CN111138749A - Antibacterial anti-static foamed elastomer material and preparation method thereof - Google Patents
Antibacterial anti-static foamed elastomer material and preparation method thereof Download PDFInfo
- Publication number
- CN111138749A CN111138749A CN201911335166.8A CN201911335166A CN111138749A CN 111138749 A CN111138749 A CN 111138749A CN 201911335166 A CN201911335166 A CN 201911335166A CN 111138749 A CN111138749 A CN 111138749A
- Authority
- CN
- China
- Prior art keywords
- phosphonium salt
- antimony oxide
- quaternary phosphonium
- tin antimony
- agent
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Granted
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- 230000000844 anti-bacterial effect Effects 0.000 title claims abstract description 38
- 229920001971 elastomer Polymers 0.000 title claims abstract description 31
- 239000000463 material Substances 0.000 title claims abstract description 23
- 239000000806 elastomer Substances 0.000 title claims abstract description 21
- 238000002360 preparation method Methods 0.000 title claims abstract description 15
- -1 phosphonium salt modified tin antimony oxide Chemical class 0.000 claims abstract description 39
- 150000004714 phosphonium salts Chemical group 0.000 claims abstract description 21
- XXLJGBGJDROPKW-UHFFFAOYSA-N antimony;oxotin Chemical compound [Sb].[Sn]=O XXLJGBGJDROPKW-UHFFFAOYSA-N 0.000 claims abstract description 20
- 238000005187 foaming Methods 0.000 claims abstract description 19
- 239000007822 coupling agent Substances 0.000 claims abstract description 15
- 239000004088 foaming agent Substances 0.000 claims abstract description 14
- 239000000203 mixture Substances 0.000 claims abstract description 10
- 239000005060 rubber Substances 0.000 claims abstract description 10
- 238000000227 grinding Methods 0.000 claims abstract description 9
- 239000002245 particle Substances 0.000 claims abstract description 8
- 239000003431 cross linking reagent Substances 0.000 claims abstract description 7
- 238000001035 drying Methods 0.000 claims abstract description 7
- 239000012266 salt solution Substances 0.000 claims abstract description 7
- 150000001875 compounds Chemical class 0.000 claims abstract description 6
- 238000002156 mixing Methods 0.000 claims abstract description 6
- 238000004132 cross linking Methods 0.000 claims abstract description 3
- 238000007493 shaping process Methods 0.000 claims abstract description 3
- 229920001200 poly(ethylene-vinyl acetate) Polymers 0.000 claims description 27
- XLOMVQKBTHCTTD-UHFFFAOYSA-N Zinc monoxide Chemical group [Zn]=O XLOMVQKBTHCTTD-UHFFFAOYSA-N 0.000 claims description 10
- 239000004372 Polyvinyl alcohol Substances 0.000 claims description 9
- 229920002451 polyvinyl alcohol Polymers 0.000 claims description 9
- 239000000243 solution Substances 0.000 claims description 9
- 229920001903 high density polyethylene Polymers 0.000 claims description 7
- 239000004700 high-density polyethylene Substances 0.000 claims description 7
- 239000004156 Azodicarbonamide Substances 0.000 claims description 6
- VTYYLEPIZMXCLO-UHFFFAOYSA-L Calcium carbonate Chemical compound [Ca+2].[O-]C([O-])=O VTYYLEPIZMXCLO-UHFFFAOYSA-L 0.000 claims description 6
- XOZUGNYVDXMRKW-AATRIKPKSA-N azodicarbonamide Chemical compound NC(=O)\N=N\C(N)=O XOZUGNYVDXMRKW-AATRIKPKSA-N 0.000 claims description 6
- 235000019399 azodicarbonamide Nutrition 0.000 claims description 6
- 229920002959 polymer blend Polymers 0.000 claims description 6
- 239000012744 reinforcing agent Substances 0.000 claims description 6
- 244000043261 Hevea brasiliensis Species 0.000 claims description 5
- 235000021355 Stearic acid Nutrition 0.000 claims description 5
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 claims description 5
- 150000004645 aluminates Chemical class 0.000 claims description 5
- 239000006229 carbon black Substances 0.000 claims description 5
- 238000000034 method Methods 0.000 claims description 5
- 229920003052 natural elastomer Polymers 0.000 claims description 5
- 229920001194 natural rubber Polymers 0.000 claims description 5
