CN116178859B - Antibacterial medical material and preparation method and application thereof - Google Patents
Antibacterial medical material and preparation method and application thereof Download PDFInfo
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- CN116178859B CN116178859B CN202310150728.1A CN202310150728A CN116178859B CN 116178859 B CN116178859 B CN 116178859B CN 202310150728 A CN202310150728 A CN 202310150728A CN 116178859 B CN116178859 B CN 116178859B
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- phenanthroline
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- 230000000844 anti-bacterial effect Effects 0.000 title claims abstract description 38
- 239000012567 medical material Substances 0.000 title claims abstract description 21
- 238000002360 preparation method Methods 0.000 title claims abstract description 13
- DOIRQSBPFJWKBE-UHFFFAOYSA-N dibutyl phthalate Chemical compound CCCCOC(=O)C1=CC=CC=C1C(=O)OCCCC DOIRQSBPFJWKBE-UHFFFAOYSA-N 0.000 claims abstract description 38
- DGEZNRSVGBDHLK-UHFFFAOYSA-N [1,10]phenanthroline Chemical compound C1=CN=C2C3=NC=CC=C3C=CC2=C1 DGEZNRSVGBDHLK-UHFFFAOYSA-N 0.000 claims abstract description 37
- -1 polyethylene Polymers 0.000 claims abstract description 34
- FOIXSVOLVBLSDH-UHFFFAOYSA-N Silver ion Chemical compound [Ag+] FOIXSVOLVBLSDH-UHFFFAOYSA-N 0.000 claims abstract description 27
- 239000006087 Silane Coupling Agent Substances 0.000 claims abstract description 25
- 229920005989 resin Polymers 0.000 claims abstract description 20
- 239000011347 resin Substances 0.000 claims abstract description 20
- 239000004698 Polyethylene Substances 0.000 claims abstract description 19
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims abstract description 19
- CJZGTCYPCWQAJB-UHFFFAOYSA-L calcium stearate Chemical compound [Ca+2].CCCCCCCCCCCCCCCCCC([O-])=O.CCCCCCCCCCCCCCCCCC([O-])=O CJZGTCYPCWQAJB-UHFFFAOYSA-L 0.000 claims abstract description 19
- 235000013539 calcium stearate Nutrition 0.000 claims abstract description 19
- 239000008116 calcium stearate Substances 0.000 claims abstract description 19
- 229910021485 fumed silica Inorganic materials 0.000 claims abstract description 19
- 229920000573 polyethylene Polymers 0.000 claims abstract description 19
- 239000002994 raw material Substances 0.000 claims abstract description 18
- 230000003385 bacteriostatic effect Effects 0.000 claims abstract description 11
- 239000000203 mixture Substances 0.000 claims description 22
- 238000001035 drying Methods 0.000 claims description 20
- 238000001816 cooling Methods 0.000 claims description 19
- 238000002156 mixing Methods 0.000 claims description 12
- 238000010438 heat treatment Methods 0.000 claims description 11
- 239000002131 composite material Substances 0.000 claims description 10
- 238000001125 extrusion Methods 0.000 claims description 10
- SQGYOTSLMSWVJD-UHFFFAOYSA-N silver(1+) nitrate Chemical compound [Ag+].[O-]N(=O)=O SQGYOTSLMSWVJD-UHFFFAOYSA-N 0.000 claims description 10
- 238000003756 stirring Methods 0.000 claims description 10
- 238000000034 method Methods 0.000 claims description 9
- MNXMBMNXSPNINS-UHFFFAOYSA-N 1,10-phenanthroline-5,6-diamine Chemical compound C1=CC=C2C(N)=C(N)C3=CC=CN=C3C2=N1 MNXMBMNXSPNINS-UHFFFAOYSA-N 0.000 claims description 6
- 229910001961 silver nitrate Inorganic materials 0.000 claims description 5
- HKMVWLQFAYGKSI-UHFFFAOYSA-N 3-triethoxysilylpropyl thiocyanate Chemical group CCO[Si](OCC)(OCC)CCCSC#N HKMVWLQFAYGKSI-UHFFFAOYSA-N 0.000 claims description 3
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims description 2
- 238000001802 infusion Methods 0.000 claims description 2
- 229910052760 oxygen Inorganic materials 0.000 claims description 2
- 239000001301 oxygen Substances 0.000 claims description 2
- 230000000379 polymerizing effect Effects 0.000 claims description 2
