CN115260411A - Medical composite material and preparation method thereof - Google Patents
Medical composite material and preparation method thereof Download PDFInfo
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- CN115260411A CN115260411A CN202211144151.5A CN202211144151A CN115260411A CN 115260411 A CN115260411 A CN 115260411A CN 202211144151 A CN202211144151 A CN 202211144151A CN 115260411 A CN115260411 A CN 115260411A
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- silicon rubber
- deionized water
- composite material
- stirring
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- 239000002131 composite material Substances 0.000 title claims abstract description 22
- 238000002360 preparation method Methods 0.000 title claims abstract description 14
- 229920002379 silicone rubber Polymers 0.000 claims abstract description 81
- 230000000844 anti-bacterial effect Effects 0.000 claims abstract description 41
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 38
- 239000008367 deionised water Substances 0.000 claims abstract description 37
- 229910021641 deionized water Inorganic materials 0.000 claims abstract description 37
- 238000006243 chemical reaction Methods 0.000 claims abstract description 31
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 26
- 239000003999 initiator Substances 0.000 claims abstract description 22
- 239000011259 mixed solution Substances 0.000 claims abstract description 20
- 238000001035 drying Methods 0.000 claims abstract description 17
- 238000010438 heat treatment Methods 0.000 claims abstract description 16
- 239000007864 aqueous solution Substances 0.000 claims abstract description 12
- 238000004140 cleaning Methods 0.000 claims abstract description 11
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims abstract description 8
- 239000001301 oxygen Substances 0.000 claims abstract description 8
- 229910052760 oxygen Inorganic materials 0.000 claims abstract description 8
- FBBDOOHMGLLEGJ-UHFFFAOYSA-N methane;hydrochloride Chemical compound C.Cl FBBDOOHMGLLEGJ-UHFFFAOYSA-N 0.000 claims abstract description 7
- 238000005406 washing Methods 0.000 claims abstract description 7
- 238000007789 sealing Methods 0.000 claims abstract description 6
- 238000003756 stirring Methods 0.000 claims description 50
- LCGLNKUTAGEVQW-UHFFFAOYSA-N Dimethyl ether Chemical compound COC LCGLNKUTAGEVQW-UHFFFAOYSA-N 0.000 claims description 26
- ISAOCJYIOMOJEB-UHFFFAOYSA-N benzoin Chemical compound C=1C=CC=CC=1C(O)C(=O)C1=CC=CC=C1 ISAOCJYIOMOJEB-UHFFFAOYSA-N 0.000 claims description 26
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 23
- 239000006229 carbon black Substances 0.000 claims description 23
- UIIMBOGNXHQVGW-UHFFFAOYSA-M Sodium bicarbonate Chemical compound [Na+].OC([O-])=O UIIMBOGNXHQVGW-UHFFFAOYSA-M 0.000 claims description 22
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims description 20
- RTZKZFJDLAIYFH-UHFFFAOYSA-N Diethyl ether Chemical compound CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 claims description 20
- VVQNEPGJFQJSBK-UHFFFAOYSA-N Methyl methacrylate Chemical compound COC(=O)C(C)=C VVQNEPGJFQJSBK-UHFFFAOYSA-N 0.000 claims description 20
- UEEJHVSXFDXPFK-UHFFFAOYSA-N N-dimethylaminoethanol Chemical compound CN(C)CCO UEEJHVSXFDXPFK-UHFFFAOYSA-N 0.000 claims description 20
- 229960002887 deanol Drugs 0.000 claims description 20
- 239000004945 silicone rubber Substances 0.000 claims description 20
- SQGYOTSLMSWVJD-UHFFFAOYSA-N silver(1+) nitrate Chemical compound [Ag+].[O-]N(=O)=O SQGYOTSLMSWVJD-UHFFFAOYSA-N 0.000 claims description 18
- 239000004115 Sodium Silicate Substances 0.000 claims description 16
- NTHWMYGWWRZVTN-UHFFFAOYSA-N sodium silicate Chemical compound [Na+].[Na+].[O-][Si]([O-])=O NTHWMYGWWRZVTN-UHFFFAOYSA-N 0.000 claims description 16
- 229910052911 sodium silicate Inorganic materials 0.000 claims description 16
- 244000028419 Styrax benzoin Species 0.000 claims description 13
- 235000000126 Styrax benzoin Nutrition 0.000 claims description 13
- 235000008411 Sumatra benzointree Nutrition 0.000 claims description 13
- 229960002130 benzoin Drugs 0.000 claims description 13
- RWCCWEUUXYIKHB-UHFFFAOYSA-N benzophenone Chemical compound C=1C=CC=CC=1C(=O)C1=CC=CC=C1 RWCCWEUUXYIKHB-UHFFFAOYSA-N 0.000 claims description 13
- 239000012965 benzophenone Substances 0.000 claims description 13
- 235000019382 gum benzoic Nutrition 0.000 claims description 13
- 229920000126 latex Polymers 0.000 claims description 11
- 239000004816 latex Substances 0.000 claims description 11
- 229910000030 sodium bicarbonate Inorganic materials 0.000 claims description 11
- 235000017557 sodium bicarbonate Nutrition 0.000 claims description 11
- 239000003054 catalyst Substances 0.000 claims description 10
- 239000003795 chemical substances by application Substances 0.000 claims description 10
- WDVGLADRSBQDDY-UHFFFAOYSA-N holmium(3+);trinitrate Chemical compound [Ho+3].[O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O WDVGLADRSBQDDY-UHFFFAOYSA-N 0.000 claims description 10
- 239000003208 petroleum Substances 0.000 claims description 10
- 229910001961 silver nitrate Inorganic materials 0.000 claims description 9
- 238000000034 method Methods 0.000 claims description 7
- NEHMKBQYUWJMIP-UHFFFAOYSA-N chloromethane Chemical compound ClC NEHMKBQYUWJMIP-UHFFFAOYSA-N 0.000 claims description 6