- QIQXTHQIDYTFRH-UHFFFAOYSA-N octadecanoic acid Chemical compound CCCCCCCCCCCCCCCCCC(O)=O QIQXTHQIDYTFRH-UHFFFAOYSA-N 0.000 claims description 5
- OQCDKBAXFALNLD-UHFFFAOYSA-N octadecanoic acid Natural products CCCCCCCC(C)CCCCCCCCC(O)=O OQCDKBAXFALNLD-UHFFFAOYSA-N 0.000 claims description 5
- 239000008117 stearic acid Substances 0.000 claims description 5
- 229920003048 styrene butadiene rubber Polymers 0.000 claims description 5
- 239000011787 zinc oxide Substances 0.000 claims description 5
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 4
- 230000004048 modification Effects 0.000 claims description 4
- 238000012986 modification Methods 0.000 claims description 4
- CCNDOQHYOIISTA-UHFFFAOYSA-N 1,2-bis(2-tert-butylperoxypropan-2-yl)benzene Chemical compound CC(C)(C)OOC(C)(C)C1=CC=CC=C1C(C)(C)OOC(C)(C)C CCNDOQHYOIISTA-UHFFFAOYSA-N 0.000 claims description 3
- DMWVYCCGCQPJEA-UHFFFAOYSA-N 2,5-bis(tert-butylperoxy)-2,5-dimethylhexane Chemical compound CC(C)(C)OOC(C)(C)CCC(C)(C)OOC(C)(C)C DMWVYCCGCQPJEA-UHFFFAOYSA-N 0.000 claims description 3
- XMNIXWIUMCBBBL-UHFFFAOYSA-N 2-(2-phenylpropan-2-ylperoxy)propan-2-ylbenzene Chemical compound C=1C=CC=CC=1C(C)(C)OOC(C)(C)C1=CC=CC=C1 XMNIXWIUMCBBBL-UHFFFAOYSA-N 0.000 claims description 3
- NBOCQTNZUPTTEI-UHFFFAOYSA-N 4-[4-(hydrazinesulfonyl)phenoxy]benzenesulfonohydrazide Chemical compound C1=CC(S(=O)(=O)NN)=CC=C1OC1=CC=C(S(=O)(=O)NN)C=C1 NBOCQTNZUPTTEI-UHFFFAOYSA-N 0.000 claims description 3
- 229910000019 calcium carbonate Inorganic materials 0.000 claims description 3
- 239000006087 Silane Coupling Agent Substances 0.000 claims description 2
- XSKNCQXBPUYSJZ-UHFFFAOYSA-M [Cl-].C(CCCCCCCCCCC)OC[P+](CCCC)(CCCC)CCCC Chemical compound [Cl-].C(CCCCCCCCCCC)OC[P+](CCCC)(CCCC)CCCC XSKNCQXBPUYSJZ-UHFFFAOYSA-M 0.000 claims description 2
- AKUNSPZHHSNFFX-UHFFFAOYSA-M tributyl(tetradecyl)phosphanium;chloride Chemical compound [Cl-].CCCCCCCCCCCCCC[P+](CCCC)(CCCC)CCCC AKUNSPZHHSNFFX-UHFFFAOYSA-M 0.000 claims description 2
- 229920002554 vinyl polymer Polymers 0.000 claims description 2
- 239000013536 elastomeric material Substances 0.000 claims 1
- 241000894006 Bacteria Species 0.000 abstract description 5
- 230000000694 effects Effects 0.000 abstract description 3
- 239000013013 elastic material Substances 0.000 abstract description 3
- 239000011159 matrix material Substances 0.000 abstract description 2
- 239000005022 packaging material Substances 0.000 abstract description 2
- 239000003795 chemical substances by application Substances 0.000 abstract 1
- 238000013329 compounding Methods 0.000 abstract 1
- 239000005038 ethylene vinyl acetate Substances 0.000 description 24
- 238000010438 heat treatment Methods 0.000 description 9
- 230000000052 comparative effect Effects 0.000 description 8
- 239000011231 conductive filler Substances 0.000 description 7
- 230000003247 decreasing effect Effects 0.000 description 7
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 6
- 239000007864 aqueous solution Substances 0.000 description 6
- 230000001580 bacterial effect Effects 0.000 description 5
- 238000007599 discharging Methods 0.000 description 4
- 238000005303 weighing Methods 0.000 description 4
- 230000032683 aging Effects 0.000 description 3
- 238000001914 filtration Methods 0.000 description 3
- 239000006260 foam Substances 0.000 description 3
- 235000013305 food Nutrition 0.000 description 3
- 239000000843 powder Substances 0.000 description 3
- 239000000523 sample Substances 0.000 description 3
- 238000002444 silanisation Methods 0.000 description 3
- 230000035882 stress Effects 0.000 description 3
- 239000000725 suspension Substances 0.000 description 3
- 238000005406 washing Methods 0.000 description 3
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 3
- 239000002131 composite material Substances 0.000 description 2
- 239000008367 deionised water Substances 0.000 description 2
- 229910021641 deionized water Inorganic materials 0.000 description 2
- 238000002474 experimental method Methods 0.000 description 2
- 239000001963 growth medium Substances 0.000 description 2
- 239000007788 liquid Substances 0.000 description 2
