CN116120680B - Hydrophilic medical material and preparation method thereof - Google Patents
Hydrophilic medical material and preparation method thereof Download PDFInfo
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- CN116120680B CN116120680B CN202310172592.4A CN202310172592A CN116120680B CN 116120680 B CN116120680 B CN 116120680B CN 202310172592 A CN202310172592 A CN 202310172592A CN 116120680 B CN116120680 B CN 116120680B
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- phenanthroline
- dimethylacetamide
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- 239000012567 medical material Substances 0.000 title claims abstract description 23
- 238000002360 preparation method Methods 0.000 title abstract description 9
- FXHOOIRPVKKKFG-UHFFFAOYSA-N N,N-Dimethylacetamide Chemical compound CN(C)C(C)=O FXHOOIRPVKKKFG-UHFFFAOYSA-N 0.000 claims abstract description 38
- DOIRQSBPFJWKBE-UHFFFAOYSA-N dibutyl phthalate Chemical compound CCCCOC(=O)C1=CC=CC=C1C(=O)OCCCC DOIRQSBPFJWKBE-UHFFFAOYSA-N 0.000 claims abstract description 36
- 239000006087 Silane Coupling Agent Substances 0.000 claims abstract description 30
- DGEZNRSVGBDHLK-UHFFFAOYSA-N [1,10]phenanthroline Chemical compound C1=CN=C2C3=NC=CC=C3C=CC2=C1 DGEZNRSVGBDHLK-UHFFFAOYSA-N 0.000 claims abstract description 27
- FOIXSVOLVBLSDH-UHFFFAOYSA-N Silver ion Chemical compound [Ag+] FOIXSVOLVBLSDH-UHFFFAOYSA-N 0.000 claims abstract description 24
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 claims abstract description 20
- 239000011593 sulfur Substances 0.000 claims abstract description 20
- 229910052717 sulfur Inorganic materials 0.000 claims abstract description 20
- 239000004698 Polyethylene Substances 0.000 claims abstract description 18
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims abstract description 18
- CJZGTCYPCWQAJB-UHFFFAOYSA-L calcium stearate Chemical compound [Ca+2].CCCCCCCCCCCCCCCCCC([O-])=O.CCCCCCCCCCCCCCCCCC([O-])=O CJZGTCYPCWQAJB-UHFFFAOYSA-L 0.000 claims abstract description 18
- 235000013539 calcium stearate Nutrition 0.000 claims abstract description 18
- 239000008116 calcium stearate Substances 0.000 claims abstract description 18
- 229910021485 fumed silica Inorganic materials 0.000 claims abstract description 18
- -1 polyethylene Polymers 0.000 claims abstract description 18
- 229920000573 polyethylene Polymers 0.000 claims abstract description 18
- 239000011347 resin Substances 0.000 claims abstract description 18
- 229920005989 resin Polymers 0.000 claims abstract description 18
- 239000002994 raw material Substances 0.000 claims abstract description 17
- 230000000844 anti-bacterial effect Effects 0.000 claims abstract description 14
- KOPOQZFJUQMUML-UHFFFAOYSA-N chlorosilane Chemical compound Cl[SiH3] KOPOQZFJUQMUML-UHFFFAOYSA-N 0.000 claims abstract description 12
- 239000007822 coupling agent Substances 0.000 claims abstract description 12
- ZAMOUSCENKQFHK-UHFFFAOYSA-N Chlorine atom Chemical compound [Cl] ZAMOUSCENKQFHK-UHFFFAOYSA-N 0.000 claims abstract description 9
- 239000000460 chlorine Substances 0.000 claims abstract description 9
- 229910052801 chlorine Inorganic materials 0.000 claims abstract description 9
- 239000000203 mixture Substances 0.000 claims description 31
- 238000001035 drying Methods 0.000 claims description 20
- 238000002156 mixing Methods 0.000 claims description 20
- 238000010438 heat treatment Methods 0.000 claims description 11
- 239000002131 composite material Substances 0.000 claims description 10
- 238000001816 cooling Methods 0.000 claims description 10
- 239000000498 cooling water 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
- 238000000034 method Methods 0.000 claims description 8
- 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
- 238000003756 stirring Methods 0.000 claims description 6
- 229910001961 silver nitrate Inorganic materials 0.000 claims description 5
- ITKVLPYNJQOCPW-UHFFFAOYSA-N chloro-(chloromethyl)-dimethylsilane Chemical group C[Si](C)(Cl)CCl ITKVLPYNJQOCPW-UHFFFAOYSA-N 0.000 claims description 4
- HKMVWLQFAYGKSI-UHFFFAOYSA-N 3-triethoxysilylpropyl thiocyanate Chemical group CCO[Si](OCC)(OCC)CCCSC#N HKMVWLQFAYGKSI-UHFFFAOYSA-N 0.000 claims description 3
- BLRPTPMANUNPDV-UHFFFAOYSA-N Silane Chemical compound [SiH4] BLRPTPMANUNPDV-UHFFFAOYSA-N 0.000 claims description 2
- 230000000379 polymerizing effect Effects 0.000 claims description 2
