CN103773308A - Long-acting antibacterial and mildew-proof silicone adhesive and preparation method thereof - Google Patents
Long-acting antibacterial and mildew-proof silicone adhesive and preparation method thereof Download PDFInfo
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- CN103773308A CN103773308A CN201310728002.8A CN201310728002A CN103773308A CN 103773308 A CN103773308 A CN 103773308A CN 201310728002 A CN201310728002 A CN 201310728002A CN 103773308 A CN103773308 A CN 103773308A
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- Prior art keywords
- mildew
- silicone adhesive
- antibacterial
- preparation
- agent
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- 239000013464 silicone adhesive Substances 0.000 title claims abstract description 70
- 230000000844 anti-bacterial effect Effects 0.000 title claims abstract description 46
- 238000002360 preparation method Methods 0.000 title claims abstract description 40
- 229910021536 Zeolite Inorganic materials 0.000 claims abstract description 40
- HNPSIPDUKPIQMN-UHFFFAOYSA-N dioxosilane;oxo(oxoalumanyloxy)alumane Chemical compound O=[Si]=O.O=[Al]O[Al]=O HNPSIPDUKPIQMN-UHFFFAOYSA-N 0.000 claims abstract description 40
- 239000010457 zeolite Substances 0.000 claims abstract description 40
- HCHKCACWOHOZIP-UHFFFAOYSA-N Zinc Chemical compound [Zn] HCHKCACWOHOZIP-UHFFFAOYSA-N 0.000 claims abstract description 39
- 229910052725 zinc Inorganic materials 0.000 claims abstract description 39
- 239000011701 zinc Substances 0.000 claims abstract description 39
- 239000000463 material Substances 0.000 claims abstract description 36
- 239000007822 coupling agent Substances 0.000 claims abstract description 32
- 239000002131 composite material Substances 0.000 claims abstract description 24
- 239000003795 chemical substances by application Substances 0.000 claims abstract description 19
- 238000000227 grinding Methods 0.000 claims abstract description 8
- 230000003115 biocidal effect Effects 0.000 claims description 68
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 43
- 238000003756 stirring Methods 0.000 claims description 37
- 239000003112 inhibitor Substances 0.000 claims description 33
- 239000003139 biocide Substances 0.000 claims description 25
- -1 methyl isopropyl Chemical group 0.000 claims description 23
- 230000000845 anti-microbial effect Effects 0.000 claims description 22
- 239000003292 glue Substances 0.000 claims description 21
- 235000013870 dimethyl polysiloxane Nutrition 0.000 claims description 18
- 229960004756 ethanol Drugs 0.000 claims description 18
- 229920000435 poly(dimethylsiloxane) Polymers 0.000 claims description 18
- WYVVKGNFXHOCQV-UHFFFAOYSA-N 3-iodoprop-2-yn-1-yl butylcarbamate Chemical compound CCCCNC(=O)OCC#CI WYVVKGNFXHOCQV-UHFFFAOYSA-N 0.000 claims description 17
- 229940043810 zinc pyrithione Drugs 0.000 claims description 17
- PICXIOQBANWBIZ-UHFFFAOYSA-N zinc;1-oxidopyridine-2-thione Chemical compound [Zn+2].[O-]N1C=CC=CC1=S.[O-]N1C=CC=CC1=S PICXIOQBANWBIZ-UHFFFAOYSA-N 0.000 claims description 17
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 claims description 16
- 230000002421 anti-septic effect Effects 0.000 claims description 16
- 238000000034 method Methods 0.000 claims description 14
- 241000894006 Bacteria Species 0.000 claims description 13
- UHOVQNZJYSORNB-UHFFFAOYSA-N Benzene Chemical compound C1=CC=CC=C1 UHOVQNZJYSORNB-UHFFFAOYSA-N 0.000 claims description 12
- 239000004205 dimethyl polysiloxane Substances 0.000 claims description 12
- PORQOHRXAJJKGK-UHFFFAOYSA-N 4,5-dichloro-2-n-octyl-3(2H)-isothiazolone Chemical compound CCCCCCCCN1SC(Cl)=C(Cl)C1=O PORQOHRXAJJKGK-UHFFFAOYSA-N 0.000 claims description 11
- 239000004902 Softening Agent Substances 0.000 claims description 10
- BLRPTPMANUNPDV-UHFFFAOYSA-N Silane Chemical compound [SiH4] BLRPTPMANUNPDV-UHFFFAOYSA-N 0.000 claims description 9
- TWFZGCMQGLPBSX-UHFFFAOYSA-N carbendazim Chemical compound C1=CC=C2NC(NC(=O)OC)=NC2=C1 TWFZGCMQGLPBSX-UHFFFAOYSA-N 0.000 claims description 9
- 238000001125 extrusion Methods 0.000 claims description 9
- 239000000945 filler Substances 0.000 claims description 9
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 8
- CRQQGFGUEAVUIL-UHFFFAOYSA-N chlorothalonil Chemical compound ClC1=C(Cl)C(C#N)=C(Cl)C(C#N)=C1Cl CRQQGFGUEAVUIL-UHFFFAOYSA-N 0.000 claims description 7
- 229960000935 dehydrated alcohol Drugs 0.000 claims description 7
- SKZKKFZAGNVIMN-UHFFFAOYSA-N Salicilamide Chemical compound NC(=O)C1=CC=CC=C1O SKZKKFZAGNVIMN-UHFFFAOYSA-N 0.000 claims description 6
- VTYYLEPIZMXCLO-UHFFFAOYSA-L calcium carbonate Substances [Ca+2].[O-]C([O-])=O VTYYLEPIZMXCLO-UHFFFAOYSA-L 0.000 claims description 6
- 235000021355 Stearic acid Nutrition 0.000 claims description 5
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 claims description 5
- YRKCREAYFQTBPV-UHFFFAOYSA-N acetylacetone Natural products CC(=O)CC(C)=O YRKCREAYFQTBPV-UHFFFAOYSA-N 0.000 claims description 5
- BFXIKLCIZHOAAZ-UHFFFAOYSA-N methyltrimethoxysilane Chemical compound CO[Si](C)(OC)OC BFXIKLCIZHOAAZ-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
- 241000191967 Staphylococcus aureus Species 0.000 claims description 4
- TVJPBVNWVPUZBM-UHFFFAOYSA-N [diacetyloxy(methyl)silyl] acetate Chemical compound CC(=O)O[Si](C)(OC(C)=O)OC(C)=O TVJPBVNWVPUZBM-UHFFFAOYSA-N 0.000 claims description 4
- 239000002253 acid Substances 0.000 claims description 4
- 229910000019 calcium carbonate Inorganic materials 0.000 claims description 4
- 230000000968 intestinal effect Effects 0.000 claims description 4
- 125000002496 methyl group Chemical group [H]C([H])([H])* 0.000 claims description 4
- 238000002156 mixing Methods 0.000 claims description 4
- 241000228245 Aspergillus niger Species 0.000 claims description 3
- 239000004593 Epoxy Substances 0.000 claims description 3
- 150000001336 alkenes Chemical class 0.000 claims description 3
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims description 3
- 230000002045 lasting effect Effects 0.000 claims description 3
- 239000001301 oxygen Substances 0.000 claims description 3
- 229910052760 oxygen Inorganic materials 0.000 claims description 3
- 125000001436 propyl group Chemical group [H]C([*])([H])C([H])([H])C([H])([H])[H] 0.000 claims description 3
- 229910000077 silane Inorganic materials 0.000 claims description 3
- 239000000377 silicon dioxide Substances 0.000 claims description 3
- LFQCEHFDDXELDD-UHFFFAOYSA-N tetramethyl orthosilicate Chemical compound CO[Si](OC)(OC)OC LFQCEHFDDXELDD-UHFFFAOYSA-N 0.000 claims description 3
- 239000010936 titanium Substances 0.000 claims description 3
- 229910052719 titanium Inorganic materials 0.000 claims description 3
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 claims 4
- 229910052710 silicon Inorganic materials 0.000 claims 1
- 239000010703 silicon Substances 0.000 claims 1
- 238000004519 manufacturing process Methods 0.000 abstract description 25
- 239000003242 anti bacterial agent Substances 0.000 abstract description 8
- 230000001954 sterilising effect Effects 0.000 abstract description 4
- 239000002699 waste material Substances 0.000 abstract description 4
- 239000000853 adhesive Substances 0.000 abstract description 2
- 230000001070 adhesive effect Effects 0.000 abstract description 2
- 239000002994 raw material Substances 0.000 abstract description 2
- 230000000694 effects Effects 0.000 description 18