- 239000011259 mixed solution Substances 0.000 description 2
- 239000007787 solid Substances 0.000 description 2
- ALGFAUZYOFDWGG-UHFFFAOYSA-N 4-hydroperoxy-4-methylpent-1-ene Chemical compound CC(C)(CC=C)OO ALGFAUZYOFDWGG-UHFFFAOYSA-N 0.000 description 1
- NAEUPYRMTNUJFQ-UHFFFAOYSA-N C(CCCCCCCCCCC)OP(CCCC)(CCCC)(CCCC)C Chemical compound C(CCCCCCCCCCC)OP(CCCC)(CCCC)(CCCC)C NAEUPYRMTNUJFQ-UHFFFAOYSA-N 0.000 description 1
- VEXZGXHMUGYJMC-UHFFFAOYSA-M Chloride anion Chemical compound [Cl-] VEXZGXHMUGYJMC-UHFFFAOYSA-M 0.000 description 1
- 229920000742 Cotton Polymers 0.000 description 1
- BLRPTPMANUNPDV-UHFFFAOYSA-N Silane Chemical compound [SiH4] BLRPTPMANUNPDV-UHFFFAOYSA-N 0.000 description 1
- 241001052560 Thallis Species 0.000 description 1
- 239000003242 anti bacterial agent Substances 0.000 description 1
- 239000002216 antistatic agent Substances 0.000 description 1
- 239000003899 bactericide agent Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 150000001767 cationic compounds Chemical class 0.000 description 1
- 125000002091 cationic group Chemical group 0.000 description 1
- 239000006258 conductive agent Substances 0.000 description 1
- 239000013068 control sample Substances 0.000 description 1
- 238000012258 culturing Methods 0.000 description 1
- GUJOJGAPFQRJSV-UHFFFAOYSA-N dialuminum;dioxosilane;oxygen(2-);hydrate Chemical compound O.[O-2].[O-2].[O-2].[Al+3].[Al+3].O=[Si]=O.O=[Si]=O.O=[Si]=O.O=[Si]=O GUJOJGAPFQRJSV-UHFFFAOYSA-N 0.000 description 1
- 238000007865 diluting Methods 0.000 description 1
- 239000006185 dispersion Substances 0.000 description 1
- 239000003814 drug Substances 0.000 description 1
- 230000005611 electricity Effects 0.000 description 1
- 239000003480 eluent Substances 0.000 description 1
- 238000007373 indentation Methods 0.000 description 1
- 238000005342 ion exchange Methods 0.000 description 1
- 238000009630 liquid culture Methods 0.000 description 1
- 230000007774 longterm Effects 0.000 description 1
- 231100000053 low toxicity Toxicity 0.000 description 1
- 238000012009 microbiological test Methods 0.000 description 1
- 244000005700 microbiome Species 0.000 description 1
- 229910052901 montmorillonite Inorganic materials 0.000 description 1
- 238000004806 packaging method and process Methods 0.000 description 1
- 239000002861 polymer material Substances 0.000 description 1
- 229910000077 silane Inorganic materials 0.000 description 1
- 238000001179 sorption measurement Methods 0.000 description 1
- 230000003068 static effect Effects 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 125000000999 tert-butyl group Chemical group [H]C([H])([H])C(*)(C([H])([H])[H])C([H])([H])[H] 0.000 description 1
- 238000010998 test method Methods 0.000 description 1
- 229920002725 thermoplastic elastomer Polymers 0.000 description 1
- PIDYNSSKPHJYEP-UHFFFAOYSA-N tributyl-chloro-tetradecyl-lambda5-phosphane Chemical compound C(CCC)P(Cl)(CCCCCCCCCCCCCC)(CCCC)CCCC PIDYNSSKPHJYEP-UHFFFAOYSA-N 0.000 description 1
- 125000000391 vinyl group Chemical group [H]C([*])=C([H])[H] 0.000 description 1
- 239000004636 vulcanized rubber Substances 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
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J9/00—Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof
- C08J9/04—Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof using blowing gases generated by a previously added blowing agent
- C08J9/06—Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof using blowing gases generated by a previously added blowing agent by a chemical blowing agent
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- C08J9/0023—Use of organic additives containing oxygen
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- C08J9/104—Hydrazines; Hydrazides; Semicarbazides; Semicarbazones; Hydrazones; Derivatives thereof
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- C08J2203/00—Foams characterized by the expanding agent
- C08J2203/04—N2 releasing, ex azodicarbonamide or nitroso compound
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- C08J2323/04—Homopolymers or copolymers of ethene
- C08J2323/08—Copolymers of ethene
