difficult to biodegradation, mainly using non-renewable petroleum resources as raw material, is unfavorable for environmentally friendly material
Development (J Appl.Polym.Sci.2005,98,1125-1134).
Chitin is the natural polymer that accumulation is only second to cellulose in nature, with good biocompatibility,
Biodegradability and unique micro-nano structure (Nature, 2015,524,7564:155-157).Chitin nano fiber be by
Monodimension nanometer material prepared by chitin, has chitin excellent properties and high-specific surface area, high-crystallinity and high-modulus concurrently, is increasing
By force, catalysis and biomedical materials field have wide practical use (Nanoscale, 2014,6,9477-9493).Therefore, it is sharp
It is expected to improve the biocompatibility of latex material while with chitin nano fiber reinforcement Heveatex.Dufresne etc. is attempted
The nanocrystalline reinforcement Heveatex of chitin obtained using Hydrochloric Acid Hydrolysis Method, because chitin is nanocrystalline between Heveatex
Compatibility is poor, and major diameter is smaller, and made compound film-strength is increased while elastic be remarkably decreased
(Biomacromolecules 2003,4,657-665；Biomacromolecules 2003,4,666-674).So far,
Not yet there is the technology using negatively charged or weakly alkaline chitin nano fiber reinforcement Heveatex.
【The content of the invention】
[technical problem to be solved]
Another object of the present invention is to provide a kind of high intensity bio-compatible chitin nano fiber/Heveatex to be combined
Film and preparation method thereof.
Another object of the present invention is to provide compatibility between a kind of raising chitin nano fiber and Heveatex
Method.
[technical scheme]
The invention provides a kind of high intensity bio-compatible chitin nano fiber/Heveatex composite membrane and its preparation side
Method, this method is combined using negatively charged or weakly alkaline chitin nano fiber and Heveatex, by impregnating or taking out
Film forming is filtered, then high intensity bio-compatible chitin nano fiber/Heveatex composite membrane is obtained through further heating vulcanization.
The present invention is achieved by the following technical solutions：
The preparation method of a kind of chitin nano fiber/Heveatex composite membrane, it is characterised in that this method includes as follows
Step：Be combined using negatively charged or weakly alkaline chitin nano fiber and Heveatex, then by the composite into
Film, vulcanization obtain chitin nano fiber/Heveatex composite membrane；The tensile strength of made composite membrane be 10.0~
Chitin nano fiber content is 0.1~10wt% in 20.0MPa, composite membrane.
According to another preferred embodiment of the application, it is characterised in that：Chitin Nanowire used in this method
Dimension is negatively charged or in alkalescent, wherein, negatively charged chitin nano fiber is made by oxidizing process；Weakly alkaline first
Shell element nanofiber is made using alkali and/or aqueous solution of urea dissolving chitin by self-assembly method.
According to another preferred embodiment of the application, it is characterised in that：Point of negatively charged chitin nano fiber
Band carboxyl in subchain, the Zeta potential of chitin nano fiber aqueous dispersions is -50~-30, and carboxyl institute is introduced using oxidizing process
Oxidising agent is any one in peroxide, persulfide, oxometallate or TEMPO reagents, oxidising agent
Concentration is 0.1~10mol/L, and oxidizing temperature is 30~100 DEG C, and oxidization time is 2~30h, gained chitin nano fiber
Draw ratio is more than 20.
According to another preferred embodiment of the application, it is characterised in that：Dissipated in alkalescent chitin nano fiber moisture
The pH value range of liquid is 7~11, one or more compositions of the alkali used by dissolving chitin in KOH, NaOH and LiOH,
The concentration of alkali is 1.5~3mol/L, and the concentration of the urea used by dissolving chitin is 0.5~1mol/L, utilizes alkali and/or urea
Aqueous dissolution chitin obtains the weak solution that concentration is 0.1~2wt%, then obtains weakly alkaline first by self assembly of dialysing
Shell element nanofiber, the draw ratio of gained chitin nano fiber is more than 20.