- UIIMBOGNXHQVGW-DEQYMQKBSA-M Sodium bicarbonate-14C Chemical compound [Na+].O[14C]([O-])=O UIIMBOGNXHQVGW-DEQYMQKBSA-M 0.000 claims description 5
- 239000006227 byproduct Substances 0.000 claims description 5
- 238000001816 cooling Methods 0.000 claims description 5
- 238000001914 filtration Methods 0.000 claims description 5
- 230000001678 irradiating effect Effects 0.000 claims description 5
- 238000006116 polymerization reaction Methods 0.000 claims description 5
- 238000010992 reflux Methods 0.000 claims description 5
- 238000009210 therapy by ultrasound Methods 0.000 claims description 5
- 238000003828 vacuum filtration Methods 0.000 claims description 5
- 238000004821 distillation Methods 0.000 claims description 4
- 239000003112 inhibitor Substances 0.000 claims description 4
- 238000004321 preservation Methods 0.000 claims description 4
- 229940050176 methyl chloride Drugs 0.000 claims description 3
- 238000005286 illumination Methods 0.000 abstract description 2
- QIGBRXMKCJKVMJ-UHFFFAOYSA-N Hydroquinone Chemical compound OC1=CC=C(O)C=C1 QIGBRXMKCJKVMJ-UHFFFAOYSA-N 0.000 description 12
- 230000000052 comparative effect Effects 0.000 description 10
- 241000894006 Bacteria Species 0.000 description 6
- 239000004342 Benzoyl peroxide Substances 0.000 description 6
- OMPJBNCRMGITSC-UHFFFAOYSA-N Benzoylperoxide Chemical compound C=1C=CC=CC=1C(=O)OOC(=O)C1=CC=CC=C1 OMPJBNCRMGITSC-UHFFFAOYSA-N 0.000 description 6
- 235000019400 benzoyl peroxide Nutrition 0.000 description 6
- 239000000523 sample Substances 0.000 description 6
- 239000000463 material Substances 0.000 description 4
- 239000000178 monomer Substances 0.000 description 4
- 241000282414 Homo sapiens Species 0.000 description 3
- 125000000217 alkyl group Chemical group 0.000 description 3
- 239000003242 anti bacterial agent Substances 0.000 description 3
- 239000007788 liquid Substances 0.000 description 3
- 230000004048 modification Effects 0.000 description 3
- 238000012986 modification Methods 0.000 description 3
- 241000588724 Escherichia coli Species 0.000 description 2
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 description 2
- 241000191967 Staphylococcus aureus Species 0.000 description 2
- 238000007792 addition Methods 0.000 description 2
- NEHMKBQYUWJMIP-NJFSPNSNSA-N chloro(114C)methane Chemical compound [14CH3]Cl NEHMKBQYUWJMIP-NJFSPNSNSA-N 0.000 description 2
- 238000001514 detection method Methods 0.000 description 2
- 125000002887 hydroxy group Chemical group [H]O* 0.000 description 2
- 239000011159 matrix material Substances 0.000 description 2
- 229910052761 rare earth metal Inorganic materials 0.000 description 2
- 229910052709 silver Inorganic materials 0.000 description 2
- 239000004332 silver Substances 0.000 description 2
- 239000000243 solution Substances 0.000 description 2
- 230000001954 sterilising effect Effects 0.000 description 2
- 230000002195 synergetic effect Effects 0.000 description 2
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 1
- 241000233866 Fungi Species 0.000 description 1
- 229910052689 Holmium Inorganic materials 0.000 description 1
- 230000001580 bacterial effect Effects 0.000 description 1
- 244000052616 bacterial pathogen Species 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000012496 blank sample Substances 0.000 description 1
- 210000000988 bone and bone Anatomy 0.000 description 1
- 239000011203 carbon fibre reinforced carbon Substances 0.000 description 1
- 238000013329 compounding Methods 0.000 description 1
- 239000013068 control sample Substances 0.000 description 1
- 238000012258 culturing Methods 0.000 description 1
- 201000010099 disease Diseases 0.000 description 1
- 208000037265 diseases, disorders, signs and symptoms Diseases 0.000 description 1
- 210000001198 duodenum Anatomy 0.000 description 1
- 239000000945 filler Substances 0.000 description 1
- 230000004927 fusion Effects 0.000 description 1
- 229920000578 graft copolymer Polymers 0.000 description 1
- 229910021389 graphene Inorganic materials 0.000 description 1
- KJZYNXUDTRRSPN-UHFFFAOYSA-N holmium atom Chemical compound [Ho] KJZYNXUDTRRSPN-UHFFFAOYSA-N 0.000 description 1
- 125000004435 hydrogen atom Chemical group [H]* 0.000 description 1
- 210000004072 lung Anatomy 0.000 description 1
- 244000000010 microbial pathogen Species 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 238000002715 modification method Methods 0.000 description 1
- 210000002445 nipple Anatomy 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 239000000047 product Substances 0.000 description 1
- 230000001902 propagating effect Effects 0.000 description 1
- 150000003242 quaternary ammonium salts Chemical group 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 238000010008 shearing Methods 0.000 description 1
- -1 silver ions Chemical class 0.000 description 1
- 238000002791 soaking Methods 0.000 description 1
- 238000003980 solgel method Methods 0.000 description 1
- 239000008223 sterile water Substances 0.000 description 1
- 238000004659 sterilization and disinfection Methods 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 239000000758 substrate Substances 0.000 description 1
- 210000003437 trachea Anatomy 0.000 description 1
Classifications
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F283/00—Macromolecular compounds obtained by polymerising monomers on to polymers provided for in subclass C08G
- C08F283/12—Macromolecular compounds obtained by polymerising monomers on to polymers provided for in subclass C08G on to polysiloxanes