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- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Health & Medical Sciences (AREA)
- Polymers & Plastics (AREA)
- Medicinal Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Organic Chemistry (AREA)
- General Chemical & Material Sciences (AREA)
- Emergency Medicine (AREA)
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- Manufacture Of Porous Articles, And Recovery And Treatment Of Waste Products (AREA)
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Abstract
The invention provides an antibacterial anti-static foamed elastomer material and a preparation method thereof, and belongs to the technical field of foamed elastic materials. The preparation method comprises the following steps: placing tin antimony oxide particles in a quaternary phosphonium salt solution to be adsorbed to saturation, and drying and grinding the washed tin antimony oxide particles to obtain quaternary phosphonium salt modified tin antimony oxide; modifying the quaternary phosphonium salt modified tin antimony oxide by using a coupling agent, and uniformly mixing the modified high-molecular blend, a foaming agent, a cross-linking agent and a modifying compounding agent to obtain a rubber compound; and (3) foaming, crosslinking and shaping the rubber compound to obtain the antibacterial and antistatic foamed elastomer material. The foamed elastomer prepared by the invention not only has antistatic property, but also has excellent antibacterial effect, and can effectively destroy bacteria in the EVA use environment; and secondly, the quaternary phosphonium salt doped tin antimony oxide can be uniformly dispersed in an EVA matrix after being modified by a coupling agent, has permanent antibacterial and antistatic effects, and can be used as products such as packaging materials, shoe materials and the like.
Description
Technical Field
The invention relates to the technical field of foamed elastic materials, in particular to an antibacterial and antistatic foamed elastic material and a preparation method thereof.
Background
In packaging or wearing materials in the industries of food, medicine, clothing and the like, antibacterial and antistatic properties are two very critical properties which are difficult to simultaneously possess. For example, foamed elastomers made of ethylene-vinyl acetate copolymer (EVA) are easy to cause bacteria on the surface or inside of EVA foam due to various microorganisms in the using environment, and the appearance and the using performance of the material are seriously influenced; and the EVA foaming material has no conductivity, and the surface of the EVA foaming material is easy to accumulate static electricity, so that the use is seriously influenced. The liquid antistatic agent added into the EVA foam or the antibacterial agent sprayed on the surface has poor dispersion and long-term effect; the common solid conductive agent usually adopts superconducting carbon black which cannot be used for light-colored EVA products, and the quaternary phosphonium salt modified tin antimony oxide can be used for preparing antibacterial, antistatic and light-colored high polymer materials. The quaternary phosphonium salt is a cationic bactericide, has the advantages of high efficiency, broad spectrum, low dosage, low toxicity, good chemical stability and the like, and is widely applied to the fields of medical treatment and health, water treatment, food industry, agriculture, daily life and the like; it can be added into EVA to make it have antibacterial effect. And the quaternary phosphonium salt serving as a cationic compound not only has certain antistatic property, but also can be intercalated into montmorillonite through ion exchange. If the composite material is compounded with conductive tin antimony oxide particles, and the composite material is mixed with EVA at high temperature, foamed and vulcanized, the quaternary phosphonium salt modified tin antimony oxide and the hybrid EVA foamed elastomer material with excellent antibacterial and antistatic effects can be obtained.