- 239000000047 product Substances 0.000 description 18
- DMSMPAJRVJJAGA-UHFFFAOYSA-N benzo[d]isothiazol-3-one Chemical class C1=CC=C2C(=O)NSC2=C1 DMSMPAJRVJJAGA-UHFFFAOYSA-N 0.000 description 11
- 208000001840 Dandruff Diseases 0.000 description 9
- 239000011248 coating agent Substances 0.000 description 8
- 238000000576 coating method Methods 0.000 description 8
- 239000006185 dispersion Substances 0.000 description 8
- 244000005700 microbiome Species 0.000 description 8
- 239000003973 paint Substances 0.000 description 8
- 239000000126 substance Substances 0.000 description 8
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 8
- 241000233866 Fungi Species 0.000 description 7
- 150000001298 alcohols Chemical class 0.000 description 7
- 230000005764 inhibitory process Effects 0.000 description 6
- 239000004033 plastic Substances 0.000 description 6
- 229920003023 plastic Polymers 0.000 description 6
- 238000012360 testing method Methods 0.000 description 6
- 239000010985 leather Substances 0.000 description 5
- 239000000203 mixture Substances 0.000 description 5
- 230000008859 change Effects 0.000 description 4
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- 230000000855 fungicidal effect Effects 0.000 description 4
- 230000008569 process Effects 0.000 description 4
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- 239000000565 sealant Substances 0.000 description 4
- 238000001228 spectrum Methods 0.000 description 4
- 239000004698 Polyethylene Substances 0.000 description 3
- 230000000843 anti-fungal effect Effects 0.000 description 3
- 229940121375 antifungal agent Drugs 0.000 description 3
- 230000033228 biological regulation Effects 0.000 description 3
- LDCRTTXIJACKKU-ONEGZZNKSA-N dimethyl fumarate Chemical group COC(=O)\C=C\C(=O)OC LDCRTTXIJACKKU-ONEGZZNKSA-N 0.000 description 3
- 229960004419 dimethyl fumarate Drugs 0.000 description 3
- 238000005516 engineering process Methods 0.000 description 3
- 238000011156 evaluation Methods 0.000 description 3
- 150000002500 ions Chemical class 0.000 description 3
- MGIYRDNGCNKGJU-UHFFFAOYSA-N isothiazolinone Chemical compound O=C1C=CSN1 MGIYRDNGCNKGJU-UHFFFAOYSA-N 0.000 description 3
- 230000002147 killing effect Effects 0.000 description 3
- 231100000053 low toxicity Toxicity 0.000 description 3
- 229920000573 polyethylene Polymers 0.000 description 3
- 230000002829 reductive effect Effects 0.000 description 3
- 241000195493 Cryptophyta Species 0.000 description 2
- 239000004743 Polypropylene Substances 0.000 description 2
- NHTFLYKPEGXOAN-UHFFFAOYSA-N Trichlamide Chemical compound CCCCOC(C(Cl)(Cl)Cl)NC(=O)C1=CC=CC=C1O NHTFLYKPEGXOAN-UHFFFAOYSA-N 0.000 description 2
- 125000002252 acyl group Chemical group 0.000 description 2
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- 238000003556 assay Methods 0.000 description 2
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- 229910052751 metal Inorganic materials 0.000 description 2
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- 230000000813 microbial effect Effects 0.000 description 2
- 230000007935 neutral effect Effects 0.000 description 2
- 230000003287 optical effect Effects 0.000 description 2
- 229920001155 polypropylene Polymers 0.000 description 2
- 229920001296 polysiloxane Polymers 0.000 description 2
- 239000004814 polyurethane Substances 0.000 description 2
- 239000003755 preservative agent Substances 0.000 description 2
- 238000011160 research Methods 0.000 description 2
- 238000007789 sealing Methods 0.000 description 2
- 150000004756 silanes Chemical class 0.000 description 2
- 239000004590 silicone sealant Substances 0.000 description 2
- 229910052709 silver Inorganic materials 0.000 description 2
- 239000004332 silver Substances 0.000 description 2
- 238000004659 sterilization and disinfection Methods 0.000 description 2
- 201000004384 Alopecia Diseases 0.000 description 1
- 241000235349 Ascomycota Species 0.000 description 1
- 241000228212 Aspergillus Species 0.000 description 1
- 241000223678 Aureobasidium pullulans Species 0.000 description 1
- 241000193830 Bacillus <bacterium> Species 0.000 description 1
- 229940123208 Biguanide Drugs 0.000 description 1
- 244000025254 Cannabis sativa Species 0.000 description 1
- 241000675108 Citrus tangerina Species 0.000 description 1
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 1
- 201000004624 Dermatitis Diseases 0.000 description 1
- JOYRKODLDBILNP-UHFFFAOYSA-N Ethyl urethane Chemical compound CCOC(N)=O JOYRKODLDBILNP-UHFFFAOYSA-N 0.000 description 1
- 208000031888 Mycoses Diseases 0.000 description 1
- BPQQTUXANYXVAA-UHFFFAOYSA-N Orthosilicate Chemical compound [O-][Si]([O-])([O-])[O-] BPQQTUXANYXVAA-UHFFFAOYSA-N 0.000 description 1
- 241001236817 Paecilomyces <Clavicipitaceae> Species 0.000 description 1
- 241000228143 Penicillium Species 0.000 description 1
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 description 1
- 241001136494 Talaromyces funiculosus Species 0.000 description 1
- ATJFFYVFTNAWJD-UHFFFAOYSA-N Tin Chemical compound [Sn] ATJFFYVFTNAWJD-UHFFFAOYSA-N 0.000 description 1
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 description 1
- ISKQADXMHQSTHK-UHFFFAOYSA-N [4-(aminomethyl)phenyl]methanamine Chemical compound NCC1=CC=C(CN)C=C1 ISKQADXMHQSTHK-UHFFFAOYSA-N 0.000 description 1
- JJLKTTCRRLHVGL-UHFFFAOYSA-L [acetyloxy(dibutyl)stannyl] acetate Chemical class CC([O-])=O.CC([O-])=O.CCCC[Sn+2]CCCC JJLKTTCRRLHVGL-UHFFFAOYSA-L 0.000 description 1
- UKLDJPRMSDWDSL-UHFFFAOYSA-L [dibutyl(dodecanoyloxy)stannyl] dodecanoate Chemical compound CCCCCCCCCCCC(=O)O[Sn](CCCC)(CCCC)OC(=O)CCCCCCCCCCC UKLDJPRMSDWDSL-UHFFFAOYSA-L 0.000 description 1
- 230000001154 acute effect Effects 0.000 description 1
- 239000000654 additive Substances 0.000 description 1
- 230000000996 additive effect Effects 0.000 description 1
- 239000002390 adhesive tape Substances 0.000 description 1
- 239000003905 agrochemical Substances 0.000 description 1
- 230000000172 allergic effect Effects 0.000 description 1
- 231100000360 alopecia Toxicity 0.000 description 1
- 230000001857 anti-mycotic effect Effects 0.000 description 1
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- 229940064004 antiseptic throat preparations Drugs 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 150000004283 biguanides Chemical class 0.000 description 1
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- 238000005520 cutting process Methods 0.000 description 1
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- AYOHIQLKSOJJQH-UHFFFAOYSA-N dibutyltin Chemical compound CCCC[Sn]CCCC AYOHIQLKSOJJQH-UHFFFAOYSA-N 0.000 description 1
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- 239000001257 hydrogen Substances 0.000 description 1
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- OGIDPMRJRNCKJF-UHFFFAOYSA-N titanium oxide Inorganic materials [Ti]=O OGIDPMRJRNCKJF-UHFFFAOYSA-N 0.000 description 1
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- 125000000391 vinyl group Chemical group [H]C([*])=C([H])[H] 0.000 description 1
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- 150000003751 zinc Chemical class 0.000 description 1
- 229910000166 zirconium phosphate Inorganic materials 0.000 description 1
- LEHFSLREWWMLPU-UHFFFAOYSA-B zirconium(4+);tetraphosphate Chemical compound [Zr+4].[Zr+4].[Zr+4].[O-]P([O-])([O-])=O.[O-]P([O-])([O-])=O.[O-]P([O-])([O-])=O.[O-]P([O-])([O-])=O LEHFSLREWWMLPU-UHFFFAOYSA-B 0.000 description 1
