CN105733268A - Mouldproof antibacterial polyorganosiloxane sealing material and preparation method thereof - Google Patents
Mouldproof antibacterial polyorganosiloxane sealing material and preparation method thereof Download PDFInfo
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- CN105733268A CN105733268A CN201610239378.6A CN201610239378A CN105733268A CN 105733268 A CN105733268 A CN 105733268A CN 201610239378 A CN201610239378 A CN 201610239378A CN 105733268 A CN105733268 A CN 105733268A
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L83/00—Compositions of macromolecular compounds obtained by reactions forming in the main chain of the macromolecule a linkage containing silicon with or without sulfur, nitrogen, oxygen or carbon only; Compositions of derivatives of such polymers
- C08L83/04—Polysiloxanes
- C08L83/06—Polysiloxanes containing silicon bound to oxygen-containing groups
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- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
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- C08L2205/02—Polymer mixtures characterised by other features containing two or more polymers of the same C08L -group
- C08L2205/025—Polymer mixtures characterised by other features containing two or more polymers of the same C08L -group containing two or more polymers of the same hierarchy C08L, and differing only in parameters such as density, comonomer content, molecular weight, structure
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- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2205/00—Polymer mixtures characterised by other features
- C08L2205/03—Polymer mixtures characterised by other features containing three or more polymers in a blend
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Abstract
The invention relates to an organosiloxane material in the field of fine chemical industry, in particular to a mouldproof antibacterial polyorganosiloxane sealing material and a preparation method thereof.The sealing material is prepared from, by mass, 95-110 parts of hydroxyl-terminated polydimethylsiloxane, 3-20 parts of an antibacterial component, 15-50 parts of an inorganic filler, 2-10 parts of a silane crosslinking agent and 20-75 parts of an organic additive.The preparation method comprises the steps that the hydroxyl-terminated polydimethylsiloxane, the antibacterial component, the inorganic filler and the organic additive are added into a kneading machine to be mixed to be uniform according to the formula and subjected to heat treatment under the vacuum condition; the mixture is ground with a three-roll grinder and then placed into a planet stirring kettle, then the silane crosslinking agent, the organic additive and a catalyst are added into the planet stirring kettle, mixing under vacuumizing is performed, and then the mixture is transferred into a material pressing machine to be packaged.The polyorganosiloxane sealing material has the excellent and lasting mouldproof and antibacterial performances.
Description
Technical field
The present invention relates to organosiloxane material in field of fine chemical, particularly a kind of antimildew and antibacterial polysiloxane sealing material and preparation method thereof.
Background technology
Functional Organic Polysiloxane has a wide range of applications field, but the phenomenons such as mouldy, xanthochromia in use usually occurs, not only affects that attractive in appearance to affect people again healthy.Especially for the fluid sealant in kitchen, toilet, due to humid environment, microbial reproduction is fast, accumulation over time, cabinet, tank, bathtub periphery encapsulant will turn black and difficult cleaning.And this black mold mostly is aspergillus niger, its spore can float in atmosphere, breeds elsewhere at home.Therefore, the selection of the encapsulant with antibacterial and mouldproof effect is just extremely important.
Existing scholar adopts the interpolation method such as antibacterials, short time drug immersion that organosilicon material carries out surface treatment at present, gives organosilicon material antibiotic property.Such as, the antibacterials such as Cefuroxime Sodium or benzoic methyl nitroazole are added silicone rubber by CN201310415685.1, are prepared for a kind of antibacterial silicon rubber composite material.Antibacterials can slowly release from composite, and then plays antibacterial action, but the membership that adds of antibacterials makes composite light transmission be deteriorated, and in this material only short time effectively, is easily generated drug resistance.