- 229910000077 silane Inorganic materials 0.000 claims description 2
- 239000000463 material Substances 0.000 abstract description 11
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 8
- 230000000052 comparative effect Effects 0.000 description 6
- 239000003242 anti bacterial agent Substances 0.000 description 5
- 238000012986 modification Methods 0.000 description 4
- 230000004048 modification Effects 0.000 description 4
- 239000000243 solution Substances 0.000 description 4
- 241000588724 Escherichia coli Species 0.000 description 3
- 241000191967 Staphylococcus aureus Species 0.000 description 3
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 3
- OXYZDRAJMHGSMW-UHFFFAOYSA-N 3-chloropropyl(trimethoxy)silane Chemical compound CO[Si](OC)(OC)CCCCl OXYZDRAJMHGSMW-UHFFFAOYSA-N 0.000 description 2
- SJECZPVISLOESU-UHFFFAOYSA-N 3-trimethoxysilylpropan-1-amine Chemical compound CO[Si](OC)(OC)CCCN SJECZPVISLOESU-UHFFFAOYSA-N 0.000 description 2
- 241000894006 Bacteria Species 0.000 description 2
- 125000001309 chloro group Chemical group Cl* 0.000 description 2
- OOCUOKHIVGWCTJ-UHFFFAOYSA-N chloromethyl(trimethyl)silane Chemical compound C[Si](C)(C)CCl OOCUOKHIVGWCTJ-UHFFFAOYSA-N 0.000 description 2
- BDAGIHXWWSANSR-UHFFFAOYSA-N methanoic acid Natural products OC=O BDAGIHXWWSANSR-UHFFFAOYSA-N 0.000 description 2
- 238000010998 test method Methods 0.000 description 2
- 238000012360 testing method Methods 0.000 description 2
- KSCAZPYHLGGNPZ-UHFFFAOYSA-N 3-chloropropyl(triethoxy)silane Chemical compound CCO[Si](OCC)(OCC)CCCCl KSCAZPYHLGGNPZ-UHFFFAOYSA-N 0.000 description 1
- KEZMLECYELSZDC-UHFFFAOYSA-N 3-chloropropyl-diethoxy-methylsilane Chemical compound CCO[Si](C)(OCC)CCCCl KEZMLECYELSZDC-UHFFFAOYSA-N 0.000 description 1
- KNTKCYKJRSMRMZ-UHFFFAOYSA-N 3-chloropropyl-dimethoxy-methylsilane Chemical compound CO[Si](C)(OC)CCCCl KNTKCYKJRSMRMZ-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
- 229920001661 Chitosan Polymers 0.000 description 1
- GCTFWCDSFPMHHS-UHFFFAOYSA-M Tributyltin chloride Chemical compound CCCC[Sn](Cl)(CCCC)CCCC GCTFWCDSFPMHHS-UHFFFAOYSA-M 0.000 description 1
- XEFQLINVKFYRCS-UHFFFAOYSA-N Triclosan Chemical compound OC1=CC(Cl)=CC=C1OC1=CC=C(Cl)C=C1Cl XEFQLINVKFYRCS-UHFFFAOYSA-N 0.000 description 1
- 230000000845 anti-microbial effect Effects 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
- 238000012136 culture method Methods 0.000 description 1
- 239000008367 deionised water Substances 0.000 description 1
- 229910021641 deionized water Inorganic materials 0.000 description 1
- WSFMFXQNYPNYGG-UHFFFAOYSA-M dimethyl-octadecyl-(3-trimethoxysilylpropyl)azanium;chloride Chemical compound [Cl-].CCCCCCCCCCCCCCCCCC[N+](C)(C)CCC[Si](OC)(OC)OC WSFMFXQNYPNYGG-UHFFFAOYSA-M 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
- 238000011081 inoculation Methods 0.000 description 1
- 238000011031 large-scale manufacturing process Methods 0.000 description 1
- 229910021645 metal ion Inorganic materials 0.000 description 1
- 239000011259 mixed solution Substances 0.000 description 1
- 238000011056 performance test Methods 0.000 description 1
- 238000012809 post-inoculation Methods 0.000 description 1
- 238000010992 reflux Methods 0.000 description 1
- 230000003068 static effect Effects 0.000 description 1
- 239000012815 thermoplastic material Substances 0.000 description 1
- 229960003500 triclosan Drugs 0.000 description 1
- 238000001291 vacuum drying Methods 0.000 description 1
- 238000005406 washing Methods 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
Landscapes
- 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)
Abstract
The invention relates to the technical field of materials, in particular to a hydrophilic medical material and a preparation method thereof. The hydrophilic 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 sulfur-containing silane coupling agent, 1-3 parts of polymerized phenanthroline/silver ion complex, 0.5-1.5 parts of N, N-dimethylacetamide and 0.8-1.2 parts of chlorine-containing silane coupling agent. According to the invention, the N, N-dimethylacetamide modified by the chlorsilane coupling agent is added, so that the hydrophilic property of the pvc material can be effectively improved, and meanwhile, the original antibacterial component cannot be negatively influenced, so that the prepared hydrophilic medical material has good hydrophilic property and excellent antibacterial effect.