Landscapes
- Agricultural Chemicals And Associated Chemicals (AREA)
Abstract
The invention relates to a long-acting antibacterial and mildew-proof silicone adhesive and a preparation method thereof. The preparation method comprises the steps: grinding an efficient and environment-friendly organic sterilizing and mildew-proof agent and an inorganic zinc loaded zeolite antibacterial agent with a porous structure at high speed in high-speed grinding equipment and thus organically combining the organic sterilizing and mildew-proof agent and the inorganic zinc loaded zeolite antibacterial agent by using a coupling agent on the basis of comprehensively researching and analyzing the characteristics of all antibacterial and mildew-proof agent systems to obtain a novel composite antibacterial and mildew-proof agent; then, adding the obtained composite antibacterial and mildew-proof agent into a silicone adhesive material by using the traditional silicone adhesive production equipment and a conventional adhesive preparation process to finish the preparation of the long-acting antibacterial and mildew-proof silicone adhesive. The antibacterial and mildew-proof silicone adhesive provided by the invention is low in raw material cost, simple in production process, free of three wastes and capable of meeting the requirement for environment friendliness. The long-acting antibacterial and mildew-proof silicone adhesive prepared by the invention is efficient and durable in antibacterial and mildew-proof performances and capable of meeting the technical requirement for use in fields such as buildings, electronic appliances, automobiles, boats and the like.
Description
Technical field
The present invention relates to seal gum field.More specifically, the present invention relates to a kind of silicone adhesive with long acting antibiotic antimildew function, also relates to the preparation method of described antibacterial and mouldproof silicone adhesive.
Background technology
Single-component room-temperature vulcanized (RTV-1) silicone adhesive is with its excellent ageing-resistant performance, good elasticity, outstanding water resistance, be widely used in the waterproof sealing of seam between the sanitary ware of kitchen, bathroom, toilet and table top, body of wall, furniture, and consumption is increasing.But because these occasions are throughout the year moister, silicone adhesive is easy to be subject to the infringement of the microorganism such as bacterium, mould, cause that adhesive tape is mouldy, variable color, come off, lose water-tight function, also can infect various diseases if these unwanted bacterias contact with human body, threaten the mankind's health time property and electrical insulating property etc.For above problem, scientific worker has prepared mildew-resistant organosilicon sealant by adding some mould inhibitors, and the performance corroding to improve its antifungal, increases the service life.Antibacterial and mouldproof mould inhibitor available on Vehicles Collected from Market mainly contains two classes: (1) mineral-type, and as metal (silver, copper, zinc, tin, rare earth etc.) inorganic salt etc., nano titanium oxide, nano zine oxide, nanometer silver etc.Its remarkable advantage is that high security, slow-releasing are good, broad spectrum antibacterial, be difficult for developing immunity to drugs, good heat resistance and easy to process, therefore its application and research is more and more subject to people's attention.Wherein outstanding with silver-series antibacterial agent performance, but its exist cost high, easy to change, to mould and the problem such as alga microbial inhibition is poor.With regard to silicone adhesive, when take antifungal and algae as main, so pure inorganic antiseptic has its limitation.(2) organic, as quaternary ammonium salt, biguanides, alcohols, phenols, organo-metallic class, pyridines, imidazoles, isothiazolinone and BIT class etc.Such antiseptic-germicide fungicidal spectrum is wide, speed is fast, but often has poor heat resistance, easily decomposes and the shortcoming such as work-ing life is short, and what have also has the stronger side effect such as toxicity and environmental pollution.
In recent years, as follows about the main report of antibacterial and mouldproof silicone adhesive preparation research:
CN10129855B has announced a kind of nanometer mildewproof sealing neutral silicone resin, and its effective mould inhibitor composition is nano-Ag particles, exists cost high, easy to change, to the shortcoming a little less than mould inhibition.
CN103130442A has announced a kind of material of construction mildewproof additive, its main component is dimethyl fumarate, this component is with low cost, fungicidal properties is good, but from October, 2008, European Union aspect has just been circulated a notice of a lot of because human consumer contacts the case that the footwear, the leather sofa etc. that contain dimethyl fumarate produce allergic, acute eczema and burn successively, makes it be subject to extensive concern.On January 29th, 2009, EU member country passed through draft resolution, the product that " contained dimethyl fumarate " from 1 day May in 2009, and it will be prohibited from entering EU market circulation and sell.
CN102485823A has announced a kind of mildew-resistant organosilicon sealant, and this patent of invention mould inhibitor used is 2n acyl group isothiazolinone and BIT (BIT), describes inaccurate through its component of great mass of data retrieval discovery 2n acyl group isothiazolinone.It is said this invention mildewproof sealant anti-mold effect excellence, but the often too fast material surface that migrates to of pure organic mould inhibitor easily causes loss, therefore affect material mildew-resistant endurance quality.
CN102604586A has announced a kind of production method of double glazing mildew-resistant silicone sealant, in its production process, do not add mildew-resistant composition, it is said that it is never mouldy in moist place, but actually operating is not necessarily so, the siloxanes organism containing in its component is easy to become the nutritive substance of microorganism growth in temperature, humidity proper environment, the active nano-calcium carbonate containing in component does not almost have inhibition to microorganism.
CN103013354A discloses a kind of preparation method of neutral mildew-resistant glass cement, and its effective constituent be it is said the Antisepticize and mildew preventive of a kind of A2 of being called, does not find its actual component structure.
When 266～268 pages of " organosilicon material " (2013,27 (4)) have reported that adding 3 kinds of mould inhibitor massfractions is less than 1%, the mildew-resistant grade of gained mildew-resistant organosilicon sealant reaches 1-0 level, undeclared 3 kinds of mould inhibitor component structures in literary composition.
CN103122238A has announced a kind of antibacterial and mouldproof silicone adhesive and preparation method thereof, its antiseptic-germicide used is that cubes zirconium phosphate carries silver compound, but this component belongs to silver-series antibacterial agent kills effect excellence to bacterium, but on the weak side to mould effect, and in use procedure, there is silver-colored yellowing variable color danger.