Disclosure of Invention
The invention aims at providing an antibacterial and antistatic foaming elastomer material with excellent antibacterial and antistatic capabilities, and aims at providing a preparation method of the material.
In order to achieve the aim, the invention provides a preparation method of an antibacterial and antistatic foaming elastomer material, which comprises the following steps:
step 1: placing tin antimony oxide particles in a quaternary phosphonium salt solution to be adsorbed to saturation, and drying and grinding the washed tin antimony oxide particles to obtain quaternary phosphonium salt modified tin antimony oxide;
step 2: modifying the quaternary phosphonium salt modified tin antimony oxide by using a coupling agent, and uniformly mixing the modified high polymer blend, a cross-linking agent, a reinforcing agent, a foaming agent and a co-foaming agent to obtain a rubber compound;
and step 3: and (3) foaming, crosslinking and shaping the rubber compound to obtain the antibacterial and antistatic foamed elastomer material.
Preferably, in the step 1, the quaternary phosphonium salt solution is one of dodecyloxymethyltributyl phosphonium chloride/polyvinyl alcohol solution, tetradecyltributyl phosphonium chloride/polyvinyl alcohol solution, and polyquaternary phosphonium salt/polyvinyl alcohol solution; the concentration of the quaternary phosphonium salt solution is 4-6 mg/mL.
Preferably, in the step 1 and the step 2, the coupling agent is one of a vinyl tri-tert-butyl peroxide silane coupling agent, a titanate coupling agent and an aluminate coupling agent; according to the mass ratio, the ratio of the quaternary phosphonium salt modified tin antimony oxide to the coupling agent is 10: 1.
Preferably, in the step 1 and the step 2, the temperature of the modification is 60 ℃, and the time of the modification is 4 h.
Preferably, in the step 2, the modified polymer blend is one of a blend of EVA-20% and EVM-40%, a blend of EVA-20%, natural rubber and styrene-butadiene rubber, and a blend of EVA-20% and High Density Polyethylene (HDPE); according to the mass ratio, the quaternary phosphonium salt modified tin antimony oxide is obtained, wherein the ratio of the modified polymer blend to the quaternary phosphonium salt modified tin antimony oxide is 3: 20; according to the mass ratio, the EVA is-20%: EVA-40% is 9: 1; according to the mass ratio, the EVA is-20%: natural rubber: the ratio of styrene butadiene rubber is 8:1: 1; according to the mass ratio, the EVA accounts for-20% and the high-density polyethylene accounts for 8: 2.
Preferably, in the step 2, the crosslinking agent is one of dicumyl peroxide, 2, 5-dimethyl-2, 5-di (tert-butylperoxy) hexane and di (tert-butylperoxyisopropyl) benzene; the reinforcing agent is one of white carbon black and calcium carbonate; the foaming agent is one of Azodicarbonamide (AC) and 4,4' -oxo-bis-benzenesulfonyl hydrazide (OBSH); the assistant foaming agent is zinc oxide and stearic acid; the quaternary phosphonium salt modified tin antimony oxide comprises the following components in percentage by mass: the cross-linking agent: the reinforcing agent comprises the foaming agent: the auxiliary foaming agent is 15:2:10:4: 2.
Preferably, in the step 3, the foaming and vulcanizing conditions are 180 ℃ and 10 min. .
In addition, the invention provides an antibacterial and antistatic foamed elastomer material, which is prepared by the preparation method.
The invention has the beneficial effects that:
1. the foamed elastomer prepared by the invention not only has antistatic property, but also has excellent antibacterial effect, and can effectively destroy bacteria in the EVA use environment.