Description
Technical Field
The invention relates to the technical field of materials, in particular to a hydrophilic medical material and a preparation method thereof.
Background
PVC is one of the most commonly used thermoplastic materials in life and is widely used in the medical and health fields because of its good transparency, good toughness and resilience, and low cost. However, since pure PVC materials do not have antibacterial ability, they are easily attached to bacteria to form a biofilm during use, so that effective antibacterial modification of PVC is necessary.
Blending with an antimicrobial agent is an effective method of improving the antimicrobial ability of PVC. Li Wei and the like, the small molecular antibacterial agent tributyltin chloride is added into PVC to successfully prepare the antibacterial soft PVC material, and the result shows that the material has good antibacterial effect on escherichia coli and staphylococcus aureus. Wu Wei the antibacterial PVC is prepared by blending nano silver antibacterial agent (AEM 5700, RHA ⁃ T2), small organic molecular antibacterial agent (BJ ⁃ 88 triclosan) and macromolecular antibacterial agent quaternized chitosan with PVC, and the result shows that when the content of the antibacterial agent is less than 1 part, the antibacterial rate of the PVC material on escherichia coli and staphylococcus aureus is 98%. However, the decrease in biocompatibility due to hydrophobicity during use is a major obstacle to the application of pvc medical materials.
Based on the above situation, the invention provides a hydrophilic medical material and a preparation method thereof.
Disclosure of Invention
The invention aims to provide a hydrophilic medical material and a preparation method thereof.
In order to achieve the above purpose, the invention provides a hydrophilic 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 sulfur-containing silane coupling agent, 1-3 parts of polymerized phenanthroline/silver ion complex, 0.5-1.5 parts of N, N-dimethylacetamide and 0.8-1.2 parts of chlorine-containing silane coupling agent.
Preferably, the coupling agent containing chlorsilane comprises one of chloromethyl trimethyl silane, chloromethyl dimethyl chlorosilane, 3-chloropropyl methyl diethoxy silane, 3-chloropropyl methyl dimethoxy silane, 3-chloropropyl triethoxy silane and 3-chloropropyl trimethoxy silane.
Preferably, the chlorsilane coupling agent is chloromethyl dimethyl chlorosilane, and cas number is 1719-57-9.
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 sulfur-containing silane is thiocyanosilane, which is 3-thiocyanopropyl triethoxysilane, cas No. 34708-08-2.
Preferably, the hydrophilic 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 sulfur-containing silane coupling agent, 3 parts of polymerized phenanthroline/silver ion complex, 1.5 parts of N, N-dimethylacetamide and 1.2 parts of chlorine-containing silane coupling agent.
Preferably, the hydrophilic 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 sulfur-containing silane coupling agent, 1 part of polymerized phenanthroline/silver ion complex, 0.5 part of N, N-dimethylacetamide and 0.8 part of chlorine-containing silane coupling agent.
The invention also provides a preparation method of the hydrophilic medical material, which comprises the following steps:
(1) Stirring and mixing N, N-dimethylacetamide and a coupling agent containing chlorsilane at the temperature of 50-55 ℃ at the rotating speed of 600-650 r/min for 45-50 min to obtain modified N, N-dimethylacetamide;
(2) Mixing pvc resin, fumed silica, dibutyl phthalate, calcium stearate, polyethylene wax, a sulfur-containing silane coupling agent, a polymerized phenanthroline/silver ion complex and modified N, N-dimethylacetamide at room temperature under the rotation speed of 400-500 r/min for 5-10 min to obtain a mixture;
(3) 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.