Also scholar is had to propose to add in the material silver ion antimicrobial agent, for instance, patent CN201110195614.6 is by TiO2The TiO of nanoparticle, butyl titanate hydrolysis2Or trifluoroacetic acid or its mixture are as antibacterial, add in silicone rubber, prepare the organic silicon rubber material of long acting antibiotic, as the anti-biological pickup coating in ocean and medical apparatus and instruments and antibacterial product clinically.The patents such as CN201080056842.9, CN201410292145.3, CN201510165646.X, by adding nano silver antimicrobials, are prepared for the silastic material with antibacterial effect.But due to the addition of silver ion antimicrobial agent, the outward appearance of antibiotic property medical silica-gel is under some influence, the transparency declines, and color is partially brown and relatively costly.
It addition, CN201210354212.0 is composite by microalgae cytokines enzyme, biologically active polypeptide, seaweed bio polysaccharide etc., it is prepared for biotype fluid sealant antifungus agent, is added in fluid sealant, for preventing the growth and breeding of mycete in fluid sealant use procedure.But degeneration easily occurs for microalgae cytokines enzyme, biologically active polypeptide, lose biological activity, and then anti-microbial property can not be played.
Therefore, exploitation one has a long effect mould proof antibacterial effect, and can to keep the new function polysiloxane sealing material of above-mentioned property stability for a long time be problem in the urgent need to address.
Summary of the invention
It is an object of the invention to provide a kind of antimildew and antibacterial polysiloxane sealing material and preparation method thereof, to overcome the shortcoming existed in above-mentioned prior art, the organopolysiloxane encapsulant of the present invention has excellent lasting antimildew and antibacterial performance.
The encapsulant of the present invention adopts the following technical scheme that
A kind of antimildew and antibacterial polysiloxane sealing material, as follows by proportion by weight:
Hydroxy-end capped polydimethylsiloxane 95～110 parts
Antibacterial components 3～20 parts
Inorganic filler 15～50 parts
Organic additive 20～75 parts
Silane crosslinker 2～10 parts
A kind of antimildew and antibacterial polysiloxane sealing material, the preferred version adopted is as follows:
Also comprise the following components:
Organotin catalysts 0～3 part
Titanium catalyst 0～1 part.
Antibacterial components is chain alkyl quaternary ammonium group oligosiloxane, this chain alkyl quaternary ammonium group oligosiloxane prepares by the following method: at 50～130 DEG C, organosilan, long-chain alkyl tertiary amine and reaction promoter are reacted 2～10h, first prepare long chain quaternary ammonium base organosilicon, then dropping deionized water or diluted acid or dilute alkaline soln react 3～8h at 20～50 DEG C, prepare chain alkyl quaternary ammonium group oligosiloxane；Or organosilan is first dripped deionized water or diluted acid or dilute alkaline soln and reacts 3～8h at 20～50 DEG C, prepare organic oligomer siloxanes, react 2～4h with allyl compound at 50～80 DEG C again, add long-chain alkyl tertiary amine and continue reaction 2～5h, prepare chain alkyl quaternary ammonium group oligosiloxane；Or organosilan, allyl compound, reaction promoter are reacted 2～4h at 50～80 DEG C, addition long-chain alkyl tertiary amine reacts 2～5h again and obtains long chain quaternary ammonium base organosilicon, then dropping deionized water or diluted acid or dilute alkaline soln react 3～8h at 20～50 DEG C, prepare chain alkyl quaternary ammonium group oligosiloxane；Described chain alkyl quaternary ammonium group oligosiloxane has topological structure, is one or more in caged, trapezoidal, regular or disordered structure.
In antibacterial components chain alkyl quaternary ammonium group oligosiloxane preparation process, the diluted acid dripped or dilute alkaline soln are the one in the weak solution of hydrochloric acid, sulphuric acid, acetic acid, ammonia, sodium hydroxide, potassium hydroxide.