-
- 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
- A61L29/00—Materials for catheters, medical tubing, cannulae, or endoscopes or for coating catheters
- A61L29/04—Macromolecular materials
- A61L29/041—Macromolecular materials obtained by reactions only involving carbon-to-carbon unsaturated bonds
- A61L29/042—Rubbers
-
- 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
- A61L29/00—Materials for catheters, medical tubing, cannulae, or endoscopes or for coating catheters
- A61L29/08—Materials for coatings
-
- 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
- A61L29/00—Materials for catheters, medical tubing, cannulae, or endoscopes or for coating catheters
- A61L29/08—Materials for coatings
- A61L29/10—Inorganic materials
- A61L29/103—Carbon
-
- 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
- A61L29/00—Materials for catheters, medical tubing, cannulae, or endoscopes or for coating catheters
- A61L29/14—Materials characterised by their function or physical properties, e.g. lubricating compositions
- A61L29/16—Biologically active materials, e.g. therapeutic substances
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F2/00—Processes of polymerisation
- C08F2/44—Polymerisation in the presence of compounding ingredients, e.g. plasticisers, dyestuffs, fillers
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F2/00—Processes of polymerisation
- C08F2/46—Polymerisation initiated by wave energy or particle radiation
- C08F2/48—Polymerisation initiated by wave energy or particle radiation by ultraviolet or visible light
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/28—Nitrogen-containing compounds
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K7/00—Use of ingredients characterised by shape
- C08K7/22—Expanded, porous or hollow particles
- C08K7/24—Expanded, porous or hollow particles inorganic
- C08K7/26—Silicon- containing compounds
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K9/00—Use of pretreated ingredients
- C08K9/12—Adsorbed ingredients, e.g. ingredients on carriers
-
- 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
- A61L2300/00—Biologically active materials used in bandages, wound dressings, absorbent pads or medical devices
- A61L2300/10—Biologically active materials used in bandages, wound dressings, absorbent pads or medical devices containing or releasing inorganic materials
- A61L2300/108—Elemental carbon, e.g. charcoal
-
- 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
- A61L2300/00—Biologically active materials used in bandages, wound dressings, absorbent pads or medical devices
- A61L2300/20—Biologically active materials used in bandages, wound dressings, absorbent pads or medical devices containing or releasing organic materials
- A61L2300/216—Biologically active materials used in bandages, wound dressings, absorbent pads or medical devices containing or releasing organic materials with other specific functional groups, e.g. aldehydes, ketones, phenols, quaternary phosphonium groups
-
- 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
- A61L2300/00—Biologically active materials used in bandages, wound dressings, absorbent pads or medical devices
- A61L2300/40—Biologically active materials used in bandages, wound dressings, absorbent pads or medical devices characterised by a specific therapeutic activity or mode of action
- A61L2300/404—Biocides, antimicrobial agents, antiseptic agents
-
- 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
- A61L2300/00—Biologically active materials used in bandages, wound dressings, absorbent pads or medical devices
- A61L2300/60—Biologically active materials used in bandages, wound dressings, absorbent pads or medical devices characterised by a special physical form
- A61L2300/606—Coatings
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02A—TECHNOLOGIES FOR ADAPTATION TO CLIMATE CHANGE
- Y02A50/00—TECHNOLOGIES FOR ADAPTATION TO CLIMATE CHANGE in human health protection, e.g. against extreme weather
- Y02A50/30—Against vector-borne diseases, e.g. mosquito-borne, fly-borne, tick-borne or waterborne diseases whose impact is exacerbated by climate change
Abstract
The invention discloses a medical composite material and a preparation method thereof, and the preparation method comprises the following steps: preparing an intermediate, adding the intermediate into deionized water, heating to 70 ℃, introducing methane chloride, keeping the temperature for reaction for 5 hours, washing after the reaction is finished, and standing for 30min to obtain a graft; ultrasonically cleaning silicon rubber by using an ethanol aqueous solution with the volume fraction of 50% for 30min, drying, then treating for 5min by using oxygen plasma, placing the silicon rubber in an initiator mixed solution after the treatment is finished, sealing and storing for 2h at 37 ℃, taking out and drying for 2h to prepare the pretreated silicon rubber; the prepared graft is added into deionized water, the pretreated silicon rubber is added, ultraviolet illumination is carried out for 5min, and then the silicon rubber is ultrasonically cleaned for 5min by ethanol aqueous solution with the volume fraction of 50 percent to prepare the medical composite material which can be used for preparing medical instruments such as medical catheters and the like and has excellent antibacterial performance.