- 239000000498 cooling water Substances 0.000 claims 1
- 239000000463 material Substances 0.000 abstract description 32
- 229910052709 silver Inorganic materials 0.000 abstract description 9
- 239000004332 silver Substances 0.000 abstract description 9
- 241000191967 Staphylococcus aureus Species 0.000 abstract description 5
- 241000588724 Escherichia coli Species 0.000 abstract description 3
- 239000002262 Schiff base Substances 0.000 abstract description 2
- 150000004753 Schiff bases Chemical class 0.000 abstract description 2
- 244000052616 bacterial pathogen Species 0.000 abstract description 2
- 230000000694 effects Effects 0.000 abstract description 2
- 230000005764 inhibitory process Effects 0.000 abstract description 2
- 230000000052 comparative effect Effects 0.000 description 17
- 239000003242 anti bacterial agent Substances 0.000 description 13
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 9
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 8
- 239000004743 Polypropylene Substances 0.000 description 8
- 229920001155 polypropylene Polymers 0.000 description 8
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 description 7
- ZNZYKNKBJPZETN-WELNAUFTSA-N Dialdehyde 11678 Chemical compound N1C2=CC=CC=C2C2=C1[C@H](C[C@H](/C(=C/O)C(=O)OC)[C@@H](C=C)C=O)NCC2 ZNZYKNKBJPZETN-WELNAUFTSA-N 0.000 description 4
- 239000000243 solution Substances 0.000 description 4
- 230000032683 aging Effects 0.000 description 3
- 238000004806 packaging method and process Methods 0.000 description 3
- 238000010998 test method Methods 0.000 description 3
- 238000012360 testing method Methods 0.000 description 3
- 241000894006 Bacteria Species 0.000 description 2
- 239000004594 Masterbatch (MB) Substances 0.000 description 2
- BLRPTPMANUNPDV-UHFFFAOYSA-N Silane Chemical compound [SiH4] BLRPTPMANUNPDV-UHFFFAOYSA-N 0.000 description 2
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical group [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 description 2
- 230000000845 anti-microbial effect Effects 0.000 description 2
- 230000006378 damage Effects 0.000 description 2
- 239000005038 ethylene vinyl acetate Substances 0.000 description 2
- BDAGIHXWWSANSR-UHFFFAOYSA-N methanoic acid Natural products OC=O BDAGIHXWWSANSR-UHFFFAOYSA-N 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 229920001200 poly(ethylene-vinyl acetate) Polymers 0.000 description 2
- 230000035755 proliferation Effects 0.000 description 2
- 229910000077 silane Inorganic materials 0.000 description 2
- 229920002379 silicone rubber Polymers 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 229910052717 sulfur Inorganic materials 0.000 description 2
- 239000011593 sulfur Substances 0.000 description 2
- WYTZZXDRDKSJID-UHFFFAOYSA-N (3-aminopropyl)triethoxysilane Chemical compound CCO[Si](OCC)(OCC)CCCN WYTZZXDRDKSJID-UHFFFAOYSA-N 0.000 description 1
- KSCAZPYHLGGNPZ-UHFFFAOYSA-N 3-chloropropyl(triethoxy)silane Chemical compound CCO[Si](OCC)(OCC)CCCCl KSCAZPYHLGGNPZ-UHFFFAOYSA-N 0.000 description 1
- DCQBZYNUSLHVJC-UHFFFAOYSA-N 3-triethoxysilylpropane-1-thiol Chemical compound CCO[Si](OCC)(OCC)CCCS DCQBZYNUSLHVJC-UHFFFAOYSA-N 0.000 description 1
- UUEWCQRISZBELL-UHFFFAOYSA-N 3-trimethoxysilylpropane-1-thiol Chemical compound CO[Si](OC)(OC)CCCS UUEWCQRISZBELL-UHFFFAOYSA-N 0.000 description 1
- OSWFIVFLDKOXQC-UHFFFAOYSA-N 4-(3-methoxyphenyl)aniline Chemical compound COC1=CC=CC(C=2C=CC(N)=CC=2)=C1 OSWFIVFLDKOXQC-UHFFFAOYSA-N 0.000 description 1
- 241000195493 Cryptophyta Species 0.000 description 1
- 239000004944 Liquid Silicone Rubber Substances 0.000 description 1
- 241000700605 Viruses Species 0.000 description 1
- 239000004599 antimicrobial Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 239000003638 chemical reducing agent Substances 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 239000007822 coupling agent Substances 0.000 description 1