Organosilan chooses one or more in simple function alkoxy silane or two functional alkoxysilanes or trifunctional alkoxy silane, it is preferable that one or more in γ-glycidyl ether oxygen propyl trimethoxy silicane, trimethoxy silane containing hydrogen, triethoxy silane containing hydrogen, dimethoxy silane containing hydrogen, diethoxy silane containing hydrogen, dimethyl silane containing hydrogen, γ-r-chloropropyl trimethoxyl silane, γ-chloropropyl triethoxysilane.
The structural formula of long-chain alkyl tertiary amine is N (CH3)2CnH2n+1, n is span is the positive integer of 6～18.
The structural formula of allyl compound is CH2=CHCH2Cl or CH2=CHCH2OCH2CHCH2O or CH2=CHCH2(C2H4O)m(C3H6O)nCH2CHCH2O, wherein m >=0, n >=0, m and n can not be 0 simultaneously.
Reaction promoter is C1～6The mixture of one or more in positive structure or isomery small molecular alcohol, dioxane, ethylene glycol monomethyl ether, ethylene glycol, butyl glycol ether, propylene glycol monomethyl ether, propylene-glycol ethyl ether, propandiol butyl ether, oxolane, ethyl acetate, monocarboxylic acid, dicarboxylic acids or tricarboxylic acid, reaction promoter consumption is 0.2～5 times of silane containing hydrogen quality.
Organic additive includes polyethers, viscosity is the polydimethylsiloxane of 100～5000mPa.S, (C2H5O)3SiC3H6Cl、Me3SiCH2COOC2H5、(CH3O)3SiC3H6Cl, aminopropyl triethoxysilane, γ-glycidyl ether oxygen propyl trimethoxy silicane, γ-(methacryloxypropyl) propyl trimethoxy silicane, N-(β-aminoethyl)-γ-aminopropyltrimethoxysilane, isocyanatopropyl triethoxysilane, N-(normal-butyl)-gamma-aminopropyl-triethoxy-silane, N-(normal-butyl)-γ-aminopropyltrimethoxysilane, N-methyl-γ-aminopropyltrimethoxysilane, urea propyl trimethoxy silicane, one or more mixture in anilinomethyl trimethoxy silane or anilinomethyl triethoxysilane.
Silane crosslinker includes EtSi (OAc)3、ViSi(OAc)3、(BuO)2Si(OAc)2、Si(OAc)4-Me2Si(OAc)2、MeSi(OMe)3、ViSi(OMe)3、MeSi(ON=CMeEt)3、ViSi(ON=CMeEt)3、Me2Si(NEtAc)2、MeViSi(NEtAc)2、MeSi(OCMe=CH2)3、ViSi(OCMe=CH2)3、(C2H5O)3SiC3H6Cl, aminopropyl triethoxysilane, γ-glycidyl ether oxygen propyl trimethoxy silicane, γ-(methacryloxypropyl) propyl trimethoxy silicane, N-(β-aminoethyl)-γ-aminopropyltrimethoxysilane, isocyanatopropyl triethoxysilane, N-(normal-butyl)-gamma-aminopropyl-triethoxy-silane, N-(normal-butyl)-γ-aminopropyltrimethoxysilane, N-methyl-γ-aminopropyltrimethoxysilane, urea propyl trimethoxy silicane, one or more mixture in anilinomethyl trimethoxy silane or anilinomethyl triethoxysilane.
Hydroxy-end capped polydimethylsiloxane preferably 100 parts.
The preparation method of aforementioned antimildew and antibacterial polysiloxane sealing material, be the technical scheme is that
The preparation method of antimildew and antibacterial polysiloxane sealing material, carry out as follows: by formula, hydroxy-end capped polydimethylsiloxane, antibacterial components, inorganic filler, organic additive are added mixing in kneader, and carry out heat treatment under vacuumized conditions；Then above-mentioned sizing material is first placed in three-roll grinder to be ground, then is placed in planet stirring still, be separately added into silane crosslinker, organic additive and catalyst, move to swager after evacuation mixing and pack.