Description
Technical Field
The invention relates to the technical field of medical instruments, in particular to a medical composite material and a preparation method thereof.
Background
The silicon rubber product is widely applied to the fields of medical treatment, life, industry and the like. Such as medical catheters, prosthesis, occluders, artificial trachea, artificial lungs, artificial bones, silicone rubber duodenum and the like, and also used for mobile phone shells, nipples for children and the like. But due to its special structure, the surface is easily attached with bacteria and fungi to cause diseases to human beings.
In daily life, a variety of pathogenic microorganisms are widely distributed in nature and pose a threat to human health. Escherichia coli and staphylococcus aureus are the most common pathogenic bacteria, which have long plagued human life, and the antibacterial property detection of the antibacterial material at the present stage is also represented by Escherichia coli and staphylococcus aureus.
In the prior art, when the silicon rubber is subjected to antibacterial modification, modification is usually performed by simple blending of antibacterial agents, such as addition of nano silver particles, but the antibacterial silicon rubber prepared by the modification method has short antibacterial duration, poor fusion with the antibacterial agent and single antibacterial property, so that the antibacterial effect is limited.
Disclosure of Invention
In order to solve the technical problems, the invention provides a medical composite material and a preparation method thereof.
The purpose of the invention can be realized by the following technical scheme:
a preparation method of a medical composite material comprises the following steps:
step S1, adding methyl methacrylate and dimethylaminoethanol into a reaction kettle, stirring at a constant speed, adding a catalyst and a polymerization inhibitor, stirring at a constant speed, heating to 105-125 ℃, refluxing for 4 hours, distilling under reduced pressure after the reaction is finished to remove unreacted methyl methacrylate and dimethylaminoethanol to obtain an intermediate, adding the intermediate into deionized water, heating to 70 ℃, introducing methane chloride, reacting at a constant temperature for 5 hours, washing after the reaction is finished, standing for 30 minutes, removing by-products under reduced pressure to obtain a graft, controlling the molar ratio of methyl methacrylate to dimethylaminoethanol to be 2-2.25: 1, controlling the dosage of the catalyst to be 1-1.5 percent of the sum of the weights of methyl methacrylate and dimethylaminoethanol, controlling the dosage of the polymerization inhibitor to be 0.1-0.3 percent of the weight of the catalyst, and controlling the molar ratio of the intermediate, the methane chloride and the deionized water to be 1: 0.2-0.3;
in the step S1, methyl methacrylate and dimethyl aminoethanol react under the action of a catalyst to generate an intermediate, and then the intermediate reacts with methane chloride to generate a graft, wherein the reaction process is as follows:
in the structure, the synthesized graft has a quaternary ammonium salt structure at one end and can participate in polymerization of carbon-carbon double bonds, and the grafted body can be endowed with excellent antibacterial performance.
S2, adding benzophenone and benzoin dimethyl ether into acetone, stirring at a constant speed for 30min to prepare initiator mixed solution, controlling the dosage ratio of the benzophenone, the benzoin dimethyl ether and the acetone to be 0.705: 0.075: 20mL, ultrasonically cleaning silicon rubber by using ethanol aqueous solution with the volume fraction of 50% for 30min, drying, then treating for 5min by using oxygen plasma, placing the silicon rubber into the initiator mixed solution after the treatment is finished, sealing and storing for 2h at 37 ℃, taking out and naturally drying for 2h to prepare pretreated silicon rubber, and controlling the weight ratio of the initiator mixed solution to the silicon rubber to be 20: 2-2.5;
and S3, adding the graft obtained in the step S1 into deionized water, adding pretreated silicon rubber, irradiating for 5min by ultraviolet light, then ultrasonically cleaning for 5min by using an ethanol aqueous solution with the volume fraction of 50% to remove unreacted monomer and initiator mixed solution, and preparing the medical composite material, wherein the weight ratio of the graft to the deionized water to the pretreated silicon rubber is controlled to be 0.5-0.8: 1: 3-5.