- 238000012136 culture method Methods 0.000 description 1
- 238000001514 detection method Methods 0.000 description 1
- 238000011156 evaluation Methods 0.000 description 1
- 239000007888 film coating Substances 0.000 description 1
- 238000009501 film coating Methods 0.000 description 1
- 238000001914 filtration Methods 0.000 description 1
- 235000019253 formic acid Nutrition 0.000 description 1
- 230000002401 inhibitory effect Effects 0.000 description 1
- 238000001746 injection moulding Methods 0.000 description 1
- 238000011081 inoculation Methods 0.000 description 1
- 229910003471 inorganic composite material Inorganic materials 0.000 description 1
- 238000011031 large-scale manufacturing process Methods 0.000 description 1
- 239000007791 liquid phase Substances 0.000 description 1
- 230000005923 long-lasting effect Effects 0.000 description 1
- 238000002844 melting Methods 0.000 description 1
- 230000008018 melting Effects 0.000 description 1
- 229910021645 metal ion Inorganic materials 0.000 description 1
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 description 1
- 244000005700 microbiome Species 0.000 description 1
- 239000011259 mixed solution Substances 0.000 description 1
- 231100000956 nontoxicity Toxicity 0.000 description 1
- 230000001590 oxidative effect Effects 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 238000011056 performance test Methods 0.000 description 1
- 238000012809 post-inoculation Methods 0.000 description 1
- 238000006722 reduction reaction Methods 0.000 description 1
- 238000010992 reflux Methods 0.000 description 1
- 239000004945 silicone rubber Substances 0.000 description 1
- 238000001291 vacuum drying Methods 0.000 description 1
- 238000005406 washing Methods 0.000 description 1
- 229910052724 xenon Inorganic materials 0.000 description 1
- FHNFHKCVQCLJFQ-UHFFFAOYSA-N xenon atom Chemical compound [Xe] FHNFHKCVQCLJFQ-UHFFFAOYSA-N 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
- C08L27/00—Compositions of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by a halogen; Compositions of derivatives of such polymers
- C08L27/02—Compositions of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by a halogen; Compositions of derivatives of such polymers not modified by chemical after-treatment
- C08L27/04—Compositions of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by a halogen; Compositions of derivatives of such polymers not modified by chemical after-treatment containing chlorine atoms
- C08L27/06—Homopolymers or copolymers of vinyl chloride
-
- 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
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- Chemical & Material Sciences (AREA)
- Health & Medical Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Organic Chemistry (AREA)
- Compositions Of Macromolecular Compounds (AREA)
- Agricultural Chemicals And Associated Chemicals (AREA)
Abstract
The invention relates to the technical field of materials, in particular to a bacteriostatic medical material and a preparation method and application thereof. The antibacterial medical material is prepared from the following raw materials in parts by weight: 90-100 parts of pvc resin, 2-6 parts of fumed silica, 20-30 parts of dibutyl phthalate, 3-5 parts of calcium stearate, 1-3 parts of polyethylene wax, 1.5-5 parts of silane coupling agent and 1-3 parts of polymerized phenanthroline/silver ion complex. The antibacterial medical material prepared by the invention contains the polymerized phenanthroline/silver ion complex, and has remarkable inhibition effect on pathogenic bacteria such as escherichia coli, staphylococcus aureus and the like. The principle is that after the silver ions are coordinated with N of Schiff base of phenanthroline, the compatibility of the silver ions in pvc material is better, so that the antibacterial capability is improved.