At present, mildew-resistant silicone adhesive product mostly is external import or domestic a few large factory production on the market, production cost is higher, 30 yuan of left and right of every sebific duct price, other is beyond affordability for ordinary people, and its mildew-resistant mechanism is mainly to rely on silica gel material self inertia to resist and performance mildew-proof function microorganism growth, the actual use procedure of human consumer as moist especially rugged environment in the frequent phenomenon of appearance " mildew-resistant glue " not mildew-resistant.So be badly in need of a kind of safety, environmental protection, efficient, long acting antibiotic mildew-resistant ketone glue on market, and also need material produce manufacture craft simple, cost is lower, meet other service requirements of ordinary people, can apply on a large scale.For this reason, the inventor has completed the present invention finally through lot of experiments.
Summary of the invention
The object of this invention is to provide a kind of long acting antibiotic mildew-resistant silicone adhesive.
Another object of the present invention is to provide the preparation method of described long acting antibiotic mildew-resistant silicone adhesive.
The present invention is achieved through the following technical solutions.
The present invention relates to a kind of long acting antibiotic mildew-resistant silicone adhesive, it is characterized in that what described long acting antibiotic mildew-resistant silicone adhesive was made up of following component by weight:
Basis glue 40-90 part;
Linking agent 2-10 part;
Filler 2-40 part;
Catalyzer 0.05-1 part;
Softening agent 0-20 part;
Coupling agent 0.5-5 part;
Composite antimicrobial mould inhibitor 0.5-2 part;
Described basic glue is α, alpha, omega-dihydroxy polydimethyl siloxane (107 glue); Described linking agent is the one in methyl triacetoxysilane, methyl tributanoximo silane, methyltrimethoxy silane or methyl isopropyl alkene TMOS; Described filler is the one in gas-phase silica or nano-calcium carbonate; Described catalyzer is the one in two acetic acid acid dibutyl tins or diisopropoxy-bis-(acetylacetone based) titanium; Described softening agent is polydimethylsiloxane; Described coupling agent is (KH-560) one in propyl trimethoxy silicane or γ-(methacryloxypropyl) propyl trimethoxy silicane (KH-570) of γ-(2,3-epoxy the third oxygen).
The antibacterial and mouldproof silicone adhesive the present invention relates to, is characterized in that what described composite antimicrobial mould inhibitor was made up of following component by weight:
Carry zinc zeolite inorganic antiseptic 75-94.5 part;
Organic biocide mildewcide 5-20 part;
Coupling agent 0.5-5 part;
Described organic biocide mildewcide is N-(2, 2-dichloroethylene) salicylic amide (A26), derosal (methyl-benzimidazolyl-2 radicals-Urethylane, BCM), m-tetrachlorophthalodinitrile (2, 4, 5, 6 one tetrachloros 1, 3 one benzene dicarbonitriles), Zinc Pyrithione (ZPT), N-octyl group-isothiazolinone (OIT), 4, 5-bis-chloro-N-octyl group-4-isothiazoline-3-ketone (DCOIT), 1, 2-benzisothiazole-3-ketone (BIT), n-butyl-1, at least one in 2-isothiazoline-3-ketone (BBIT) or IPBC (IPBC), described coupling agent is three stearic acid isopropyl titanates.
The invention still further relates to the preparation method of long acting antibiotic mildew-resistant silicone adhesive, it is characterized in that the step of the method is as follows:
A, first by organic biocide mildewcide, carry zinc zeolite inorganic antiseptic, coupling agent and grinding aid dehydrated alcohol adds in blue-type mulling machine together, under normal temperature, under 1000-2000rpm rotating speed, grind 60-120min; Then heat to 60-80 ℃ of unlatching vacuum, continue to stir 30-60min and remove ethanol, and reclaim ethanol; Finally emit material and can make composite antimicrobial mould inhibitor, for subsequent use.
B, first composite antimicrobial mould inhibitor prepared to basic glue, softening agent, steps A is dropped in multifunctional mixer to vacuum stirring 15-30min at 80-120 ℃ by proportioning; Then add linking agent and filler to continue to stir 30-60min; Secondly add catalyzer and coupling agent by proportioning, vacuum stirring 30-60min at 100-150 ℃; Finally be cooled to 30-40 ℃ of extrusion material and pack, complete the preparation of long acting antibiotic mildew-resistant silicone adhesive.
The principle of institute of the present invention foundation is: make silicone adhesive reach good anti-mold effect, its key is the screening of added mould inhibitor and effectively combination, and technological core of the present invention is the preparation of composite antimicrobial mould inhibitor.In the process of preparation, the comprehensive feature of analyzing existing inorganic antiseptic and organic biocide mildewcide self, the two is organically combined by any special measures, make its advantage with inorganic antiseptic high safety, good endurance, there is again has a broad antifungal spectrum, quick-acting antibacterial and mouldproof.Consider in addition expensive, the allochroic shortcoming of silver-series antibacterial agent, determine to select zinc series antibacterial agent as inorganic antiseptic component, and select to have year zinc zeolite antibacterial agent of vesicular structure, cost is lower, colourless change problem.To pay close attention to its hypotoxicity, the feature of environmental protection and high-efficiency broad spectrum selecting organic biocide mildewcide simultaneously.The preparation of composite antimicrobial mould inhibitor completes on basket-type grinder, use dehydrated alcohol as grinding aid, itself and organic biocide mildewcide have certain consistency, can guarantee that organic biocide mildewcide forms ultra-fine particles under speed lapping state, penetrate into dehydrated alcohol in the vesicular structure that carries zinc zeolite, titanate coupling agent that the present invention adds both can form firm keyed jointing by covalent linkage or hydrogen bond with organic biocide mildewcide Semi-polarity group or atom simultaneously, also can form firm keyed jointing with activity hydroxy in year zinc zeolite cavity structure silicate simultaneously, so titanate coupling agent can be keyed to zeolite cavity surface securely by entering the organic biocide mildewcide carrying in zinc zeolite cavity, guarantee its in use slowly releases the same with zine ion, improve useful life longevity, simultaneously together with zine ion to bacterium, the harmful microorganisms such as mould form collaborative inhibitory or killing effect, there is good synergistic effect.
Antibacterial and mouldproof silicone adhesive type of the present invention is the de-acetic acid type of single-component, single-component ketoxime removing type, single-component dealcoholization-type or single-component deacetone, can meet the different technical requirements in silicone adhesive different application field.
Product stock stable performance of the present invention, raw materials safety and environmental protection, in use antibacterial and mouldproof silicone adhesive is greater than 99% to the antibiotic rate of intestinal bacteria and streptococcus aureus, six kinds of mildew-resistant grades of mixing mould such as aspergillus niger, terreus are reached to 1～0 grade, and antibacterial and mouldproof lasting effect excellent performance.
The present invention will be described below in more detail.
The present invention relates to a kind of long acting antibiotic mildew-resistant silicone adhesive, it is characterized in that what described long acting antibiotic mildew-resistant silicone adhesive was made up of following component by weight:
Basis glue 40-90 part;
Linking agent 2-10 part;
Filler 2-40 part;
Catalyzer 0.05-1 part;
Softening agent 0-20 part;
Coupling agent 0.5-5 part;
Composite antimicrobial mould inhibitor 0.5-2 part.