In the step S2, benzophenone and benzoin dimethyl ether are used as photoinitiators at the same time for compounding, oxygen plasma is used for treating the surface of silicon rubber to enable hydrophilic hydroxyl groups to be generated on the surface of the silicon rubber, the silicon rubber is soaked in initiator mixed liquid to facilitate the photoinitiator to be adsorbed on the surface of the silicon rubber to prepare pretreated silicon rubber, then in the step S3, under ultraviolet illumination, the benzophenone in the photoinitiator can capture hydrogen atoms on the surface of the silicon rubber to generate active free radicals, and the benzoin dimethyl ether can be uniformly cracked to enable the surface of the silicon rubber to generate free radicals, so that double bonds of a graft are polymerized and grafted on the silicon rubber, and the silicon rubber is endowed with good antibacterial performance.
Further, the method comprises the following steps: the silicone rubber is prepared by the following steps:
step S11, adding sodium silicate and sodium bicarbonate into deionized water, heating to 90-95 ℃, uniformly stirring and reacting for 20min, adding the sodium silicate again, uniformly stirring for 5min, adding the sodium bicarbonate, uniformly stirring and reacting for 1h, adding holmium nitrate and silver nitrate, uniformly stirring and reacting for 1h, cooling, filtering and drying after the reaction is finished to obtain the antibacterial white carbon black, wherein the dosage ratio of the sodium silicate to the sodium bicarbonate to the deionized water is controlled to be 0.01 mol: 100mL, and the dosage ratio of the holmium nitrate to the deionized water is controlled to be 0.5 mmol: 0.05 mol: 1000mL;
in the step S11, sodium silicate and sodium bicarbonate are used as raw materials, a white carbon black matrix is prepared through a sol-gel method, rare earth elements holmium and silver ions are loaded on the prepared white carbon black matrix to prepare the antibacterial white carbon black, and the antibacterial effect of silver can be improved by introducing the rare earth elements.
And S12, adding the antibacterial white carbon black into petroleum ether, performing ultrasonic treatment, pouring into silicon rubber latex, performing vacuum filtration after uniform stirring, stirring at a constant speed of 200r/min, adding a curing agent, continuously stirring until no bubbles are generated, pouring into a mold, and curing for 10-12 hours to obtain the silicon rubber, wherein the dosage ratio of the antibacterial white carbon black, the petroleum ether, the silicon rubber latex to the curing agent is controlled to be 0.20-0.25 g: 10-15 mL: 50-60 g: 1-2g.
A medical composite material is prepared by the preparation method.
The invention has the beneficial effects that:
the invention relates to a medical composite material, which is an antibacterial silicone rubber material, can be used for preparing medical devices such as medical catheters and the like, and has excellent antibacterial performance, wherein in the preparation process, antibacterial white carbon black is prepared firstly, then the antibacterial white carbon black is used as a filler to be blended with silicone rubber latex, and is solidified to prepare silicone rubber with antibacterial performance, and then benzophenone and benzoin dimethyl ether are used as photoinitiators to be compounded for use, oxygen plasma is used for treating the surface of the silicone rubber, so that hydrophilic hydroxyl groups are generated on the surface of the silicone rubber, the silicone rubber is soaked in initiator mixed liquid, so that the photoinitiators are conveniently adsorbed on the surface of the silicone rubber, and pretreated silicone rubber is prepared;
according to the invention, the blended white carbon black antibacterial agent can release antibacterial factors to realize an antibacterial effect, and the graft is polymerized in a structural network of a substrate to directly play a role in bacteria adhered to the surface, and synergistic antibacterial is carried out through two modes.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
Example 1
The silicone rubber is prepared by the following steps:
step S11, adding sodium silicate and sodium bicarbonate into deionized water, heating to 90 ℃, uniformly stirring and reacting for 20min, adding sodium silicate again, uniformly stirring for 5min, adding sodium bicarbonate, uniformly stirring and reacting for 1h, adding holmium nitrate and silver nitrate, uniformly stirring and reacting for 1h, cooling, suction filtering and drying after the reaction is finished to obtain the antibacterial white carbon black, wherein the dosage ratio of the sodium silicate, the sodium bicarbonate and the deionized water is controlled to be 0.01 mol: 100mL, and the dosage ratio of the holmium nitrate, the silver nitrate and the deionized water is controlled to be 0.5 mmol: 0.05 mol: 1000mL;
and S12, adding the antibacterial white carbon black into petroleum ether, performing ultrasonic treatment, pouring into silicon rubber latex, performing vacuum filtration after uniform stirring, stirring at a constant speed of 200r/min, adding a curing agent, namely alkyl diethanolamide, continuously stirring until no bubbles are generated, pouring into a mold, and curing for 10 hours to obtain the silicon rubber, wherein the dosage ratio of the antibacterial white carbon black, the petroleum ether, the silicon rubber latex to the curing agent is controlled to be 0.20 g: 10 mL: 50 g: 1g.