Compared with the prior art, the invention has the following beneficial effects:
1. according to the invention, the N, N-dimethylacetamide modified by the chlorsilane coupling agent is added, so that the hydrophilic property of the pvc material can be effectively improved, and meanwhile, the original antibacterial component cannot be negatively influenced, so that the prepared hydrophilic medical material has good hydrophilic property and excellent antibacterial effect.
2. The preparation method disclosed by the invention is convenient to operate, easy to produce on a large scale and stable in quality.
3. 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-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 to the 2, 9-dialdehyde-1, 10-phenanthroline to the silver nitrate is 1:1:1.5.
example 2
The amounts of the raw materials are shown in Table 1.
(1) Stirring and mixing N, N-dimethylacetamide and a coupling agent containing chlorsilane at the temperature of 50 ℃ and the rotating speed of 600r/min for 50min to obtain modified N, N-dimethylacetamide;
(2) Mixing pvc resin, fumed silica, dibutyl phthalate, calcium stearate, polyethylene wax, a sulfur-containing silane coupling agent, a polymerized phenanthroline/silver ion complex and modified N, N-dimethylacetamide at room temperature under stirring at a rotating speed of 400r/min for 10min to obtain a mixture;
(3) 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 5 hours at 70 ℃ to obtain the composite material.
Example 3
The amounts of the raw materials are shown in Table 1.
(1) Mixing N, N-dimethylacetamide and a coupling agent containing chlorsilane at 55 ℃ and a rotating speed of 650r/min for 45min to obtain modified N, N-dimethylacetamide;
(2) Mixing pvc resin, fumed silica, dibutyl phthalate, calcium stearate, polyethylene wax, a sulfur-containing silane coupling agent, a polymerized phenanthroline/silver ion complex and modified N, N-dimethylacetamide at room temperature under the condition of 500r/min for 5min to obtain a mixture;
(3) 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 hours at 80 ℃ to obtain the composite material.
Example 4
The amounts of the raw materials are shown in Table 1.
(1) Mixing N, N-dimethylacetamide and a coupling agent containing chlorsilane at 55 ℃ and a rotating speed of 650r/min for 50min to obtain modified N, N-dimethylacetamide;
(2) Mixing pvc resin, fumed silica, dibutyl phthalate, calcium stearate, polyethylene wax, a sulfur-containing silane coupling agent, a polymerized phenanthroline/silver ion complex and modified N, N-dimethylacetamide at room temperature under the condition of 500r/min for 10min to obtain a mixture;
(3) 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 5 hours at 80 ℃ to obtain the composite material.
Comparative example 1
Unlike example 4, N-dimethylacetamide and a silane coupling agent containing chlorine groups were not added. The amounts of the raw materials are shown in Table 1. The method comprises the following specific steps:
(1) Mixing pvc resin, fumed silica, dibutyl phthalate, calcium stearate, polyethylene wax, a sulfur-containing silane coupling agent and polymerized phenanthroline/silver ion complex for 10min at room temperature under stirring at a rotating speed of 500r/min 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 5 hours at 80 ℃ to obtain the composite material.
Comparative example 2
Unlike example 4, N-dimethylacetamide was not modified. The amounts of the raw materials are shown in Table 1. The method comprises the following specific steps:
(1) Mixing pvc resin, fumed silica, dibutyl phthalate, calcium stearate, polyethylene wax, a sulfur-containing silane coupling agent, polymerized phenanthroline/silver ion complex and N, N-dimethylacetamide for 10min at room temperature under stirring at a rotating speed of 500r/min 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 5 hours at 80 ℃ to obtain the composite material.
Comparative example 3
Unlike example 4, the silane coupling agent used for the modification of N, N-dimethylacetamide was 3-aminopropyl trimethoxysilane having no chlorine group. The amounts of the raw materials are shown in Table 1. The method comprises the following specific steps:
(1) Mixing N, N-dimethylacetamide and 3-aminopropyl trimethoxy silane at 55 ℃ at a rotating speed of 650r/min for 50min to obtain modified N, N-dimethylacetamide;
(2) Mixing pvc resin, fumed silica, dibutyl phthalate, calcium stearate, polyethylene wax, a sulfur-containing silane coupling agent, a polymerized phenanthroline/silver ion complex and modified N, N-dimethylacetamide at room temperature under the condition of 500r/min for 10min to obtain a mixture;
(3) 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 5 hours at 80 ℃ to obtain the composite material.