According to a kind of optimal way of the present invention, described basic glue is α, alpha, omega-dihydroxy polydimethyl siloxane (107 glue); Described linking agent is the one in methyl triacetoxysilane, methyl tributanoximo silane, methyltrimethoxy silane or methyl isopropyl alkene TMOS; Described filler is the one in gas-phase silica or nano-calcium carbonate; Described catalyzer is the one in two acetic acid acid dibutyl tins or diisopropoxy-bis-(acetylacetone based) titanium; Described softening agent is polydimethylsiloxane; Described coupling agent is (KH-560) one in propyl trimethoxy silicane or γ-(methacryloxypropyl) propyl trimethoxy silicane (KH-570) of γ-(2,3-epoxy the third oxygen).The above basic material of preparing silicone adhesive of the present invention is commercially available conventional products.
The antibacterial and mouldproof silicone adhesive the present invention relates to, is characterized in that what described composite antimicrobial mould inhibitor was made up of following component by weight:
Carry zinc zeolite inorganic antiseptic 75-94.5 part;
Organic biocide mildewcide 5-20 part;
Coupling agent 0.5-5 part.
According to a kind of optimal way of the present invention, the described zinc zeolite antibacterial agent that carries is that zine ion is loaded to and in porous natural zeolite or synthetic zeolite, formed the novel compositions with antibacterial effect by ion-exchange, the median size of used year zinc zeolite of the present invention is 1-10 μ m, is the product of market sale.
According to another kind of optimal way of the present invention, described organic biocide mildewcide is N-(2, 2-dichloroethylene) salicylic amide (A26), derosal (methyl-benzimidazolyl-2 radicals-Urethylane, BCM), m-tetrachlorophthalodinitrile (2, 4, 5, 6 one tetrachloros 1, 3 one benzene dicarbonitriles), Zinc Pyrithione (ZPT), N-octyl group-isothiazolinone (OIT), 4, 5-bis-chloro-N-octyl group-4-isothiazoline-3-ketone (DCOIT), 1, 2-benzisothiazole-3-ketone (BIT), n-butyl-1, at least one in 2-isothiazoline-3-ketone (BBIT) or IPBC (IPBC), described coupling agent is three stearic acid isopropyl titanates.
N-(2,2-dichloroethylene) salicylic amide (A26), has another name called fungi spirit or trichlamide, and CAS is numbered 70193-21-4, and molecular formula is C
13h
16cl
5nO
3, pale powder, is a kind of good high-efficiency low-toxicity mould inhibitor, is widely used in the antimycotic antiseptics such as leather, coating, cloth plastic cement, spinning sizing agent.There is an extremely strong inhibition to Aspergillus and Penicillium fungi and chactomium globosum, bread mould, reaping hook are mould etc., the various microorganisms such as intestinal bacteria, streptococcus aureus, tangerine grass bacillus are all had to extremely strong killing action, and the minimum inhibitory concentration (MIC) to various bacterium is 50～500ppm.The present invention mould inhibitor A26 used is the product of Shandong Ai Pu chemical company production and sales.
Derosal, has another name called carbendazol, carbendazol, and CAS is numbered 10605-21-7, and formal name used at school methyl-benzimidazolyl-2 radicals-Urethylane is called for short BCM.Derosal is a kind of broad-spectrum germicide, and the disease that various crop is caused by fungi (as imperfect fungi, many ascomycetess) has prevention effect.Can be used for foliar spray, seed treatment and soil treatment etc.The present invention's derosal used is the product of Huayang Agricultural Chemial Group Co Ltd, Shandong or the production and sales of Jiangsu Tai Cang Nong Hua company limited.
M-tetrachlorophthalodinitrile (2,4,5,6 one tetrachloro one 1,3 one benzene dicarbonitriles), CAS is numbered 1897-45-6, and molecular formula is C
8n
2cl
4, be a kind of low toxicity, non-internal-absorting wide-spectrum bactericide, various crop fungal disease is had to prophylactic effect.
ZPT, English name is Pyrithionc Zinc, writes a Chinese character in simplified form ZPT, calls as Pyrithionc Zinc, and CAS is numbered 13463-41-7, and molecular formula is C
10h
8n
2o
2s
2zn, molecular weight is 317.7.For shampoo anti-dandruff, can suppress the growth of Gram-positive, negative bacteria and mould.Hair conditioning effectively, delays the aging of hair, controls the generation of white hair and alopecia.Also be used as in addition makeup preservatives or finish, coating biocide; As the biocide mildewcide of the product such as coating and plastics, use also very extensive.The present invention's ZPT used (ZPT) is the set a prairie fire product of Chemical Co., Ltd.'s production and sales of Hebei KeYu biochemical industry company limited or Jiangsu.
N-octyl group-isothiazolinone, CAS is numbered 26530-20-1, is called for short OIT, is dissolved in organic solvent, is slightly soluble in water, is a kind of low toxicity, efficient, broad spectrum type biocide mildewcide, and bacterium, mould etc. are had to very strong killing action, can reach desirable anti-mold effect.Can be widely used in all multi-products such as coating, paint, lubricating oil, shoe polish, leather chemistry, timber-work and historical relic's protection.VOC free, high light and high temperatures, sterilization broad-spectrum high efficacy, can effectively prevent bacterium and fungi in plastics.The present invention OIT used is the product of Dalian Bai Ao chemical company or Beijing Tianqing Chemical Co., Ltd.'s production and sales.
The chloro-N-octyl group-4-of 4,5-bis-isothiazoline-3-ketone, CAS is numbered 64359-81-5, is called for short DCOIT, is a kind of wide-spectrum bactericide.Can be widely used in the plastic industries such as paint, coating, polyethylene, polyurethane, leather, paint, coating, sewage, papermaking, timber, tackiness agent, the fields such as ink, can replace the compound such as organoarsenic of huge poison.The present invention DCOIT used is the product of Dalian Bai Ao chemical company or Beijing Tianqing Chemical Co., Ltd.'s production and sales.
BIT, CAS is numbered 2634-33-5, is called for short BIT, is main industrial sterilization, anticorrosion, anti-enzyme agent.There is the grow effects of microorganism in organic medium such as outstanding mould fungus inhibition (fungi, bacterium), algae, solved that the organic products that microbial growth causes is mouldy, fermentation, rotten, breakdown of emulsion, smelly, etc. series of problems.The present invention DCOIT used is the product of Dalian Bai Ao chemical company production and sales.
N-butyl-1,2-isothiazoline-3-ketone, CAS is numbered CAS 4299-07-4, be called for short BBIT, be exclusively used in to kill and corrode the microorganism being attached on the macromolecular materials such as urethane (PU), polyvinyl chloride (PVC), polysiloxane (silicone), polyethylene (PE), polypropylene (PP), can be miscible with softening agent, organic carrier and thinner, easy to use.The present invention BBIT used is the product of Shandong Ai Pu chemical company production and sales.
IPBC (IPBC), is numbered 55406-53-6 No. CAS, and molecular formula is C
8h
12iNO
2, be a kind of effectively fungicidal preservative, be mainly used in the variable color control, textiles, paper-making industry, ink, tackiness agent of makeup, household chemicals, paint, leather, plastics, timber, metal cutting solution, timber etc.The present invention IPBC used is the product of Hangzhou Shang You Chemical Co., Ltd. production and sales.
Preferably, organic biocide mildewcide of the present invention is N-(2,2-dichloroethylene) salicylic amide (A26), Zinc Pyrithione (ZPT), 4,5-bis-chloro-N-octyl group-4-isothiazoline-3-ketone (DCOIT), 1,2-benzisothiazole-3-ketone (BIT), n-butyl-1, at least one in 2-isothiazoline-3-ketone (BBIT) or IPBC (IPBC).
More preferably, organic biocide mildewcide of the present invention is N-(2,2-dichloroethylene) salicylic amide (A26), Zinc Pyrithione (ZPT), n-butyl-1, at least one in 2-isothiazoline-3-ketone (BBIT) or IPBC (IPBC).