Description
Technical Field
The invention relates to the technical field of materials, in particular to a bacteriostatic medical material and a preparation method and application thereof.
Background
Antibacterial materials are a class of materials that can inhibit proliferation or kill bacteria, mold, algae, even viruses, etc. that are contaminated on the surface of the material in a use environment, and that keep themselves clean by inhibiting the proliferation of microorganisms. In particular, in food packaging, a packaging product of an antibacterial material plays an important role in prolonging the shelf life of food and improving the safety of food.
The antibacterial material is used by firstly meeting the necessary requirements of physical, chemical, mechanical and other properties of the material when the material is used as a basic material, and simultaneously taking the requirement of the special function of antibacterial and the additional factors generated by the requirement into consideration. Therefore, the antibacterial material has good mechanical strength appearance, chemical stability and processability. In terms of antibacterial properties, antibacterial materials are required to be able to adapt to the use environment, and should have high-efficiency, broad-spectrum, long-lasting antibacterial properties. Because the antibacterial material contains a small amount of antibacterial agent, the antibacterial agent is required to achieve the specified sanitary safety, and the final antibacterial material finished product meets the requirements of no toxicity, no peculiar smell and no harm to the environment.
Antibacterial agents are often added to the master batch of materials from which the material article is made, thereby obtaining the antibacterial material article. The antibacterial agents added at present are generally mainly organic antibacterial agents and inorganic antibacterial agents. All of which can be used in the material. However, when the antibacterial agent is used, the antibacterial agent is required to have an antibacterial effect on the surface of the material, but the antibacterial agent on the surface is easy to run off, so that the antibacterial efficiency and the antibacterial durability of the conventional antibacterial material packaging product are not ideal.
At present, the widely used antibacterial agent in the inorganic antibacterial material is mainly nano silver or silver ions, has the characteristics of broad spectrum and high antibacterial efficiency, and for example, patent CN 109912982B discloses biomedical silicone rubber with antibacterial property, which comprises nano silver wrapped by graphene quantum dots, liquid silicone rubber and a curing agent; patent CN 109233300B discloses a preparation method of nano silver antibacterial agent, antibacterial material and preparation method of antibacterial material. The preparation method of the nano silver antibacterial agent comprises the steps of adopting a liquid phase chemical reduction method, reducing Ag+ into nano Ag particles at a certain temperature, adding the silver-containing antibacterial agent into ethylene vinyl acetate copolymer (EVA resin) master batch, uniformly mixing, pouring into a forming machine, extruding through a nut, melting at a high temperature, and finally injection molding; finally obtaining the required organic/inorganic composite material. However, the use of nano silver or silver ions as an antimicrobial agent is costly, and during the use of the antimicrobial material, silver leaks into the environment, thereby oxidizing to affect the antimicrobial effect.
Based on the above situation, the invention provides a bacteriostatic medical material and a preparation method and application thereof.
Disclosure of Invention
The invention aims to provide a bacteriostatic medical material and a preparation method and application thereof.
In order to achieve the above purpose, the invention provides a bacteriostatic medical material, which is prepared from the following raw materials in parts by weight: 90-100 parts of pvc resin, 2-6 parts of fumed silica, 20-30 parts of dibutyl phthalate, 3-5 parts of calcium stearate, 1-3 parts of polyethylene wax, 1.5-5 parts of silane coupling agent and 1-3 parts of polymerized phenanthroline/silver ion complex.
Preferably, the antibacterial medical material is prepared from the following raw materials in parts by weight: 90 parts of pvc resin, 2 parts of fumed silica, 20 parts of dibutyl phthalate, 3 parts of calcium stearate, 1 part of polyethylene wax, 1.5 parts of silane coupling agent and 1 part of polymerized phenanthroline/silver ion complex.
Preferably, the antibacterial medical material is prepared from the following raw materials in parts by weight: 100 parts of pvc resin, 6 parts of fumed silica, 30 parts of dibutyl phthalate, 5 parts of calcium stearate, 3 parts of polyethylene wax, 5 parts of silane coupling agent and 3 parts of polymerized phenanthroline/silver ion complex.