Example 2
The silicone rubber is prepared by the following steps:
step S11, adding sodium silicate and sodium bicarbonate into deionized water, heating to 92 ℃, stirring at a constant speed and reacting for 20min, adding the sodium silicate again, stirring at a constant speed for 5min, adding the sodium bicarbonate, stirring at a constant speed and reacting for 1h, adding holmium nitrate and silver nitrate, stirring at a constant speed and reacting for 1h, cooling, filtering and drying after the reaction is finished to obtain the antibacterial white carbon black, wherein the dosage ratio of the sodium silicate, the sodium bicarbonate and the deionized water is controlled to be 0.01 mol: 100mL, and the dosage ratio of the holmium nitrate, the silver nitrate and the deionized water is controlled to be 0.5 mmol: 0.05 mol: 1000mL;
and S12, adding the antibacterial white carbon black into petroleum ether, performing ultrasonic treatment, pouring into silicon rubber latex, performing vacuum filtration after uniform stirring, stirring at a constant speed of 200r/min, adding a curing agent, namely alkyl diethanolamide, continuously stirring until no bubbles are generated, pouring into a mold, and curing for 11 hours to obtain the silicon rubber, wherein the dosage ratio of the antibacterial white carbon black, the petroleum ether, the silicon rubber latex to the curing agent is controlled to be 0.22g to 12mL to 55g to 1.5g.
Example 3
The silicone rubber is prepared by the following steps:
step S11, adding sodium silicate and sodium bicarbonate into deionized water, heating to 95 ℃, uniformly stirring and reacting for 20min, adding the sodium silicate again, uniformly stirring for 5min, adding the sodium bicarbonate, uniformly stirring and reacting for 1h, adding holmium nitrate and silver nitrate, uniformly stirring and reacting for 1h, cooling, filtering and drying after the reaction is finished to obtain the antibacterial white carbon black, wherein the dosage ratio of the sodium silicate, the sodium bicarbonate and the deionized water is controlled to be 0.01 mol: 100mL, and the dosage ratio of the holmium nitrate, the silver nitrate and the deionized water is controlled to be 0.5 mmol: 0.05 mol: 1000mL;
and S12, adding the antibacterial white carbon black into petroleum ether, performing ultrasonic treatment, pouring into silicon rubber latex, performing vacuum filtration after uniform stirring, stirring at a constant speed of 200r/min, adding a curing agent, namely alkyl diethanolamide, continuously stirring until no bubbles are generated, pouring into a mold, and curing for 12 hours to obtain the silicon rubber, wherein the dosage ratio of the antibacterial white carbon black, the petroleum ether, the silicon rubber latex to the curing agent is controlled to be 0.25 g: 15 mL: 60 g: 2g.
Example 4
A preparation method of a medical composite material comprises the following steps:
step S1, adding methyl methacrylate and dimethylaminoethanol into a reaction kettle, stirring at a constant speed, adding benzoyl peroxide and hydroquinone, stirring at a constant speed, heating to 105 ℃, carrying out reflux reaction for 4 hours, carrying out reduced pressure distillation after the reaction is finished to remove unreacted methyl methacrylate and dimethylaminoethanol to obtain an intermediate, adding the intermediate into deionized water, heating to 70 ℃, introducing methane chloride, carrying out heat preservation reaction for 5 hours, washing after the reaction is finished, standing for 30 minutes, and removing by-products under reduced pressure to obtain a graft, wherein the molar ratio of the methyl methacrylate to the dimethylaminoethanol is controlled to be 2: 1, the dosage of the benzoyl peroxide is 1 percent of the sum of the methyl methacrylate and the dimethylaminoethanol, the dosage of the hydroquinone is 0.1 percent of the weight of a catalyst, and the molar ratio of the intermediate, the methane chloride and the deionized water is 1: 0.2;
step S2, adding benzophenone and benzoin dimethyl ether into acetone, stirring at a constant speed for 30min to prepare initiator mixed solution, controlling the using amount ratio of the benzophenone, the benzoin dimethyl ether and the acetone to be 0.705: 0.075: 20mL, ultrasonically cleaning silicon rubber for 30min by using ethanol aqueous solution with the volume fraction of 50%, drying, treating for 5min by using oxygen plasma, placing the silicon rubber into the initiator mixed solution after the treatment is finished, sealing and storing for 2h at 37 ℃, taking out and naturally drying for 2h to prepare pretreated silicon rubber, and controlling the weight ratio of the initiator mixed solution to the silicon rubber to be 20: 2;
and S3, adding the graft obtained in the step S1 into deionized water, adding pretreated silicon rubber, irradiating for 5min by ultraviolet light, then ultrasonically cleaning for 5min by using an ethanol aqueous solution with the volume fraction of 50% to remove unreacted monomer and initiator mixed solution, and preparing the medical composite material, wherein the weight ratio of the graft to the deionized water to the pretreated silicon rubber is controlled to be 0.5: 1: 3.