According to another preferred embodiment of the application, it is characterised in that：By negatively charged described in claim 2 or
Chitin nano fiber/Heveatex composite solution is obtained in weakly alkaline chitin nano fiber and Heveatex are compound, so
Afterwards by the method film forming of dipping or suction filtration, and bio-compatible chitin nano fiber/natural gum is obtained by heating vulcanization
Newborn composite membrane, the temperature of heat cure is 60~100 DEG C, and the time is 0.5~2h.
The chitin nano fiber prepared according to described method/Heveatex composite membrane, it is characterised in that this is answered
The tensile strength for closing film is 10.0~20.0MPa, and Young's modulus is 5.0~70.0MPa, and elongation rate of tensile failure is 660~900%,
Chitin nano fiber content is 0.1~10wt% in composite membrane.
Chitin nano fiber/application of the Heveatex composite membrane in condom material field.
Chitin nano fiber/Heveatex composite membrane is in organizational project, regenerative medicine, and Medical rack Material Field
In application.
A kind of method for improving compatibility between chitin nano fiber and Heveatex, it is characterised in that utilize oxidizing process
By band carboxyl on the strand of chitin nano fiber, so as to obtain negatively charged chitin nano fiber, and by itself and day
Right latex carries out compound so as to improve compatibility therebetween；
Or using alkali and/or aqueous solution of urea dissolving chitin, weakly alkaline chitin is made by self-assembly method and received
Rice fiber, and itself and Heveatex are carried out compound so as to improve compatibility therebetween.
Chitin nano fiber content is 0.1~10wt%, tool in foregoing chitin nano fiber/Heveatex composite membrane
There are excellent mechanical property and good biocompatibility, its tensile strength is 10.0~20.0MPa, and elongation at break is 660
~900%, Young's modulus is 5.0~70.0MPa, and without cytotoxicity, can significantly improve the biofacies of Heveatex
Capacitive.
Described chitin source is the bone of arthropod, shell, the cell membrane of fungi, algae and some rudimentary plants
Deng using the method purifying of preceding process known technology without special limitation.Such as acid treatment removing calcium salt, alkali process takes off egg
In vain, oxidation bleaching depigmentation and alkali process are partially deacetylated etc..
Described Heveatex is pre-vulcanized natural latex, its fresh Heveatex for including coming from para ruber or
The Heveatex of concentration, and using the vulcanizing system of sulphur, accelerator ZDC and zinc oxide composition.It is preferred that dry glue solid content is
45%th, ammonia content is 0.7% presulfurization concentrated natural latex.
Described chitin nano fiber/Heveatex composite membrane, it is characterised in that the chitin nanometer in the composite membrane
Fiber is obtained using oxidizing process or using self-assembly method.Negatively charged chitin is made using oxidizing process introducing carboxyl to receive
Rice fiber；Chitin is dissolved using alkali/aqueous solution of urea, and weakly alkaline chitin nano fiber is made by self-assembly method.
Described negatively charged chitin nano fiber is that chitin powder is dispersed in oxidising agent after reaction to pass through
Centrifugation or dialysis regulation pH are obtained in the processing of neutral and assisting ultrasonic.Chitin powder is dispersed in the quality point in oxidising agent
Number is 0.1~2wt%, and gained nanofiber is negatively charged, and its draw ratio is more than 20.By changing oxidizing temperature or time
Carboxyl-content on regulation and control chitin molecule chain can realize nanofiber stable dispersion in aqueous, and Zeta potential is -50
~-30mV.During the oxidising agent can be peroxide, persulfide, oxometallate ammonium persulfate or TEMPO reagents
Any one, the concentration of oxidising agent is 0.5~2mol/L, and oxidizing temperature is 40~80 DEG C, and the heat time is 2~30h.