Preferably, the antibacterial medical material is prepared from the following raw materials in parts by weight: 95 parts of pvc resin, 4 parts of fumed silica, 25 parts of dibutyl phthalate, 4 parts of calcium stearate, 2 parts of polyethylene wax, 3 parts of silane coupling agent and 2 parts of polymerized phenanthroline/silver ion complex.
Preferably, the polymerized phenanthroline/silver ion complex is prepared by mixing polymerized phenanthroline with silver nitrate.
Preferably, the polymerized phenanthroline is prepared by polymerizing 5,6 diamino 1,10 phenanthroline and 2,9 dialdehyde 1,10 phenanthroline.
Preferably, the molar ratio of 5,6 diamino 1,10 phenanthroline, 2,9 dialdehyde 1,10 phenanthroline and silver nitrate in the polymerized phenanthroline/silver ion complex is 1:1:1.5.
preferably, the silane coupling agent is a sulfur-containing silane.
Preferably, the sulfur-containing silane is thiocyanosilane, which is 3-thiocyanopropyl triethoxysilane, cas No. 34708-08-2.
The invention also provides a preparation method of the antibacterial medical material, which comprises the following steps:
(1) Premixing pvc resin, fumed silica, dibutyl phthalate, calcium stearate, polyethylene wax, a silane coupling agent and a polymerized phenanthroline/silver ion complex to obtain a premix, transferring the premix into a high-speed mixer, and stirring and mixing at a rotating speed of 400-500 r/min for 5-10 min at room temperature to obtain a mixture;
(2) Adding the mixture into a double-screw extruder through a charging hopper for heating extrusion treatment, wherein the temperature interval of the double-screw extruder is 180-210 ℃, extruding by the double-screw extruder, cooling by water at 25 ℃ in sequence, drying by air cooling, granulating in a granulator at a rotating speed of 3000r/min, and finally drying for 4-5 hours at 70-80 ℃ to obtain the composite material.
The invention provides the use of bacteriostatic medical material in preparing medical pvc products of the following types, but not limited to: medical pvc infusion tube, medical pvc glove, medical pvc emergency ball, medical pvc oxygen mask.
Compared with the prior art, the invention has the following beneficial effects:
1. the antibacterial medical material prepared by the invention contains the polymerized phenanthroline/silver ion complex, and has remarkable inhibition effect on pathogenic bacteria such as escherichia coli, staphylococcus aureus and the like. The principle is that after the silver ions are coordinated with N of Schiff base of phenanthroline, the compatibility of the silver ions in pvc material is better, so that the antibacterial capability is improved.
2. According to the invention, the thiocyanosilane coupling agent is added, so that the damage of light waves to the coordination bond of silver ions and phenanthroline can be effectively prevented, and a good antibacterial effect is maintained.
3. The preparation method disclosed by the invention is convenient to operate, easy to produce on a large scale and stable in quality.
4. The raw materials of the invention are abundant in China and have proper price, so that the large-scale production of the invention has no high cost limit.
Detailed Description
EXAMPLE 1 preparation of polymerized phenanthroline/silver ion Complex
Reference 202211576888.4 method for preparing polymeric phenanthroline/silver ion complexes
(1) 5,6 diamino 1,10 phenanthroline, formic acid and ethanol are mixed according to a mole ratio of 1:0.2:60, preparing a solution A;
(2) 2,9 dialdehyde group 1,10 phenanthroline and ethanol are mixed according to a mole ratio of 1:60, preparing a solution B;
(3) Slowly dripping the solution A into the solution B, and reacting for 12 hours at 30 ℃;
(4) Silver nitrate and ethanol are mixed according to a mole ratio of 1:75, then slowly dripping the mixture into the mixed solution in the step (3), heating to 65 ℃ and carrying out reflux reaction for 4 hours;
(5) Filtering, washing with ethanol, and vacuum drying to obtain a polymerized phenanthroline/metal ion complex; wherein, the molar ratio of the 5,6 diamino 1,10 phenanthroline, the 2,9 dialdehyde 1,10 phenanthroline and the silver nitrate is 1:1:1.5.
example 2
The amounts of the raw materials are shown in Table 1.