Comparative example 4
Unlike example 4, the chlorine-based silane coupling agent used was chloromethyltrimethylsilane. The amounts of the raw materials are shown in Table 1. The method comprises the following specific steps:
(1) Mixing N, N-dimethylacetamide and a coupling agent containing chlorsilane at 55 ℃ and a rotating speed of 650r/min for 50min to obtain modified N, N-dimethylacetamide;
(2) Mixing pvc resin, fumed silica, dibutyl phthalate, calcium stearate, polyethylene wax, a sulfur-containing silane coupling agent, a polymerized phenanthroline/silver ion complex and modified N, N-dimethylacetamide at room temperature under the condition of 500r/min for 10min to obtain a mixture;
(3) 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 5 hours at 80 ℃ to obtain the composite material.
Comparative example 5
Unlike example 4, the chlorine-based silane coupling agent used was 3-chloropropyl trimethoxysilane. The amounts of the raw materials are shown in Table 1. The method comprises the following specific steps:
(1) Mixing N, N-dimethylacetamide and a coupling agent containing chlorsilane at 55 ℃ and a rotating speed of 650r/min for 50min to obtain modified N, N-dimethylacetamide;
(2) Mixing pvc resin, fumed silica, dibutyl phthalate, calcium stearate, polyethylene wax, a sulfur-containing silane coupling agent, a polymerized phenanthroline/silver ion complex and modified N, N-dimethylacetamide at room temperature under the condition of 500r/min for 10min to obtain a mixture;
(3) 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 5 hours at 80 ℃ to obtain the 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 static water contact angle of the pvc sample was determined by dropping 3 μl of deionized water onto the pvc sheet surface using a water contact angle tester. The results are shown in Table 2.
Table 2 antibacterial test of materials
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 hydrophilic 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 sulfur-containing silane coupling agent, 1-3 parts of polymerized phenanthroline/silver ion complex, 0.5-1.5 parts of N, N-dimethylacetamide and 0.8-1.2 parts of chlorine-containing silane coupling agent;
the coupling agent containing chlorsilane is chloromethyl dimethyl chlorosilane;
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 sulfur-containing silane is thiocyanosilane, and the thiocyanosilane is 3-thiocyanopropyl triethoxysilane.
2. The hydrophilic medical material according to claim 1, wherein the hydrophilic 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 a sulfur-based silane coupling agent, 3 parts of a polymerized phenanthroline/silver ion complex, 1.5 parts of N, N-dimethylacetamide and 1.2 parts of a chlorine-based silane coupling agent.
3. The hydrophilic medical material according to claim 1, wherein the hydrophilic 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 a sulfur-containing silane coupling agent, 1 part of a polymerized phenanthroline/silver ion complex, 0.5 part of N, N-dimethylacetamide and 0.8 part of a chlorine-containing silane coupling agent.
4. The hydrophilic medical material according to claim 1, wherein the hydrophilic 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 a sulfur-based silane coupling agent, 2 parts of a polymerized phenanthroline/silver ion complex, 1 part of N, N-dimethylacetamide and 1 part of a chlorisil silane coupling agent.
5. A method for preparing the hydrophilic medical material according to any one of claims 1 to 4, comprising the steps of:
(1) Stirring and mixing N, N-dimethylacetamide and a coupling agent containing chlorsilane at the temperature of 50-55 ℃ at the rotating speed of 600-650 r/min for 45-50 min to obtain modified N, N-dimethylacetamide;
(2) PVC resin, fumed silica, dibutyl phthalate, calcium stearate, polyethylene wax, a sulfur-containing silane coupling agent, a polymerized phenanthroline/silver ion complex and modified N, N-dimethylacetamide are stirred and mixed for 5-10 min at a rotating speed of 400-500 r/min under the condition of room temperature, so as to obtain a mixture;
(3) 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. The use of a hydrophilic medical material according to any one of claims 1 to 4 for preparing a medical PVC antibacterial product.
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| CN115028953A (en) * | 2022-07-29 | 2022-09-09 | 青岛农业大学 | Antibacterial medical PVC material and preparation method thereof |
| CN115612241A (en) * | 2022-12-09 | 2023-01-17 | 黄兴盛 | Antistatic and antibacterial modified ABS resin and preparation method thereof |
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| JP4314467B2 (en) * | 2003-11-06 | 2009-08-19 | Ｊｓｒ株式会社 | Thermoplastic elastomer composition and molded article |
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