Described alkalescent chitin nano fiber be using chitin weak solution dialysed in water self assembly be made, use
The dissolving of chitin is realized with patent CN103059319A identical methods.Chitin powder is dissolved in alkali/aqueous solution of urea
Mass fraction be 0.1~2wt%, gained nanofiber be in alkalescent, and its draw ratio be more than 20.By controlling during dialysis
Between can adjust chitin nano fiber aqueous dispersions pH scopes be 7~11.In the alkali/aqueous solution of urea, alkali is selected from
One or more compositions in KOH, NaOH and LiOH, the concentration of alkali is 1.5~3mol/L, the concentration of urea for 0.5~
1mol/L。
The preparation method of described chitin nano fiber/Heveatex composite membrane, it is characterised in that by negatively charged or
The weakly alkaline chitin nano fiber aqueous dispersions of person and Heveatex are in proportion after mixing and stirring, by impregnating or taking out
Filter method film forming, then obtains high-performance bio-compatible chitin nano fiber/Heveatex composite membrane by further heating.Plus
The temperature of heat cure is 60~100 DEG C, and the time is 0.5~2h.
Mixing and stirring refers to that chitin is received to described chitin nano fiber aqueous dispersions in proportion with Heveatex
The mixing of rice fiber aqueous dispersions and Heveatex is carried out under conditions of continuously stirring, and stir speed (S.S.) is 200~2000r/
Min, mixing time is 5~30min, and temperature is 10~40 DEG C, and it is 0.1 to control chitin nano fiber content in composite membrane
~10wt%.
Described dipping film forming refers to using different impregnation molds in chitin nano fiber/Heveatex mixed liquor
At the uniform velocity pulling growth film forming, pull rate is 2~10mm/min.
Described suction filtration film forming, which refers to chitin nano fiber/Heveatex mixed liquor being placed under the conditions of field of flow, to depressurize
Suction filtration film forming.
[beneficial effect]
The present invention uses above-mentioned technical proposal, has the following advantages that：
1st, the chitin nano fiber in the present invention is negatively charged or in alkalescent, and draw ratio is higher, the present invention
In chitin nano fiber and Heveatex there is excellent compatibility.
2nd, chitin nano fiber/Heveatex composite membrane of the invention has an excellent mechanical property, tensile stress compared with
Pure glued membrane can improve 3 times, and Young's modulus can improve 35 times, and elongation strain is all more than 660%；Chitin nano fiber is mended
The elasticity of latex material can be kept well while strong Heveatex.
3rd, chitin nano fiber/Heveatex composite membrane no cytotoxicity of the invention, with excellent bio-compatible
Property, have wide practical use (Fig. 4) in condom material, organizational project and Medical rack Material Field.
4th, the production technology environmental protection of chitin nano fiber/Heveatex composite membrane, low, the products obtained therefrom performance of power consumption
It is excellent, it is the important breakthrough to prior art, with boundless actual application prospect.
【Brief description of the drawings】
Fig. 1 is that chitin nano fiber, Heveatex and chitin nano fiber/Heveatex composite solution place 1
Photo in kind after month.
Fig. 2 is the photo in kind of pure natural glued membrane and chitin nano fiber/Heveatex composite membrane.
Fig. 3 is the mechanical curves of pure natural glued membrane and chitin nano fiber/Heveatex composite membrane.
Fig. 4 is the cytotoxicity test result of pure natural glued membrane and chitin nano fiber/Heveatex composite membrane.
【Embodiment】
Technical scheme is described further below in conjunction with specific embodiment, but the protection model of the present invention
Enclose and be not limited only to this.