(1) Premixing pvc resin, fumed silica, dibutyl phthalate, calcium stearate, polyethylene wax, a silane coupling agent and a polymerized phenanthroline/silver ion complex to obtain a premix, transferring the premix into a high-speed mixer, and stirring and mixing at a rotating speed of 400r/min for 10min at room temperature to obtain a mixture;
(2) Adding the mixture into a double-screw extruder through a charging hopper for heating extrusion treatment, wherein the temperature interval of the double-screw extruder is 180-210 ℃, extruding by the double-screw extruder, cooling by water at 25 ℃ in sequence, drying by air cooling, granulating in a granulator at a rotating speed of 3000r/min, and finally drying for 5h at 70 ℃ to obtain the modified polypropylene composite material.
Example 3
The amounts of the raw materials are shown in Table 1.
(1) Premixing pvc resin, fumed silica, dibutyl phthalate, calcium stearate, polyethylene wax, a silane coupling agent and a polymerized phenanthroline/silver ion complex to obtain a premix, transferring the premix into a high-speed mixer, and stirring and mixing at a rotating speed of 500r/min for 5min at room temperature to obtain a mixture;
(2) Adding the mixture into a double-screw extruder through a charging hopper for heating extrusion treatment, wherein the temperature interval of the double-screw extruder is 180-210 ℃, extruding by the double-screw extruder, cooling by water at 25 ℃ in sequence, drying by air cooling, granulating in a granulator at a rotating speed of 3000r/min, and finally drying for 4 hours at 80 ℃ to obtain the modified polypropylene composite material.
Example 4
The amounts of the raw materials are shown in Table 1.
(1) Premixing pvc resin, fumed silica, dibutyl phthalate, calcium stearate, polyethylene wax, a silane coupling agent and a polymerized phenanthroline/silver ion complex to obtain a premix, transferring the premix into a high-speed mixer, and stirring and mixing at a rotating speed of 500r/min for 10min at room temperature to obtain a mixture;
(2) Adding the mixture into a double-screw extruder through a charging hopper for heating extrusion treatment, wherein the temperature interval of the double-screw extruder is 180-210 ℃, extruding by the double-screw extruder, cooling by water at 25 ℃ in sequence, drying by air cooling, granulating in a granulator at a rotating speed of 3000r/min, and finally drying for 5h at 80 ℃ to obtain the modified polypropylene composite material.
Comparative example 1
Unlike example 4, the silane coupling agent used was 3-mercaptopropyl triethoxysilane. The amounts of the raw materials are shown in Table 1. The method comprises the following specific steps:
(1) Premixing pvc resin, fumed silica, dibutyl phthalate, calcium stearate, polyethylene wax, a silane coupling agent and a polymerized phenanthroline/silver ion complex to obtain a premix, transferring the premix into a high-speed mixer, and stirring and mixing at a rotating speed of 500r/min for 10min at room temperature to obtain a mixture;
(2) Adding the mixture into a double-screw extruder through a charging hopper for heating extrusion treatment, wherein the temperature interval of the double-screw extruder is 180-210 ℃, extruding by the double-screw extruder, cooling by water at 25 ℃ in sequence, drying by air cooling, granulating in a granulator at a rotating speed of 3000r/min, and finally drying for 5h at 80 ℃ to obtain the modified polypropylene composite material.
Comparative example 2
Unlike example 4, the silane coupling agent used was 3-mercaptopropyl trimethoxysilane. The amounts of the raw materials are shown in Table 1. The method comprises the following specific steps:
(1) Premixing pvc resin, fumed silica, dibutyl phthalate, calcium stearate, polyethylene wax, a silane coupling agent and a polymerized phenanthroline/silver ion complex to obtain a premix, transferring the premix into a high-speed mixer, and stirring and mixing at a rotating speed of 500r/min for 10min at room temperature to obtain a mixture;
(2) Adding the mixture into a double-screw extruder through a charging hopper for heating extrusion treatment, wherein the temperature interval of the double-screw extruder is 180-210 ℃, extruding by the double-screw extruder, cooling by water at 25 ℃ in sequence, drying by air cooling, granulating in a granulator at a rotating speed of 3000r/min, and finally drying for 5h at 80 ℃ to obtain the modified polypropylene composite material.