According to another kind of optimal way of the present invention, described coupling agent is three stearic acid isopropyl titanates, belong to titante coupling agent, its CAS is numbered 61417-49-0, and the active group containing in this compounds can form strong chemical bond linkage easily with the active group that contains in inorganic materials, organic materials etc.The present invention's three stearic acid isopropyl titanates used are commerical prods that the trade mark of Nanjing Xu Yang Chemical Co., Ltd. production and sales is XY-32.
The invention still further relates to the preparation method of long acting antibiotic mildew-resistant silicone adhesive, it is characterized in that the step of the method is as follows:
A, first by organic biocide mildewcide, carry zinc zeolite inorganic antiseptic, coupling agent and grinding aid dehydrated alcohol adds in blue-type mulling machine together, under normal temperature, under 1000-2000rpm rotating speed, grind 60-120min; Then heat to 60-80 ℃ of unlatching vacuum, continue to stir 30-60min and remove ethanol, and reclaim ethanol; Finally emit material and can make composite antimicrobial mould inhibitor, for subsequent use.
B, first composite antimicrobial mould inhibitor prepared to basic glue, softening agent, steps A is dropped in multifunctional mixer to vacuum stirring 15-30min at 80-120 ℃ by proportioning; Then add linking agent and filler to continue to stir 30-60min; Secondly add catalyzer and coupling agent by proportioning, vacuum stirring 30-60min at 100-150 ℃; Finally be cooled to 30-40 ℃ of extrusion material and pack, complete the preparation of long acting antibiotic mildew-resistant silicone adhesive.
According to the bright a kind of preferred implementation of this law, be that the basket-type grinder in described preparation method's steps A is still blue-type mulling machine, belong to wet grinding device, be applicable to the industries high to fineness requirement such as coating, ink, pigment, mill base, makeup, agricultural chemicals, medicine.This equipment has changed traditional production technique, and former dispersion sand milling two procedures is united two into one, and has reduced technological process, has improved production efficiency, has reduced material waste.The present invention's still basket-type grinder used is the equipment of Shanghai Ai Feng mechanical & electronic equipment corporation, Ltd production and sales.
According to the bright another kind of preferred implementation of this law, be that described grinding aid is dehydrated alcohol, its add-on is organic biocide mildewcide, carries the 10-15% of zinc zeolite inorganic antiseptic, coupling agent three gross weight, and this proportional range can guarantee that material is fully wetting, and avoids causing waste.
According to the bright a kind of preferred implementation of this law, be that described multifunctional mixer is for the two multifunctional mixers that disperse of two frames, the two closed-in constructions of this machine have the end of scraping function, and its stirring rake also rotation in revolution, make the upper and lower and surrounding motion of material, thereby can reach in a short period of time mixed effect; It is a kind of high-efficiency appliance that collects reaction, mixes, is separated into one, be applicable to electronics, chemical industry, pharmacy, the building materials such as tackiness agent, rubber tool glue, silicone sealant, polyurethane sealant, ointment, the techniques such as the mixing of the liquid of pesticide industry and liquid, solid and liquid material, reaction, dissolving.The two dispersion of used pair of frame of the present invention multifunctional mixer is the equipment of Shanghai Suowei Electromechanical Equipment Co., Ltd.'s production and sales.
According to the bright another kind of preferred implementation of this law, the vacuum tightness of multifunctional mixer described in described preparation technology is-0.07～0.12MPa, and rotating speed is 500-800rpm.In product of the present invention preparation, material system must remain in high vacuum state, contained humidity in material is departed from away, otherwise can affect the storage effect of moulding product; It is moderate that material spoils speed, both guaranteed material kneading fully, do not waste energy again, thinks that equipment mixing speed is controlled at 500-800rpm most suitable through great many of experiments.
Describe the detection test of the antibacterial and mouldproof performance of long acting antibiotic mildew-resistant silicone adhesive prepared by the present invention below in detail.
Detection method and detected result are as follows: the anti-bacterial effect evaluation test of antibacterial and mouldproof silicone adhesive prepared by the present invention is by the film applicator coating test of GB/T 21866-2008 " antibiotic paint (paint film) germ resistance assay method and antibacterial effect " standard regulation, and test bacterial classification is intestinal bacteria (ATCC25922) and streptococcus aureus (ATCC6538); And the measurement of test method that anti-mold effect evaluation stipulates by GB/T 1741-2007 " paint film fungus resistance assay method " standard, bacterial classification is that six kinds of aspergillus niger (AS 3.4463), terreus (AS 3.3935), paecilomyces varioti (AS 3.4253), penicillium funiculosum (AS 3.3875), ball hair shell (AS 3.4254), Aureobasidium pullulans (AS 3.3984) etc. mix moulds.In addition, the antibacterial and mouldproof silicone adhesive print that prepared by water treatment condition (soaking print 16h in the distilled water water-bath of 50 ± 2 ℃) processing the present invention of the evaluation building water pipe endurance quality of reference standard JC/T939-2004 " antibacterium plastics tubing antibacterium performance for building " regulation evaluates its water-fast antibacterial and mouldproof effect; The UV Light condition of simultaneously evaluating the antibacterial endurance quality method of paint film in reference standard GB/T 21866-2008 is processed antibacterial and mouldproof silicone adhesive print prepared by the present invention and is evaluated its fast light antibacterial and mouldproof effect.Its test-results is listed in table 1.
Table 1: the antibacterial and mouldproof test-results of antibacterial and mouldproof silicone adhesive of the present invention
While using as can be seen from Table 1 single zeolite to carry zinc inorganic antiseptic in silicone adhesive, water treatment and optical processing front and back anti-microbial property decrease but still keep antibiotic rate more than 90%, but anti-mold effect is all very poor before and after processing, and illustrates that this type of antiseptic-germicide is to mould inhibition deviation; Use single organic biocide mildewcide in silicone adhesive time, before and after water treatment and optical processing, antibacterial and mouldproof effect occurs to reduce largely, and antibiotic rate is below 90%, and fungicidal properties has been reduced to 2～3 grades by 0 grade; The long acting antibiotic mildew-resistant silicone adhesive that large the present invention makes is less through water, photo-irradiation treatment front and back antibiotic rate and mildew-resistant change of rank after tested, all remain on very high level, antibiotic rate is all greater than 99%, mildew-resistant grade reaches 1～0 grade, the intermediate product NEW TYPE OF COMPOSITE antibacterial mildew inhibitor that this explanation obtains through preparation technology of the present invention has had better activity, higher water-fast light fastness than single zeolite inorganic antiseptic or organic biocide mildewcide, therefore the antibacterial and mouldproof silicone adhesive of the present invention being prepared by it just has more durable, long-acting antibacterial and mouldproof effect.
The present invention has following beneficial effect:
First the present invention analyzes on the basis of various system antibacterial mildew inhibitor features in synthetic study, utilizes coupling agent that efficient, the organic biocide mildewcide of environmental protection and the zinc zeolite inorganic antiseptic that carries with vesicular structure are combined together; Then utilize existing silicone adhesive production unit, frequent gained composite antimicrobial mould inhibitor regulation adhesive process is added in silicone adhesive material and gone, complete long acting antibiotic mildew-resistant silicone adhesive and produce.Production technique is simple, and facility investment is few, is easy to suitability for industrialized production, and production cost is low, environmentally friendly, has the very strong market competitiveness.The present invention is by adjusting basic material kind, easily realize multiple types as the production of de-acetic acid type, ketoxime removing type, dealcoholizing-type and the anti-algae silicone adhesive of deacetone, meet different field without technical requirements, be specially adapted to the very moist environment such as the kitchen, toilet, bathroom of house decoration.Antibacterial and mouldproof silicone adhesive storge quality prepared by the present invention is stable, and antibacterial and mouldproof performance is efficient, lasting.