Example 5
A preparation method of a medical composite material comprises the following steps:
step S1, adding methyl methacrylate and dimethylaminoethanol into a reaction kettle, stirring at a constant speed, adding benzoyl peroxide and hydroquinone, stirring at a constant speed, heating to 120 ℃, carrying out reflux reaction for 4 hours, carrying out reduced pressure distillation after the reaction is finished to remove unreacted methyl methacrylate and dimethylaminoethanol to obtain an intermediate, then adding the intermediate into deionized water, heating to 70 ℃, introducing methyl chloride, carrying out heat preservation reaction for 5 hours, washing and standing for 30 minutes after the reaction is finished, removing by-products under reduced pressure to obtain a graft, controlling the molar ratio of methyl methacrylate to dimethylaminoethanol to be 2.15: 1, controlling the dosage of benzoyl peroxide to be 1.2% of the sum of the weights of methyl methacrylate and dimethylaminoethanol, controlling the dosage of hydroquinone to be 0.2% of the weight of a catalyst, and controlling the molar ratio of the intermediate, the methyl chloride and the deionized water to be 1: 0.3;
step S2, adding benzophenone and benzoin dimethyl ether into acetone, stirring at a constant speed for 30min to prepare initiator mixed solution, controlling the using amount ratio of the benzophenone, the benzoin dimethyl ether and the acetone to be 0.705: 0.075: 20mL, ultrasonically cleaning silicon rubber for 30min by using ethanol aqueous solution with the volume fraction of 50%, drying, treating for 5min by using oxygen plasma, placing the silicon rubber into the initiator mixed solution after the treatment is finished, sealing and storing for 2h at 37 ℃, taking out and naturally drying for 2h to prepare pretreated silicon rubber, and controlling the weight ratio of the initiator mixed solution to the silicon rubber to be 20: 2.3;
and S3, adding the graft obtained in the step S1 into deionized water, adding pretreated silicon rubber, irradiating for 5min by ultraviolet light, then ultrasonically cleaning for 5min by using an ethanol aqueous solution with the volume fraction of 50% to remove unreacted monomer and initiator mixed solution, and preparing the medical composite material, wherein the weight ratio of the graft to the deionized water to the pretreated silicon rubber is controlled to be 0.6: 1: 4.
Example 6
A preparation method of a medical composite material comprises the following steps:
step S1, adding methyl methacrylate and dimethylaminoethanol into a reaction kettle, stirring at a constant speed, adding benzoyl peroxide and hydroquinone, stirring at a constant speed, heating to 125 ℃, carrying out reflux reaction for 4 hours, carrying out reduced pressure distillation after the reaction is finished to remove unreacted methyl methacrylate and dimethylaminoethanol to obtain an intermediate, then adding the intermediate into deionized water, heating to 70 ℃, introducing methyl chloride, carrying out heat preservation reaction for 5 hours, washing and standing for 30 minutes after the reaction is finished, removing by-products under reduced pressure to obtain a graft, controlling the molar ratio of methyl methacrylate to dimethylaminoethanol to be 2.25: 1, controlling the dosage of benzoyl peroxide to be 1-1.5 percent of the sum of the weight of methyl methacrylate and dimethylaminoethanol, the dosage of hydroquinone to be 0.3 percent of the weight of a catalyst, and controlling the molar ratio of the intermediate, the methyl chloride and the deionized water to be 1: 0.3;
s2, adding benzophenone and benzoin dimethyl ether into acetone, stirring at a constant speed for 30min to prepare initiator mixed solution, controlling the dosage ratio of the benzophenone, the benzoin dimethyl ether and the acetone to be 0.705: 0.075: 20mL, ultrasonically cleaning silicon rubber by using ethanol aqueous solution with the volume fraction of 50% for 30min, drying, treating for 5min by using oxygen plasma, placing the silicon rubber into the initiator mixed solution after the treatment is finished, sealing and storing for 2h at 37 ℃, taking out and naturally drying for 2h to prepare pretreated silicon rubber, and controlling the weight ratio of the initiator mixed solution to the silicon rubber to be 20: 2.5;
and S3, adding the graft obtained in the step S1 into deionized water, adding pretreated silicon rubber, irradiating for 5min by ultraviolet light, then ultrasonically cleaning for 5min by using an ethanol aqueous solution with the volume fraction of 50% to remove unreacted monomer and initiator mixed solution, and preparing the medical composite material, wherein the weight ratio of the graft to the deionized water to the pretreated silicon rubber is controlled to be 0.8: 1: 5.
Comparative example 1
Compared with the example 4, the antibacterial white carbon black is not added into the silicon rubber.
Comparative example 2
In comparison with example 4, the surface of the silicone rubber of this comparative example has no graft polymer.
Comparative example 3
This comparative example is an antibacterial silicone rubber material produced by a commercially available company.
Comparative example 4
Compared with example 4, the comparative example uses graphene to replace antibacterial white carbon black.