Comparative example 3
Unlike example 4, the silane coupling agent used was 3-aminopropyl triethoxysilane. The amounts of the raw materials are shown in Table 1. The method comprises the following specific steps:
(1) Premixing pvc resin, fumed silica, dibutyl phthalate, calcium stearate, polyethylene wax, a silane coupling agent and a polymerized phenanthroline/silver ion complex to obtain a premix, transferring the premix into a high-speed mixer, and stirring and mixing at a rotating speed of 500r/min for 10min at room temperature to obtain a mixture;
(2) Adding the mixture into a double-screw extruder through a charging hopper for heating extrusion treatment, wherein the temperature interval of the double-screw extruder is 180-210 ℃, extruding by the double-screw extruder, cooling by water at 25 ℃ in sequence, drying by air cooling, granulating in a granulator at a rotating speed of 3000r/min, and finally drying for 5h at 80 ℃ to obtain the modified polypropylene composite material.
Comparative example 4
Unlike example 4, the silane coupling agent used was 3-chloropropyl triethoxysilane. The amounts of the raw materials are shown in Table 1. The method comprises the following specific steps:
(1) Premixing pvc resin, fumed silica, dibutyl phthalate, calcium stearate, polyethylene wax, a silane coupling agent and a polymerized phenanthroline/silver ion complex to obtain a premix, transferring the premix into a high-speed mixer, and stirring and mixing at a rotating speed of 500r/min for 10min at room temperature to obtain a mixture;
(2) Adding the mixture into a double-screw extruder through a charging hopper for heating extrusion treatment, wherein the temperature interval of the double-screw extruder is 180-210 ℃, extruding by the double-screw extruder, cooling by water at 25 ℃ in sequence, drying by air cooling, granulating in a granulator at a rotating speed of 3000r/min, and finally drying for 5h at 80 ℃ to obtain the modified polypropylene composite material.
Comparative example 5
Unlike example 4, a silane coupling agent was not added. The amounts of the raw materials are shown in Table 1. The method comprises the following specific steps:
(1) Premixing pvc resin, fumed silica, dibutyl phthalate, calcium stearate, polyethylene wax and polymerized phenanthroline/silver ion complex to obtain premix, transferring the premix into a high-speed mixer, and stirring and mixing at a rotating speed of 500r/min for 10min at room temperature to obtain a mixture;
(2) Adding the mixture into a double-screw extruder through a charging hopper for heating extrusion treatment, wherein the temperature interval of the double-screw extruder is 180-210 ℃, extruding by the double-screw extruder, cooling by water at 25 ℃ in sequence, drying by air cooling, granulating in a granulator at a rotating speed of 3000r/min, and finally drying for 5h at 80 ℃ to obtain the modified polypropylene composite material.
TABLE 1
Performance test and evaluation
The materials obtained in each example and comparative example were prepared into square sample pieces of 50mm×50mm×5mm by referring to the standard "test method for surface antibacterial Property of Material (GB/T31402 2015), and antibacterial rates of each test sample against Escherichia coli and Staphylococcus aureus were obtained by referring to the above standard for the bacteria pre-culture, inoculation, film coating, post-inoculation culture and test methods. The results are shown in Table 2.
Table 2 antibacterial test of materials
| Coli bacterium | Staphylococcus aureus | |
| Example 1 | 97.26 | 95.11 |
| Example 2 | 98.41 | 97.32 |
| Example 3 | 99.58 | 98.26 |
| Comparative example 1 | 98.15 | 96.74 |
| Comparative example 2 | 98.36 | 97.63 |
| Comparative example 3 | 97.52 | 95.27 |
| Comparative example 4 | 96.31 | 94.33 |
| Comparative example 5 | 95.18 | 92.18 |
And (3) ageing resistance detection: the aging-resistant material samples obtained in examples and comparative examples were subjected to aging treatment with reference to "materials laboratory light source exposure test method" GB/T16422.2-2014, a xenon arc lamp was filtered by a filter for simulating sunlight, exposure cycles were performed according to method A cycle number 1, and after irradiation for 600 hours, the antibacterial rate was detected according to the above-described scheme. The results are shown in Table 3.