Embodiment
To understand better the present invention by following these embodiment.
embodiment 1:the preparation of long acting antibiotic mildew-resistant silicone adhesive of the present invention
A, first by 10 parts of A26,5 parts of OIT, 82 parts carry zinc zeolite, 3 parts of XY-32 coupling agents and 10 parts of dehydrated alcohols and add together in the still blue-type mulling machine that Shanghai Ai Feng mechanical & electronic equipment corporation, Ltd produces, under normal temperature, under 1500rpm rotating speed, grind 60min; Then heat to 60-80 ℃ of unlatching vacuum, continue to stir 40-50min and remove ethanol, and reclaim ethanol; Finally emit material and can make composite antimicrobial mould inhibitor (A26/OIT/ carries zinc zeolite), for subsequent use.
B, first by 78.4 parts of α, alpha, omega-dihydroxy polydimethyl siloxane (107 glue), 5 parts of polydimethylsiloxanes, 1.5 parts of prepared A26/OIT/ of steps A carry zinc zeolite and drop into two the dispersion in multifunctional mixer of two frames that Shanghai Suowei Electromechanical Equipment Co., Ltd. produces, vacuum stirring 20-30min at 80 ℃ by proportioning; Then add 2 parts of methyl triacetoxysilanes and 10 parts of thermal silicas to continue to stir 30-40min; Secondly add 0.1 part of two acetic acid acid dibutyl tin and 3 parts of KH560 vacuum stirring 50-60min at 120 ℃ by proportioning; Finally be cooled to 30-40 ℃ of extrusion material and pack, complete the preparation of the de-acetic acid type silicone adhesive of long acting antibiotic mildew-resistant.The vacuum tightness of stirrer is-0.07～0.12MPa, and rotating speed is 600rpm.
embodiment 2:the preparation of long acting antibiotic mildew-resistant silicone adhesive of the present invention
A, first by 15 parts of BCM, 3 parts of DCOIT, 78 parts carry zinc zeolite, 4 parts of XY-32 coupling agents and 12 parts of dehydrated alcohols and add together in the still blue-type mulling machine that Shanghai Ai Feng mechanical & electronic equipment corporation, Ltd produces, under normal temperature, under 2000rpm rotating speed, grind 100min; Then heat to 60-80 ℃ of unlatching vacuum, continue to stir 40-50min and remove ethanol, and reclaim ethanol; Finally emit material and can make composite antimicrobial mould inhibitor (BCM/DCOIT/ carries zinc zeolite), for subsequent use.
B, first by 63.5 parts of α, alpha, omega-dihydroxy polydimethyl siloxane (107 glue), 3 parts of polydimethylsiloxanes, 1 part of prepared BCM/DCOIT/ of steps A carry zinc zeolite and drop into two the dispersion in multifunctional mixer of two frames that Shanghai Suowei Electromechanical Equipment Co., Ltd. produces, vacuum stirring 20-30min at 90 ℃ by proportioning; Then add 5 parts of methyl tributanoximo silanes and 15 parts of nano-calcium carbonates to continue to stir 50-60min; Secondly add 0.5 diisopropoxy-bis-(acetylacetone based) titaniums and 5 parts of KH570 vacuum stirring 50-60min at 150 ℃ by proportioning; Finally be cooled to 30-40 ℃ of extrusion material and pack, complete the preparation of long acting antibiotic mildew-resistant ketoxime removing type silicone adhesive.The vacuum tightness of stirrer is-0.07～0.12MPa, and rotating speed is 800rpm.
embodiment 3:the preparation of long acting antibiotic mildew-resistant silicone adhesive of the present invention
A, first 20 parts of ZPT, 75 parts are carried to zinc zeolite, 5 parts of XY-32 coupling agents and 15 parts of dehydrated alcohols and add together in the still blue-type mulling machine that Shanghai Ai Feng mechanical & electronic equipment corporation, Ltd produces, under normal temperature, under 2000rpm rotating speed, grind 120min; Then heat to 60-80 ℃ of unlatching vacuum, continue to stir 40-50min and remove ethanol, and reclaim ethanol; Finally emit material and can make composite antimicrobial mould inhibitor (ZPT/ carries zinc zeolite), for subsequent use.
B, first by 43.8 parts of α, alpha, omega-dihydroxy polydimethyl siloxane (107 glue), 15 parts of polydimethylsiloxanes, 1.1 parts of prepared ZPT/ of steps A carry zinc zeolite and drop into two the dispersion in multifunctional mixer of two frames that Shanghai Suowei Electromechanical Equipment Co., Ltd. produces, vacuum stirring 20-30min at 90 ℃ by proportioning; Then add 8 parts of methyltrimethoxy silanes and 30 parts of thermal silicas to continue to stir 50-60min; Secondly add 0.1 part of dibutyltin diacetate and 2 parts of KH560 vacuum stirring 50-60min at 150 ℃ by proportioning; Finally be cooled to 30-40 ℃ of extrusion material and pack, complete the preparation of long acting antibiotic mildew-resistant dealcoholizing-type silicone adhesive.The vacuum tightness of stirrer is-0.07～0.12MPa, and rotating speed is 700rpm.
embodiment 4:the preparation of long acting antibiotic mildew-resistant silicone adhesive of the present invention
A, first 10 parts of m-tetrachlorophthalodinitriles, 5 parts of IPBC, 81 parts are carried to zinc zeolite, 4 parts of XY-32 coupling agents and 13 parts of dehydrated alcohols and add together in the still blue-type mulling machine that Shanghai Ai Feng mechanical & electronic equipment corporation, Ltd produces, under normal temperature, under 1000rpm rotating speed, grind 50min; Then heat to 60-80 ℃ of unlatching vacuum, continue to stir 40-50min and remove ethanol, and reclaim ethanol; Finally emit material and can make composite antimicrobial mould inhibitor (m-tetrachlorophthalodinitrile/IPBC/ carries zinc zeolite), for subsequent use.
B, first by 75.1 parts of α, alpha, omega-dihydroxy polydimethyl siloxane (107 glue), 8 parts of polydimethylsiloxanes, 0.8 part of prepared m-tetrachlorophthalodinitrile/IPBC/ of steps A carry zinc zeolite and drop into two the dispersion in multifunctional mixer of two frames that Shanghai Suowei Electromechanical Equipment Co., Ltd. produces, vacuum stirring 20-30min at 90 ℃ by proportioning; Then add 5 parts of methyl isopropyl alkene TMOSs and 10 parts of thermal silicas to continue to stir 50-60min; Secondly add 0.6 part of dibutyl tin laurate and 0.5 part of KH560 vacuum stirring 50-60min at 100 ℃ by proportioning; Finally be cooled to 30-40 ℃ of extrusion material and pack, complete the preparation of long acting antibiotic mildew-resistant deacetone silicone adhesive.The vacuum tightness of stirrer is-0.07～0.12MPa, and rotating speed is 500rpm.
embodiment 5:the preparation of long acting antibiotic mildew-resistant silicone adhesive of the present invention
A, first 10 parts of BBIT, 89.5 parts are carried to zinc zeolite, 0.5 part of XY-32 coupling agent and 10 parts of dehydrated alcohols and add together in the still blue-type mulling machine that Shanghai Ai Feng mechanical & electronic equipment corporation, Ltd produces, under normal temperature, under 1000rpm rotating speed, grind 60min; Then heat to 60-80 ℃ of unlatching vacuum, continue to stir 40-50min and remove ethanol, and reclaim ethanol; Finally emit material and can make composite antimicrobial mould inhibitor (BBIT/ carries zinc zeolite), for subsequent use.