2. The quaternary phosphonium salt doped tin antimony oxide can be uniformly dispersed in an EVA matrix after being modified by a coupling agent, and has permanent antibacterial and antistatic effects, so that the quaternary phosphonium salt doped tin antimony oxide can be used as products such as packaging materials, shoe materials and the like.
Detailed Description
In order to clearly illustrate the technical features of the present solution, the present solution is explained below by way of specific embodiments. However, the embodiment of the present invention is not limited thereto, and conventional conditions are referred to for parameters not particularly mentioned.
Example 1
The embodiment of the invention provides an antibacterial quaternary phosphonium salt modified tin antimony oxide conductive filler and a preparation method of a hybrid EVA foamed elastomer thereof. Which comprises the following steps:
(1) weighing 15g of nano tin antimony oxide, heating at 60 ℃ for 4h, drying, and grinding to obtain tin antimony oxide powder (the average particle size is 0.05 mu m);
(2) preparing 100g of dodecyloxy methyl tributyl phosphorus chloride and 0.15g of polyvinyl alcohol into an aqueous solution with the quaternary phosphonium salt concentration of 4mg/mL, placing tin antimony oxide in the aqueous solution for adsorption until saturation (the quaternary phosphonium salt is kept excessive), filtering, heating at 60 ℃ for 4h for drying, and grinding to obtain the quaternary phosphonium salt modified tin antimony oxide conductive filler;
(3) then adding a solution of 1.5g of vinyl tert-butyl hydroperoxide and 30g of ethanol (the mass ratio of silane to quaternary phosphonium salt modified tin antimony oxide is 0.1), and heating for 3h at 60 ℃;
(4) sequentially adding and uniformly mixing EVA90g, EVM10g, silanized quaternary phosphonium salt modified tin antimony oxide 15g, white carbon black 10g, zinc oxide 1g, stearic acid 1g, AC 4g and dicumyl peroxide 2g in an internal mixer, removing rubber, discharging tablets and ageing for 8 hours;
(5) foaming and vulcanizing at 180 ℃ for 10min by using a foaming mold to obtain the antibacterial and antistatic foaming elastomer based on the quaternary phosphonium salt modified tin antimony oxide hybrid EVA.
Example 2
The embodiment of the invention provides an antibacterial quaternary phosphonium salt modified tin antimony oxide conductive filler and a preparation method of a hybrid EVA foamed elastomer thereof. Which comprises the following steps:
(1) weighing 15g of nano tin antimony oxide, heating at 60 ℃ for 4h, drying, and grinding to obtain tin antimony oxide powder;
(2) weighing 100g of tetradecyl tributyl phosphorus chloride and 0.25g of polyvinyl alcohol to prepare an aqueous solution with the quaternary phosphonium salt concentration of 4mg/mL, placing tin antimony oxide in the aqueous solution to be adsorbed until saturation (the quaternary phosphonium salt is kept excessive), fully washing the tin antimony oxide with deionized water after filtering, heating the mixture at 60 ℃ for 4 hours to dry the mixture, and grinding the mixture to obtain the quaternary phosphonium salt modified tin antimony oxide conductive filler;
(3) then adding a mixed solution of 1.5g of titanate coupling agent and 30g of ethanol (the mass ratio of titanate to quaternary phosphonium salt modified tin antimony oxide is 0.1), and heating for 3h at 60 ℃;
(4) adding and mixing uniformly in an internal mixer according to the proportion of 80g of EVA, 10g of natural rubber, 10g of styrene butadiene rubber, 15g of titanate/quaternary phosphonium salt modified tin antimony oxide, 10g of white carbon black, 1g of zinc oxide, 1g of stearic acid, 4g of OBSH and 2g of 2, 5-dimethyl-2, 5-di (tert-butylperoxy) hexane in turn, removing rubber, discharging pieces and then aging for 8 hours;
(5) foaming and vulcanizing at 180 ℃ for 10min by using a foaming mold to obtain the antibacterial and antistatic foaming elastomer based on the quaternary phosphonium salt modified tin antimony oxide hybrid EVA.