Embodiment 1
By the commercially available chitin dilute HCl soaking at room temperature 12h of 0.1mol/L, distill and 0.1mol/L NaOH water is used after water washing
Solution soaks 12h, then with 0.3wt%NaClO after distilling water washing2Depigmentation, drying obtains the crust that acetyl degree is 95%
Plain powder.0.5g chitin powder is dispersed in 99.5g 1mol/L ammonium persulfate aqueous solution, in magnetic agitation at 60 DEG C
20h makes the methylol on chitin molecule chain be oxidized to carboxyl, is then made negatively charged by the assisting ultrasonic that centrifuges or dialyse
The chitin nano fiber of lotus, the Zeta potential of chitin nano fiber aqueous dispersions is -30.Chitin nano fiber moisture dissipates
Liquid and pre-vulcanized natural latex that solid content is 45% are the corresponding ratios of 0.5wt% by chitin nano fiber content in composite membrane
Example is well mixed to obtain chitin nano fiber/Heveatex composite solution, and the composite solution is highly stable, places 1 month nothing
Significant change (Fig. 1).Chitin nano fiber/Heveatex composite solution is vulcanized by suction filtration film forming through 90 DEG C of heating 1h
To high-performance chitin nano fiber/Heveatex composite membrane.Made chitin nano fiber/Heveatex composite membrane has excellent
Different mechanical property, its tensile strength is 14.0MPa, and Young's modulus is 28MPa, and elongation at break is 745%, and with good
Good biocompatibility, it is adaptable to sheath, regenerative medicine, and Medical rack material.
Embodiment 2
Material therefor species, consumption and technological process be the same as Example 1, the difference is that 0.5g chitin powder is dispersed in
In 99.5g 1mol/L persulfate aqueous solution, negatively charged chitin Nanowire is prepared in magnetic agitation 48h at 60 DEG C
Dimension, the Zeta potential of chitin nano fiber aqueous dispersions is -50.Made chitin nano fiber/Heveatex composite membrane tool
There is good mechanical property, its tensile strength is 12.8MPa, and Young's modulus is 26MPa, and elongation at break is 720%, and is had
There is good biocompatibility, it is adaptable to sheath, regenerative medicine, and Medical rack material.
Embodiment 3
Material therefor species, consumption and technological process be the same as Example 1, the difference is that 0.5g chitin powder is dispersed in
In the 99.5g 1mol/L Na2Fe04 aqueous solution, negatively charged chitin Nanowire is prepared in magnetic agitation 5h at 80 DEG C
Dimension, the Zeta potential of chitin nano fiber aqueous dispersions is -30.Made chitin nano fiber/Heveatex composite membrane tool
There is good mechanical property, its tensile strength is 13.5MPa, and Young's modulus is 32MPa, and elongation at break is 690%, and is had
There is good biocompatibility, it is adaptable to sheath, regenerative medicine, and Medical rack material.
Embodiment 4
Material therefor species, consumption and technological process be the same as Example 3, the difference is that 0.5g chitin powder is dispersed in
Negatively charged chitin nano fiber is prepared in the 99.5g 1mol/L potassium ferrate aqueous solution.Made chitin Nanowire
Dimension/Heveatex composite membrane has good mechanical property, and its tensile strength is 13.0MPa, and Young's modulus is 33MPa, fracture
Elongation is 700%, and with good biocompatibility, it is adaptable to sheath, regenerative medicine, and Medical rack material
Material.
Embodiment 5
Material therefor species, consumption and technological process be the same as Example 1, the difference is that 1.0g chitin powder is dispersed in
99.0g 1mol/L TEMPO reagents (TEMPO:NaClO:NaClO2Mol ratio is 1:10:100) in, stirred in magnetic force at 80 DEG C
Mix 2h and prepare negatively charged chitin nano fiber, the Zeta potential of the aqueous dispersions of chitin nano fiber is -30.Crust
Plain nanofiber aqueous dispersions press chitin nano fiber content in composite membrane with solid content for 45% pre-vulcanized natural latex
Chitin nano fiber/Heveatex composite solution is obtained for the corresponding ratios of 0.5wt% are well mixed, the composite solution is very
It is stable, 1 month is placed without significant change.Made chitin nano fiber/Heveatex composite membrane has excellent mechanical property,
Its tensile strength is 14.0MPa, and Young's modulus is 30MPa, and elongation at break is 740%, and with good bio-compatible
Property, it is adaptable to sheath, regenerative medicine, and Medical rack material.