Accompanying drawing illustrates:
Fig. 1 is the inhibition zone photo of QS-1～QS-7 prepared by the present invention.
Detailed description of the invention
Below in conjunction with embodiment in detail the present invention is described in detail:
Embodiment 1:
Under nitrogen protection; 23.63g γ-glycidyl ether oxygen propyl trimethoxy silicane, 10.67g Dodecyl Dimethyl Amine, 14.88g octadecyldimethyl tertiary amine, 20g isopropanol and 4.6g formic acid are placed in reactor; 4h is reacted under agitation in 75 DEG C; first prepare dodecyl silane quaternary; then drip deionized water again and react 6h at 30 DEG C; under-0.1MPa condition, de-low 30min, prepares dodecyl quaternary ammonium group oligosiloxane (QS-1).
nullBy each 50 parts hydroxy-end capped of the polydimethylsiloxane that viscosity is 80Pa.S and 20Pa.S，10 parts of QS-1，White carbon 15 parts、Precipitated calcium carbonate 30 parts、5 parts of (white carbons of silica flour、Precipitated calcium carbonate and silica flour are as inorganic filler)、Viscosity is the polydimethylsiloxane 10 parts of 100mPa.S、2Pa.S polydimethylsiloxane 15 parts，20 parts of (polydimethylsiloxane of 100mPa.S of 5Pa.S polydimethylsiloxane、The polydimethylsiloxane of 2Pa.S and the polydimethylsiloxane three of 5Pa.S are organic additive)，Add in kneader，Open stirring，Make material at 130 DEG C、Heat treatment 2h is carried out under-0.1MPa condition，Above-mentioned sizing material is placed in three-roll grinder again and grinds 30min，It is subsequently placed in planet stirring still，Add (C2H5O)3SiC3H6Cl and each 0.5 part of ((C of aminopropyl triethoxysilane2H5O)3SiC3H6Cl and aminopropyl triethoxysilane are both as organic additive), methyl tributanoximo silane 4 parts (methyl tributanoximo silane is as silane crosslinker), organotin catalysts 0.1 part, evacuation mixing 60min, move to swager to pack, prepare antimildew and antibacterial organopolysiloxane encapsulant.
Embodiment 2:
Under nitrogen protection, 19.87g γ-r-chloropropyl trimethoxyl silane, 40g butyl glycol ether are added in reactor, under agitation dropping 21.34g Dodecyl Dimethyl Amine, reacts 10h in 110 DEG C, first prepares dodecyl silane quaternary.Then system is down to room temperature, dropping deionized water reaction 4h, then under-0.1MPa condition, takes off low 30min, prepare dodecyl quaternary ammonium group oligosiloxane (QS-2).
By each 50 parts hydroxy-end capped of the polydimethylsiloxane that viscosity is 80Pa.S and 20Pa.S, 5 parts of QS-2, white carbon 20 parts, precipitated calcium carbonate 45 parts, silica flour 5 parts, viscosity is each 15 parts of the polydimethylsiloxane of 100mPa.S and 5Pa.S, adds in kneader, opens stirring, make material at 130 DEG C, heat treatment 2h under-0.1MPa condition, above-mentioned sizing material is placed in three-roll grinder again and grinds 30min, be subsequently placed in planet stirring still, add (C2H5O)3SiC3H6Cl and each 0.5 part of aminopropyl triethoxysilane, methyl tributanoximo silane 5 parts, organotitanium 0.05 part, evacuation mixing 40min, move to swager and pack, and prepares antimildew and antibacterial organopolysiloxane encapsulant.
Embodiment 3:
Under nitrogen protection, 19.87g γ-r-chloropropyl trimethoxyl silane, 40g butyl glycol ether are added in reactor, is under agitation added dropwise to 29.76g octadecyldimethyl tertiary amine, react 8h at 110 DEG C, first prepare octadecyl silane quaternary.Then system is down to room temperature, dropping deionized water reaction 4h, then under-0.1MPa condition, takes off low 30min, prepare octadecyl quaternary ammonium group oligosiloxane (QS-3).