Table 3 antibacterial test of materials
| Coli bacterium | Staphylococcus aureus | |
| Example 1 | 96.15 | 93.25 |
| Example 2 | 97.51 | 96.82 |
| Example 3 | 98.48 | 97.12 |
| Comparative example 1 | 72.35 | 70.22 |
| Comparative example 2 | 69.65 | 65.91 |
| Comparative example 3 | 80.18 | 77.38 |
| Comparative example 4 | 79.45 | 74.15 |
| Comparative example 5 | 43.62 | 31.85 |
The foregoing descriptions of specific exemplary embodiments of the present invention are presented for purposes of illustration and description. It is not intended to limit the invention to the precise form disclosed, and obviously many modifications and variations are possible in light of the above teaching. The exemplary embodiments were chosen and described in order to explain the specific principles of the invention and its practical application to thereby enable one skilled in the art to make and utilize the invention in various exemplary embodiments and with various modifications as are suited to the particular use contemplated. It is intended that the scope of the invention be defined by the claims and their equivalents.
Claims (6)
1. The antibacterial medical material is characterized by being prepared from the following raw materials in parts by weight: 90-100 parts of pvc resin, 2-6 parts of fumed silica, 20-30 parts of dibutyl phthalate, 3-5 parts of calcium stearate, 1-3 parts of polyethylene wax, 1.5-5 parts of silane coupling agent and 1-3 parts of polymerized phenanthroline/silver ion complex;
the polymerized phenanthroline is prepared by polymerizing 5, 6-diamino-1, 10-phenanthroline and 2, 9-dialdehyde-1, 10-phenanthroline; the molar ratio of the 5, 6-diamino-1, 10-phenanthroline, 2, 9-dialdehyde-1, 10-phenanthroline and silver nitrate in the polymerized phenanthroline/silver ion complex is 1:1:1.5;
the silane coupling agent is 3-thiocyanopropyl triethoxysilane.
2. The bacteriostatic medical material according to claim 1, which is prepared from the following raw materials in parts by weight: 90 parts of pvc resin, 2 parts of fumed silica, 20 parts of dibutyl phthalate, 3 parts of calcium stearate, 1 part of polyethylene wax, 1.5 parts of silane coupling agent and 1 part of polymerized phenanthroline/silver ion complex.
3. The bacteriostatic medical material according to claim 1, which is prepared from the following raw materials in parts by weight: 100 parts of pvc resin, 6 parts of fumed silica, 30 parts of dibutyl phthalate, 5 parts of calcium stearate, 3 parts of polyethylene wax, 5 parts of silane coupling agent and 3 parts of polymerized phenanthroline/silver ion complex.
4. The bacteriostatic medical material according to claim 1, which is prepared from the following raw materials in parts by weight: 95 parts of pvc resin, 4 parts of fumed silica, 25 parts of dibutyl phthalate, 4 parts of calcium stearate, 2 parts of polyethylene wax, 3 parts of silane coupling agent and 2 parts of polymerized phenanthroline/silver ion complex.
5. A method for preparing the bacteriostatic medical material according to any one of claims 1-4, which is characterized by comprising the following steps:
(1) Premixing pvc resin, fumed silica, dibutyl phthalate, calcium stearate, polyethylene wax, a silane coupling agent and a polymerized phenanthroline/silver ion complex to obtain a premix, transferring the premix into a high-speed mixer, and stirring and mixing at a rotating speed of 400-500 r/min for 5-10 min at room temperature to obtain a mixture;
(2) And adding the mixture into a double-screw extruder through a charging hopper for heating extrusion treatment, wherein the temperature interval of the double-screw extruder is 180-210 ℃, after the mixture is extruded by the double-screw extruder, cooling water at 25 ℃ and drying by air cooling in sequence, granulating in a granulator at a rotating speed of 3000r/min, and finally drying for 4-5 hours at 70-80 ℃ to obtain the composite material.
6. Use of the bacteriostatic medical material according to any one of claims 1-4 for the preparation of medical pvc products of the type including but not limited to: medical pvc infusion tube, medical pvc glove, medical pvc emergency ball, and medical pvc oxygen mask.
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