Shearing the silicon rubber materials prepared in the examples 4-6 and the comparative examples 1-3 into samples to be tested with the size of 50 multiplied by 50mm, soaking the samples for 1min by using ethanol solution with the volume fraction of 70%, taking out the samples, washing the samples by using sterile water, and sterilizing other experimental instruments for 20min at the temperature of 121 ℃; the sample to be tested is placed in a sterilized flat dish, 1.0 plus or minus 0.1mL of prepared bacteria are respectively dripped on the sample to be tested, and three parallel samples are prepared in each group. Attaching the covering film to a sample to be detected by using tweezers to ensure that the bacterial liquid is uniformly dispersed on a control sample and an experimental sample; numbering, and putting the flat dish into a constant-temperature incubator at 37 ℃ for 24 hours; after culturing, growing and propagating single cells to form colonies, counting the number of the colonies, calculating the number of bacteria in the sample, and comparing the number of bacteria in the blank sample with the number of bacteria in the detection sample to obtain the sterilization rate; the results are shown in the table:
it can be seen from the above table that the silicone rubbers prepared in examples 4 to 6 of the present invention have more excellent antibacterial properties, and compared to comparative example 4, the present invention has more excellent antibacterial properties, and further compared to comparative example 4, the present invention has synergistic antibacterial effects.
The foregoing is merely exemplary and illustrative of the principles of the present invention and various modifications, additions and substitutions of the specific embodiments described herein may be made by those skilled in the art without departing from the principles of the present invention or exceeding the scope of the claims set forth herein.
Claims (5)
1. A preparation method of a medical composite material is characterized by comprising the following steps: the method comprises the following steps:
step S1, adding methyl methacrylate and dimethylaminoethanol into a reaction kettle, stirring at a constant speed, adding a catalyst and a polymerization inhibitor, stirring at a constant speed, heating to 105-125 ℃, performing reflux reaction for 4 hours, performing reduced pressure distillation after the reaction is finished to obtain an intermediate, adding the intermediate into deionized water, heating to 70 ℃, introducing methane chloride, performing heat preservation reaction for 5 hours, washing after the reaction is finished, standing for 30 minutes, and removing a byproduct under reduced pressure to obtain a graft;
s2, adding benzophenone and benzoin dimethyl ether into acetone, stirring at a constant speed for 30min to prepare an initiator mixed solution, controlling the dosage ratio of the benzophenone, the benzoin dimethyl ether and the acetone to be 0.705: 0.075: 20mL, ultrasonically cleaning silicon rubber for 30min by using an ethanol aqueous solution with the volume fraction of 50%, drying, treating for 5min by using oxygen plasma, placing the silicon rubber into the initiator mixed solution after the treatment is finished, sealing and storing for 2h at 37 ℃, taking out and drying for 2h to prepare the pretreated silicon rubber;
and S3, adding the graft obtained in the step S1 into deionized water, adding pretreated silicon rubber, irradiating for 5min by using ultraviolet light, and then ultrasonically cleaning for 5min by using an ethanol aqueous solution with the volume fraction of 50% to obtain the medical composite material.
2. The method for preparing a medical composite material according to claim 1, wherein the method comprises the following steps: in the step S1, the molar ratio of methyl methacrylate to dimethylaminoethanol is controlled to be 2-2.25: 1, the dosage of the catalyst is 1-1.5% of the sum of the weight of methyl methacrylate and dimethylaminoethanol, the dosage of the polymerization inhibitor is 0.1-0.3% of the weight of the catalyst, the molar ratio of the intermediate, methyl chloride and deionized water is 1: 0.2-0.3, the weight ratio of the initiator mixed solution to the silicone rubber is controlled to be 20: 2-2.5 in the step S2, and the weight ratio of the graft, the deionized water and the pretreated silicone rubber is controlled to be 0.5-0.8: 1: 3-5 in the step S3.
3. The method for preparing a medical composite material according to claim 1, wherein the method comprises the following steps: the silicone rubber is prepared by the following steps:
step S11, adding sodium silicate and sodium bicarbonate into deionized water, heating to 90-95 ℃, uniformly stirring and reacting for 20min, adding the sodium silicate again, uniformly stirring for 5min, adding the sodium bicarbonate, uniformly stirring and reacting for 1h, adding holmium nitrate and silver nitrate, uniformly stirring and reacting for 1h, cooling, filtering and drying after the reaction is finished, and obtaining the antibacterial white carbon black;
and S12, adding the antibacterial white carbon black into petroleum ether, performing ultrasonic treatment, pouring into the silicone rubber latex, uniformly stirring, performing vacuum filtration, uniformly stirring at a rotating speed of 200r/min, adding a curing agent, continuously stirring until no bubbles are generated, pouring into a mold, and curing for 10-12 hours to obtain the silicone rubber.
4. A method for preparing a medical composite material according to claim 3, characterized in that: in the step S11, the dosage ratio of the sodium silicate, the sodium bicarbonate and the deionized water is controlled to be 0.01 mol: 100mL, the dosage ratio of the holmium nitrate, the silver nitrate and the deionized water is controlled to be 0.5 mmol: 0.05 mol: 1000mL, and the dosage ratio of the antibacterial white carbon black, the petroleum ether, the silicon rubber latex and the curing agent is controlled to be 0.20-0.25 g: 10-15 mL: 50-60 g: 1-2g in the step S12.
5. A medical composite material, characterized by being prepared by the preparation method of any one of claims 1 to 4.
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