Under nitrogen protection; 23.63g γ-glycidyl ether oxygen propyl trimethoxy silicane, 21.34g Dodecyl Dimethyl Amine, 20g isopropanol and 6.0g acetic acid are placed in reactor; 4h is reacted under agitation in 75 DEG C; first prepare dodecyl silane quaternary; then dropping deionized water reacts 6h at 30 DEG C; de-low 30min under-0.1MPa condition, prepares 12 quaternary ammonium group oligosiloxanes (QS-4) again.
By the polydimethylsiloxane 70 parts that viscosity is hydroxy-end capped for 20Pa.S, polydimethylsiloxane hydroxy-end capped for 5Pa.S 30 parts, each 10 parts of QS-3 and QS-4, white carbon 20 parts, precipitated calcium carbonate 25 parts, 5 parts of kieselguhr, viscosity is each 15 parts of the polydimethylsiloxane of 500mPa.S and 5Pa.S, add in kneader, open stirring, make material 130 DEG C, process 2h under-0.1MPa condition, above-mentioned sizing material is placed in three-roll grinder again and grinds 30min, it is subsequently placed in planet stirring still, adds 0.2 part of aminopropyl triethoxysilane, 0.8 part of Me3SiCH2COOC2H5With 4 parts of methyl triacetoxysilanes, evacuation mixing 60min, move to swager and pack, prepare antimildew and antibacterial organopolysiloxane encapsulant.
Embodiment 4:
Under nitrogen protection; 23.63g γ-glycidyl ether oxygen propyl trimethoxy silicane, 29.76g octadecyldimethyl tertiary amine, 20g isopropanol and 4.6g formic acid are placed in reactor; react 4h in 75 DEG C under agitation, prepare octadecyl silane quaternary A.Under nitrogen protection, 19.87g γ-r-chloropropyl trimethoxyl silane, 40g butyl glycol ether are added in reactor, is under agitation added dropwise to 21.34g Dodecyl Dimethyl Amine, react 10h at 110 DEG C, prepare dodecyl silane quaternary B.Take octadecyl silane quaternary A and each 15g of dodecyl silane quaternary B respectively, under nitrogen protection, dropping deionized water reaction 6h, then under-0.1MPa condition, take off low 30min, prepare chain alkyl quaternary ammonium group oligosiloxane (QS-5).
By the polydimethylsiloxane 40 parts that viscosity is hydroxy-end capped for 20Pa.S, polydimethylsiloxane hydroxy-end capped for 5Pa.S totally 60 parts, 12 parts of QS-5, white carbon 20 parts, precipitated calcium carbonate 25,5 parts of kieselguhr, viscosity is each 15 parts of the polydimethylsiloxane of 500mPa.S and 2.5mPa.S, add in kneader, open stirring, make material 130 DEG C, process 3h under-0.1MPa condition, above-mentioned sizing material is placed in three-roll grinder again and grinds 30min, it is subsequently placed in planet stirring still, adds aminopropyl triethoxysilane and Me3SiCH2COOC2H5Each 0.5 part, methyl triacetoxysilane 4 parts, organotitanium 0.03 part, evacuation mixing 40min, move to swager and pack, prepare antimildew and antibacterial organopolysiloxane encapsulant.
Embodiment 5:
Under nitrogen protection; 16.4g triethoxy silane containing hydrogen and 20g isopropanol are placed in there-necked flask; dilute hydrochloric acid solution is dripped with the speed of 30/min under stirring; after dropwising; reactor is reacted 4h in 50 DEG C; prepare hydrogeneous oligosiloxane; it is subsequently adding 11.4g allyl glycidyl ether and chloroplatinic acid catalyst; 2h is reacted at 75 DEG C; prepare light yellow transparent liquid; add 10.67g Dodecyl Dimethyl Amine, 14.88g octadecyldimethyl tertiary amine and 6g glacial acetic acid reaction 4h, prepare chain alkyl quaternary ammonium group oligosiloxane (QS-6).