Example 3
The embodiment of the invention provides an antibacterial quaternary phosphonium salt modified tin antimony oxide conductive filler and a preparation method of a hybrid EVA foamed elastomer thereof. Which comprises the following steps:
(1) weighing 15g of nano tin antimony oxide, heating at 60 ℃ for 4h, drying, and grinding to obtain tin antimony oxide powder;
(2) preparing an aqueous solution with the concentration of the polyquaternary phosphonium salt being 6mg/mL according to the mass ratio of the polyquaternary phosphonium salt/polyvinyl alcohol =100/0.45, placing tin antimony oxide in the aqueous solution to be adsorbed to saturation (the quaternary phosphonium salt is kept excessive), fully washing the obtained product with deionized water after filtering, heating the obtained product at 60 ℃ for 4h to dry the obtained product, and grinding the obtained product to obtain the polyquaternary phosphonium salt modified tin antimony oxide conductive filler;
(3) then adding a mixed solution of aluminate coupling agent/ethanol =5/100 (the mass ratio of aluminate to quaternary phosphonium salt modified tin antimony oxide is 0.1), and heating at 60 ℃ for 3 h;
(4) adding 80g of EVA, 20g of HDPE, 15g of aluminate/polyquaternary phosphonium salt modified tin antimony oxide, 10g of calcium carbonate, 1g of zinc oxide, 1g of stearic acid, 4g of AC and 2g of di (tert-butyl peroxyisopropyl) benzene in an internal mixer in sequence, uniformly mixing, discharging rubber, discharging slices and then aging for 8 hours;
(5) foaming and vulcanizing at 180 ℃ for 10min by using a foaming mold to obtain the antibacterial and antistatic foaming elastomer based on the polyquaternary phosphonium salt modified tin antimony oxide hybrid EVA.
Comparative example 1
This material differs from example 1 only in that: the dosage of the silanization quaternary phosphonium salt modified tin antimony oxide in the step (4) is 10 parts.
Comparative example 2
This material differs from example 1 only in that: the dosage of the silanization quaternary phosphonium salt modified tin antimony oxide in the step (4) is 5 parts.
Comparative example 3
This material differs from example 1 only in that: the dosage of the silanization quaternary phosphonium salt modified tin antimony oxide in the step (4) is 0 part.
Experimental methods
1. The antistatic property, the antibacterial property and the mechanical property of example 1, comparative example 2 and comparative example 3 were measured, respectively. The volume resistivity is tested according to GBT 1410-. When the antibacterial performance is tested, firstly preparing bacterial suspension with a certain bacterial liquid concentration (the number of thalli is 103 cfu/mL); then respectively taking a proper amount of bacterial suspension to soak a control sample (a sterilized flat plate with the diameter of 90 mm) and a sterilized sample to be tested (50 mm multiplied by 2 mm), and culturing for 24 hours under the condition that the relative humidity is more than 90% at 37 ℃; taking out the cultured sample, wiping redundant bacterial suspension with a sterilized cotton swab, repeatedly washing the film with 10ml of eluent into a sterilized plate, fully shaking up, and diluting by 10-1, 10-2 and 10-3 times with a liquid culture medium; then a certain amount of the bacteria are inoculated in a solid culture medium, after the bacteria are cultured for 24 hours at 37 ℃, the viable count is determined according to GB/T4789.2-2016 method for determining the total number of the bacterial colonies in the microbiological test of food hygiene. The final formula for calculating the bacteriostasis rate is as follows: bacteriostasis rate = (number of control colonies-number of test sample colonies)/number of control colonies × 100%. Apparent density was tested according to GB/T6343-1995, determination of the apparent density of foams and rubbers. The Shore C type hardness is tested according to GB/T531-2009 test method for indentation hardness of vulcanized rubber or thermoplastic rubber; the tensile strength, the elongation and the stress at definite elongation are tested according to GB/T528-; the ball drop rebound is tested according to GB/T6670-; the results are shown in Table 1.
Table 1 antistatic, antibacterial and mechanical properties of the hybrid materials of example 1 and comparative examples 1, 2, 3
Example 1 and comparative examples 1 and 2, which contain 4, 6 and 8 parts of foaming agent, respectively, have sequentially decreased mass density, increased resistivity, decreased antibacterial properties, decreased strength, elongation, stress at definite elongation and hardness, and increased elasticity. Example 1 contains 15, 10, 5 parts of conductive filler, respectively, and has successively decreased mass density, increased resistivity, decreased antibacterial property, decreased strength, increased elongation and stress at definite elongation, decreased hardness, and increased elasticity, as compared with comparative examples 3 and 4. The five samples all meet the requirements of antistatic and antibacterial properties, and have good mechanical properties.