Embodiment 6
Material therefor species, consumption and technological process be the same as Example 5, the difference is that the oxidation reaction process magnetic agitation time
For 5h, the Zeta potential of the aqueous dispersions of chitin nano fiber is -50.Made chitin nano fiber/Heveatex is combined
Film has excellent mechanical property, and its tensile strength is 12.5MPa, and Young's modulus is 28MPa, and elongation at break is 680%, and
And with good biocompatibility, it is adaptable to sheath, regenerative medicine, and Medical rack material.
Embodiment 7
Material therefor species, consumption and technological process be the same as Example 5, the difference is that 1.0g chitin powder is dispersed in
99.0g 1mol/L TEMPO reagents (TEMPO:NaBr:NaClO mol ratios are 1:10:50) negatively charged crust is prepared in
Plain nanofiber.Made chitin nano fiber/Heveatex composite membrane has excellent mechanical property, and its tensile strength is
13.5MPa, Young's modulus is 31MPa, and elongation at break is 750%, and with good biocompatibility, it is adaptable to practise contraception
Set, regenerative medicine, and Medical rack material.
Embodiment 8
Material therefor species, consumption and technological process be the same as Example 1, the difference is that chitin powder is dispersed in into 3mol/L
KOH and 0.5mol/L aqueous solution of urea in obtain mass fraction be 0.5wt% chitin solution.Chitin solution passes through
The method self assembly of dialysis prepares weakly alkaline chitin nano fiber, and the pH for controlling chitin nano fiber aqueous dispersions is
10, the pre-vulcanized natural latex for being then 45% with solid content is 0.3wt% pairs by chitin nano fiber content in composite membrane
The ratio answered is well mixed and obtains chitin nano fiber/Heveatex composite solution, and the composite solution is highly stable, places 1
Individual month without significant change.Made chitin nano fiber/Heveatex composite membrane (Fig. 2) has excellent mechanical property and good
Biocompatibility, the load-deformation curve under its stretch mode is shown in Figure 3, it is adaptable to sheath, regenerative medicine, and
Medical rack material.
Embodiment 9
Material therefor species, consumption and technological process be the same as Example 8, unlike by chitin nano fiber aqueous dispersions
In chitin nano fiber content in composite membrane it is the corresponding ratios of 0.5wt% with pre-vulcanized natural latex that solid content is 45%
Well mixed to obtain chitin nano fiber/Heveatex composite solution, the composite solution is highly stable, places 1 month without bright
Aobvious change.Made chitin nano fiber/Heveatex composite membrane (Fig. 2) has excellent mechanical property and good biofacies
Load-deformation curve under capacitive, its stretch mode is shown in Figure 3, it is adaptable to sheath, regenerative medicine, and Medical rack
Material.
Embodiment 10
Material therefor species, consumption and technological process be the same as Example 8, unlike by chitin nano fiber aqueous dispersions
In chitin nano fiber content in composite membrane it is the corresponding ratios of 1.0wt% with pre-vulcanized natural latex that solid content is 45%
Well mixed to obtain chitin nano fiber/Heveatex composite solution, the composite solution is highly stable, places 1 month without bright
Aobvious change.Made chitin nano fiber/Heveatex composite membrane (Fig. 2) has excellent mechanical property and good biofacies
Load-deformation curve under capacitive, its stretch mode is shown in Figure 3, it is adaptable to sheath, regenerative medicine, and Medical rack
Material.
Embodiment 11
Material therefor species, consumption and technological process be the same as Example 8, unlike by chitin nano fiber aqueous dispersions
In chitin nano fiber content in composite membrane it is the corresponding ratios of 2.0wt% with pre-vulcanized natural latex that solid content is 45%
Well mixed to obtain chitin nano fiber/Heveatex composite solution, the composite solution is highly stable, places 1 month without bright
Aobvious change.Made chitin nano fiber/Heveatex composite membrane (Fig. 2) has excellent mechanical property and good biofacies
Load-deformation curve under capacitive, its stretch mode is shown in Figure 3, it is adaptable to sheath, regenerative medicine, and Medical rack
Material.