Under nitrogen protection; 10.94g triethoxy silane containing hydrogen, 4.47g methyl diethoxy silane containing hydrogen are placed in there-necked flask with 20g isopropanol; dilute hydrochloric acid solution is dripped under stirring; 4h is reacted at 50 DEG C after dropwising; first prepare hydrogeneous oligosiloxane; it is subsequently adding 11.4g allyl glycidyl ether and chloroplatinic acid catalyst; after reacting 2h at 75 DEG C; add 10.67g Dodecyl Dimethyl Amine, 14.88g octadecyldimethyl tertiary amine and 6g glacial acetic acid reaction 4h, prepare chain alkyl quaternary ammonium group oligosiloxane (QS-7).
By each 50 parts hydroxy-end capped of the polydimethylsiloxane that viscosity is 20Pa.S and 5Pa.S, each 8 parts of QS-6 and QS-7, white carbon 20 parts, precipitated calcium carbonate 30 parts, totally 10 parts of kieselguhr, viscosity is 350mPa.S polydimethylsiloxane 10 parts, 2.5mPa.S polydimethylsiloxane 20 parts, add in kneader, open stirring, make material 130 DEG C, process 2h under-0.1MPa condition, again above-mentioned sizing material is placed in three-roll grinder to be ground, it is subsequently placed in planet stirring still, adds 0.3 part of aminopropyl triethoxysilane, 0.2 part of Me3SiCH2COOC2H5With 5 parts of methyl triacetoxysilanes, organotin catalysts 0.1 part, evacuation mixing 60min, move to swager and pack, prepare antimildew and antibacterial organopolysiloxane encapsulant.
Embodiment 6
By each 50 parts hydroxy-end capped of the polydimethylsiloxane that viscosity is 80Pa.S and 20Pa.S, white carbon 20 parts, precipitated calcium carbonate 45, silica flour 5 parts, viscosity is each 15 parts of the polydimethylsiloxane of 100mPa.S and 2.5mPa.S, add in kneader, open stirring, make material 130 DEG C ,-0.1MPa condition processes 2h, more above-mentioned sizing material is placed in three-roll grinder is ground, it is subsequently placed in planet stirring still, adds (C2H5O)3SiC3H6Cl and each 0.5 part of aminopropyl triethoxysilane, methyl tributanoximo silane 5 parts, organotin catalysts 0.1 part, evacuation mixing 30min, move to swager and pack, and prepares the blank sample of organopolysiloxane encapsulant.
The antibacterial effect detection of chain alkyl quaternary ammonium group oligosiloxane
With staphylococcus aureus for representative, adopt Bactericidal test that the anti-microbial property of the chain alkyl quaternary ammonium group oligosiloxane of synthesis is evaluated.
By S. aureus Inoculate on beef-protein medium, cultivate 24h at 37 DEG C, be then seeded into equipped with the test tube of sterilized water is configured to bacteria suspension.
Respectively with methanol dissolved dilution, chain alkyl quaternary ammonium group oligosiloxane (QS-1～QS-7) of synthesis being settled to concentration is 0.10g/mL, take 10 μ L with pipettor and be added drop-wise on the filter paper that diameter is 6mm, after solvent volatilizees, as chain alkyl quaternary ammonium group oligosiloxane test piece, it is designated as 1#～7#.Separately pipette 10 μ L methanol to a filter paper, as blank after methanol volatilizees, be designated as 8# test piece.Then above-mentioned test piece is smooth in the culture medium scribbling staphylococcus aureus bacterium solution respectively, 37 DEG C of constant temperature culture 12h.By the inhibition zone outer diameter dimension in vernier caliper measurement culture dish.As shown in Figure 1, occur without inhibition zone around 8# blank test piece, and present obvious inhibition zone around 1#～7# test piece and antibacterial circle diameter is all higher than 10mm, illustrate that QS-1～QS-7 has significant antibacterial activity.