B, first by 56.2 parts of part α, alpha, omega-dihydroxy polydimethyl siloxane (107 glue), 5 parts of polydimethylsiloxanes, 0.8 part of prepared BBIT/ of steps A carry zinc zeolite and drop into two the dispersion in multifunctional mixer of two frames that Shanghai Suowei Electromechanical Equipment Co., Ltd. produces, vacuum stirring 20-30min at 90 ℃ by proportioning; Then add 2 parts of vinyl tributyl ketoximyl silanes and 30 parts of nano-calcium carbonates to continue to stir 50-60min; Secondly add 1 part of diisopropoxy-bis-(acetylacetone based) titaniums and 5 parts of KH570 vacuum stirring 50-60min at 150 ℃ by proportioning; Finally be cooled to 30-40 ℃ of extrusion material and pack, complete the preparation of long acting antibiotic mildew-resistant ketoxime removing type silicone adhesive.The vacuum tightness of stirrer is-0.07～0.12MPa, and rotating speed is 600rpm.
embodiment 6:the preparation of long acting antibiotic mildew-resistant silicone adhesive of the present invention
A, first by 10 parts of BCM, 10 parts of BIT, 75 parts carry zinc zeolite, 5 parts of XY-32 coupling agents and 15 parts of dehydrated alcohols and add together in the still blue-type mulling machine that Shanghai Ai Feng mechanical & electronic equipment corporation, Ltd produces, under normal temperature, under 1500rpm rotating speed, grind 100min; Then heat to 60-80 ℃ of unlatching vacuum, continue to stir 40-50min and remove ethanol, and reclaim ethanol; Finally emit material and can make composite antimicrobial mould inhibitor (BCM/BIT/ carries zinc zeolite), for subsequent use.
B, first by 79.3 parts of α, alpha, omega-dihydroxy polydimethyl siloxane (107 glue), 8 parts of polydimethylsiloxanes, 0.8 part of prepared BCM/BIT/ of steps A carry zinc zeolite and drop into two the dispersion in multifunctional mixer of two frames that Shanghai Suowei Electromechanical Equipment Co., Ltd. produces, vacuum stirring 20-30min at 100 ℃ by proportioning; Then add 5 parts of methyltrimethoxy silanes and 6 parts of thermal silicas to continue to stir 50-60min; Secondly add 5 parts of dibutyltin diacetates and 0.5 part of KH560 vacuum stirring 50-60min at 100 ℃ by proportioning; Finally be cooled to 30-40 ℃ of extrusion material and pack, complete the preparation of long acting antibiotic mildew-resistant deacetone silicone adhesive.The vacuum tightness of stirrer is-0.07～0.12MPa, and rotating speed is 700rpm.
Adopt the testing method of describing in this specification sheets, tested the antibacterial and mouldproof performance of long acting antibiotic mildew-resistant silicone adhesive prepared by the present embodiment 1-6, its test result is listed in table 2.
Table 2: the antibacterial and mouldproof performance test results of antibacterial and mouldproof silicone adhesive prepared by embodiment 1-6
Claims (7)
1. a long acting antibiotic mildew-resistant silicon silicone adhesive, is characterized in that what described long acting antibiotic mildew-resistant silicone adhesive was made up of following component by weight:
Basis glue 40-90 part;
Linking agent 2-10 part;
Filler 2-40 part;
Catalyzer 0.05-1 part;
Softening agent 0-20 part;
Coupling agent 0.5-5 part;
Composite antimicrobial mould inhibitor 0.5-2 part;
Described basic glue is α, alpha, omega-dihydroxy polydimethyl siloxane (107 glue); Described linking agent is the one in methyl triacetoxysilane, methyl tributanoximo silane, methyltrimethoxy silane or methyl isopropyl alkene TMOS; Described filler is the one in gas-phase silica or nano-calcium carbonate; Described catalyzer is the one in two acetic acid acid dibutyl tins or diisopropoxy-bis-(acetylacetone based) titanium; Described softening agent is polydimethylsiloxane; Described coupling agent is (KH-560) one in propyl trimethoxy silicane or γ-(methacryloxypropyl) propyl trimethoxy silicane (KH-570) of γ-(2,3-epoxy the third oxygen).
2. long acting antibiotic mildew-resistant silicone adhesive according to claim 1, is characterized in that what described composite antimicrobial mould inhibitor was made up of following component by weight:
Carry zinc zeolite inorganic antiseptic 75-94.5 part;
Organic biocide mildewcide 5-20 part;
Coupling agent 0.5-5 part;
Described organic biocide mildewcide is N-(2, 2-dichloroethylene) salicylic amide (A26), derosal (methyl-benzimidazolyl-2 radicals-Urethylane, BCM), m-tetrachlorophthalodinitrile (2, 4, 5, 6 one tetrachloros 1, 3 one benzene dicarbonitriles), Zinc Pyrithione (ZPT), N-octyl group-isothiazolinone (OIT), 4, 5-bis-chloro-N-octyl group-4-isothiazoline-3-ketone (DCOIT), 1, 2-benzisothiazole-3-ketone (BIT), n-butyl-1, at least one in 2-isothiazoline-3-ketone (BBIT) or IPBC (IPBC), described coupling agent is three stearic acid isopropyl titanates.
3. according to the preparation method of the long acting antibiotic mildew-resistant silicone adhesive described in claim 1-2, it is characterized in that the step of the method is as follows:
A, first by organic biocide mildewcide, carry zinc zeolite inorganic antiseptic, coupling agent and grinding aid dehydrated alcohol adds in blue-type mulling machine together, under normal temperature, under 1000-2000rpm rotating speed, grind 60-120min; Then heat to 60-80 ℃ of unlatching vacuum, continue to stir 30-60min and remove ethanol, and reclaim ethanol; Finally emit material and can make composite antimicrobial mould inhibitor, for subsequent use;
B, first composite antimicrobial mould inhibitor prepared to basic glue, softening agent, steps A is dropped in multifunctional mixer to vacuum stirring 15-30min at 80-120 ℃ by proportioning; Then add linking agent and filler to continue to stir 30-60min; Secondly add catalyzer and coupling agent by proportioning, vacuum stirring 30-60min at 100-150 ℃; Finally be cooled to 30-40 ℃ of extrusion material and pack, complete the preparation of long acting antibiotic mildew-resistant silicone adhesive.
4. preparation method according to claim 3, it is characterized in that the basket-type grinder in described preparation method's steps A is still blue-type mulling machine, the add-on of described grinding aid dehydrated alcohol is the 10-15% of organic biocide mildewcide, year zinc zeolite inorganic antiseptic, coupling agent three gross weight.
5. preparation method according to claim 3, is characterized in that in described preparation method B, multifunctional mixer is the two multifunctional mixers that disperse of two frames, and the vacuum tightness of described stirrer is-0.07～0.12MPa, and rotating speed is 500-800rpm.
6. according to the long acting antibiotic mildew-resistant silicone adhesive described in claim 1-5, it is characterized in that described silicone adhesive type is the de-acetic acid type of single-component, single-component ketoxime removing type, single-component dealcoholization-type or single-component deacetone.
7. according to the long acting antibiotic mildew-resistant silicone adhesive described in claim 1-6, it is characterized in that described antibacterial and mouldproof silicone adhesive is greater than 99% to the antibiotic rate of intestinal bacteria and streptococcus aureus, six kinds of mildew-resistant grades of mixing mould such as aspergillus niger, terreus are reached to 1～0 grade, and antibacterial and mouldproof lasting effect excellent performance.
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