Embodiment 12
Material therefor species, consumption and technological process be the same as Example 10, the difference is that chitin powder is dispersed in
Weakly alkaline chitin nano fiber is prepared in 2.5mol/L NaOH and 0.67mol/L aqueous solution of urea, it is 7 to control pH.
Chitin nano fiber/Heveatex composite membrane vulcanizes 30min through 100 DEG C of heating.Made chitin nano fiber/Heveatex
Composite membrane has excellent mechanical property, and its tensile strength is 14.0MPa, and Young's modulus is 50MPa, and elongation at break is
780%, and with good biocompatibility, it is adaptable to sheath, regenerative medicine, and Medical rack material.
Embodiment 13
Material therefor species, consumption and technological process be the same as Example 12, the difference is that chitin nano fiber moisture is dissipated
The pH controls of liquid are 9.Made chitin nano fiber/Heveatex composite membrane has excellent mechanical property, its tensile strength
For 15.5MPa, Young's modulus is 51MPa, and elongation at break is 800%, and with good biocompatibility, it is adaptable to keep away
Pregnant set, regenerative medicine, and Medical rack material.
Embodiment 14
Material therefor species, consumption and technological process be the same as Example 12, the difference is that chitin nano fiber moisture is dissipated
The pH controls of liquid are 11.Made chitin nano fiber/Heveatex composite membrane has excellent mechanical property, its tensile strength
For 15MPa, Young's modulus is 51MPa, and elongation at break is 790%, and with good biocompatibility, it is adaptable to practise contraception
Set, regenerative medicine, and Medical rack material.
Embodiment 15
Material therefor species, consumption and technological process be the same as Example 10, the difference is that chitin powder is dispersed in into 2mol/
Weakly alkaline chitin nano fiber is prepared in L LiOH and 1mol/L aqueous solution of urea, chitin nano fiber water is controlled
The pH of dispersion liquid is 10.Made chitin nano fiber/Heveatex composite membrane has excellent mechanical property, its tensile strength
For 14.5MPa, Young's modulus is 45MPa, and elongation at break is 750%, and with good biocompatibility, it is adaptable to keep away
Pregnant set, regenerative medicine, and Medical rack material.Comparative example 1
Material therefor species, consumption and technological process be the same as Example 1, the difference is that chitin powder is dispersed in into 33wt%
It is 25~30% to control the deacetylation of chitin in 90 DEG C of heating response 2h in the NaOH aqueous solution.Then by the crust of pretreatment
Element is dispersed in water the chitin dispersion liquid for obtaining that mass fraction is 0.5wt%, and regulation pH is 3, and the magnetic force under normal temperature condition
Stirring 48h makes chitin be uniformly dispersed, while realizing that surface amino groups are protonated, then obtains positively charged by ultrasound stripping
Chitin nano fiber.Positively charged chitin suspension and solid content are pressed into composite membrane for 45% pre-vulcanized natural latex
Middle chitin nano fiber content is flocculation after the corresponding ratio mixing of 1.0wt%, and mixed liquor crackle occurs through suction filtration, it is impossible to make
High intensity chitin fiber/Heveatex composite membrane is obtained, the requirement as structural material or bio-medical material can not be met.
Comparative example 2
Material therefor species, consumption and technological process be the same as Example 1, the difference is that chitin powder is dispersed in into 3mol/L
HCl in obtain the chitin suspension that mass fraction is 0.5wt%, it is nanocrystalline that 90 DEG C of heating stirring 5h are made chitin, leads to
Cross dialysis or centrifugally regulated pH obtains weakly acidic chitin nano fiber dispersion liquid for 3~6, weakly acidic chitin is hanged
Supernatant liquid is 1.0wt% corresponding by chitin nano fiber content in composite membrane with pre-vulcanized natural latex that solid content is 45%
Flocculated after ratio mixing, mixed liquor crackle occurs through suction filtration, it is impossible to high intensity chitin fiber/Heveatex composite membrane is made,
The requirement as structural material or bio-medical material can not be met.