2. The antistatic property, the antibacterial property and the mechanical property of example 2 and example 3 were measured. The experimental method is as above. The results are shown in Table 2.
Table 2 antistatic, antibacterial and mechanical properties of the hybrid materials of example 2 and example 3
Compared with the common EVA foaming elastomer (the volume resistivity is more than 1012 omega cm, and the antibacterial activity is not generated), the antistatic and antibacterial performance requirements are met in the example 3 (containing 15 parts of tetradecyl tributyl phosphorus chloride modified tin antimony oxide) and the example 4 (containing 15 parts of polyquaternary phosphonium salt modified tin antimony oxide), and the mechanical performance is better.
Claims (8)
1. The preparation method of the antibacterial anti-static foamed elastomer material is characterized by comprising the following steps:
step 1: placing tin antimony oxide particles in a quaternary phosphonium salt solution to be adsorbed to saturation, and drying and grinding the washed tin antimony oxide particles to obtain quaternary phosphonium salt modified tin antimony oxide;
step 2: modifying the quaternary phosphonium salt modified tin antimony oxide by using a coupling agent, and uniformly mixing the modified high polymer blend, a cross-linking agent, a reinforcing agent, a foaming agent and a co-foaming agent to obtain a rubber compound;
and step 3: and (3) foaming, crosslinking and shaping the rubber compound to obtain the antibacterial and antistatic foamed elastomer material.
2. The method of claim 1, wherein in step 1, the quaternary phosphonium salt solution is one of dodecyloxymethyltributyl phosphonium chloride/polyvinyl alcohol solution, tetradecyltributyl phosphonium chloride/polyvinyl alcohol solution, and polyquaternary phosphonium salt/polyvinyl alcohol solution; the concentration of the quaternary phosphonium salt solution is 4-6 mg/mL.
3. The preparation method according to claim 1, wherein in the step 2, the coupling agent is one of vinyl t-butyl hydroperoxide silane coupling agent, titanate coupling agent and aluminate coupling agent; according to the mass ratio, the ratio of the quaternary phosphonium salt modified tin antimony oxide to the coupling agent is 10: 1.
4. The method according to claim 1, wherein the temperature of the modification in step 2 is 60 ℃ and the time of the modification is 4 hours.
5. The preparation method according to claim 1, wherein in the step 2, the modified polymer blend is one of a blend of EVA-20% and EVM-40%, a blend of EVA-20%, natural rubber and styrene-butadiene rubber, and a blend of EVA-20% and High Density Polyethylene (HDPE); according to the mass ratio, the quaternary phosphonium salt modified tin antimony oxide is obtained, wherein the ratio of the modified polymer blend to the quaternary phosphonium salt modified tin antimony oxide is 3: 20; according to the mass ratio, the EVA is-20%: EVA-40% is 9: 1; according to the mass ratio, the EVA is-20%: natural rubber: the ratio of styrene butadiene rubber is 8:1: 1; according to the mass ratio, the EVA accounts for-20% and the high-density polyethylene accounts for 8: 2.
6. The method according to claim 1, wherein in the step 2, the crosslinking agent is one of dicumyl peroxide, 2, 5-dimethyl-2, 5-di (t-butylperoxy) hexane, and di (t-butylperoxyisopropyl) benzene; the reinforcing agent is one of white carbon black and calcium carbonate; the foaming agent is one of Azodicarbonamide (AC) and 4,4' -oxo-bis-benzenesulfonyl hydrazide (OBSH); the assistant foaming agent is zinc oxide and stearic acid; the quaternary phosphonium salt modified tin antimony oxide comprises the following components in percentage by mass: the cross-linking agent: the reinforcing agent comprises the foaming agent: the auxiliary foaming agent is 15:2:10:4: 2.
7. The preparation method according to claim 1, wherein in the step 3, the foaming and vulcanizing conditions are 180 ℃ and 10 min.
8. An antibacterial antistatic foamed elastomeric material, characterized in that it is obtained by the process according to any one of claims 1 to 8.
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