Comparative example 3
By solid content for 45% pre-vulcanized natural latex by suction filtration film forming, then obtain day through 90 DEG C of heating 1h vulcanizations
Right glued membrane.The elongation strain of Heveatex composite membrane is larger, but tensile strength and modulus are smaller (Fig. 3), and bio-compatible
Property is poor, is restricted in the application of sheath, regenerative medicine, and Medical rack Material Field.
Claims (9)
1. the preparation method of a kind of chitin nano fiber/Heveatex composite membrane, it is characterised in that this method includes following step
Suddenly：Be combined using negatively charged or weakly alkaline chitin nano fiber and Heveatex, then by the composite film forming,
Vulcanization obtains chitin nano fiber/Heveatex composite membrane；The tensile strength of made composite membrane is 10.0~20.0MPa,
Chitin nano fiber content is 0.1~10wt% in composite membrane.
2. preparation method according to claim 1, it is characterised in that：Chitin nano fiber band used in this method
Negative electrical charge or in alkalescent, wherein, negatively charged chitin nano fiber is made by oxidizing process；Weakly alkaline chitin
Nanofiber is made using alkali and/or aqueous solution of urea dissolving chitin by self-assembly method.
3. preparation method according to claim 2, it is characterised in that：The strand of negatively charged chitin nano fiber
Upper band carboxyl, the Zeta potential of chitin nano fiber aqueous dispersions is -50~-30, is introduced using oxidizing process used by carboxyl
Oxidising agent is any one in peroxide, persulfide, oxometallate or TEMPO reagents, the concentration of oxidising agent
For 0.1~10mol/L, oxidizing temperature is 30~100 DEG C, and oxidization time is 2~30h, the major diameter of gained chitin nano fiber
Than more than 20.
4. preparation method according to claim 2, it is characterised in that：In alkalescent chitin nano fiber aqueous dispersions
PH value range is 7~11, one or more compositions of the alkali used by dissolving chitin in KOH, NaOH and LiOH, alkali
Concentration is 1.5~3mol/L, and the concentration of the urea used by dissolving chitin is 0.5~1mol/L, water-soluble using alkali and/or urea
Liquid dissolving chitin obtains the weak solution that concentration is 0.1~2wt%, then obtains weakly alkaline chitin by self assembly of dialysing
Nanofiber, the draw ratio of gained chitin nano fiber is more than 20.
5. the preparation method of chitin nano fiber/Heveatex composite membrane according to claim 1, it is characterised in that：Will
Negatively charged described in claim 2 obtains chitin and received in weakly alkaline chitin nano fiber and Heveatex are compound
Rice fiber/Heveatex composite solution, then by the method film forming of dipping or suction filtration, and obtains the life by heating vulcanization
The compatible chitin nano fiber of thing/Heveatex composite membrane, the temperature of heat cure is 60~100 DEG C, and the time is 0.5~2h.
6. the chitin nano fiber prepared according to the method described in claim 1/Heveatex composite membrane, its feature exists
In the composite membrane tensile strength be 10.0~20.0MPa, Young's modulus be 5.0~70.0MPa, elongation rate of tensile failure be 660~
900%, chitin nano fiber content is 0.1~10wt% in composite membrane.
7. chitin nano fiber/application of the Heveatex composite membrane in condom material field described in claim 6.
8. chitin nano fiber/Heveatex composite membrane described in claim 6 is in organizational project, regenerative medicine, and doctor
With the application in timbering material field.
9. a kind of method for improving compatibility between chitin nano fiber and Heveatex, it is characterised in that will using oxidizing process
Band carboxyl on the strand of chitin nano fiber, so as to obtain negatively charged chitin nano fiber, and by its with it is natural
Latex carries out compound so as to improve compatibility therebetween；Or using alkali and/or aqueous solution of urea dissolving chitin, pass through
Weakly alkaline chitin nano fiber is made in self-assembly method, and itself and Heveatex be combined improving therebetween
Compatibility.
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