Bacteriostasis rate is tested
Adopting AATCC100/ film contacts method, with staphylococcus aureus for representative, organopolysiloxane material prepared by embodiment 1～6 carries out the test of bacteriostasis rate, and operating procedure is as follows:
Organopolysiloxane material sample prepared by embodiment 1～6 is made the test piece of 2cm × 2cm, is 5 × 10 with physiological saline solution compound concentration5Bacteria suspension, pipette the staphylococcus aureus bacterial suspension inoculation of 0.4mL to test piece, then sterilised membrane filter is covered, after 37 DEG C of cultivation 18h, remove sterilised membrane filter, repeatedly rinse strip with physiological saline solution, then water lotion is cultivated, adopt colony counting method to measure the quantity of this strip viable bacteria.Wherein the test piece of example 6 preparation is as blank sample.Antibacterial effect is judged by calculating bacteriostasis rate.
Computing formula: R (%)=(B-C)/B × 100%
In formula: R is bacteriostasis rate (%), B is blank control sample clump count, and C is sample clump count.
As shown in Table 1, the blank sample surface attachment of embodiment 6 preparation has and has bioactive staphylococcus aureus in a large number, the staphylococcus aureus of the strip attachment of embodiment 1～5 preparation is then wholly or largely killed, the bacteriostasis rate of the antimicrobial sealing material of embodiment 1～5 preparation is all higher than 99.95%, illustrates that test piece prepared by embodiment 1～5 has the antibacterial effect of excellence.
Table 1 example 1～6 prepares the bacteriostasis rate of sample
Claims (10)
1. an antimildew and antibacterial polysiloxane sealing material, as follows by proportion by weight:
Hydroxy-end capped polydimethylsiloxane 95～110 parts
Antibacterial components 3～20 parts
Inorganic filler 20～70 parts
Silane crosslinker 2～10 parts
Organic additive 20～75 parts.
2. antimildew and antibacterial polysiloxane sealing material according to claim 1, it is characterised in that: also comprise the following components:
Organotin catalysts 0～3 part
Titanium catalyst 0～1 part.
3. antimildew and antibacterial polysiloxane sealing material according to claim 1, it is characterized in that: antibacterial components is chain alkyl quaternary ammonium group oligosiloxane, this chain alkyl quaternary ammonium group oligosiloxane prepares by the following method: at 50～130 DEG C, organosilan, long-chain alkyl tertiary amine and reaction promoter are reacted 2～10h, first prepare long chain quaternary ammonium base organosilicon, then dropping deionized water or diluted acid or dilute alkaline soln react 3～8h, prepare chain alkyl quaternary ammonium group oligosiloxane；Or organosilan is first dripped deionized water or diluted acid or dilute alkaline soln reaction 3～8h, prepare organic oligomer siloxanes, react 2～4h with allyl compound at 50～80 DEG C again, add long-chain alkyl tertiary amine reaction 2～5h, prepare chain alkyl quaternary ammonium group oligosiloxane；Or organosilan, allyl compound, reaction promoter are reacted 2～4h at 50～80 DEG C, addition long-chain alkyl tertiary amine reacts 2～5h again and obtains long chain quaternary ammonium base organosilicon, then dropping deionized water or diluted acid or dilute alkaline soln react 3～8h, prepare chain alkyl quaternary ammonium group oligosiloxane；Described chain alkyl quaternary ammonium group oligosiloxane has topological structure, is one or more in caged, trapezoidal, regular or disordered structure.
4. antimildew and antibacterial polysiloxane sealing material according to claim 3, it is characterised in that: organosilan chooses one or more in simple function alkoxy silane or two functional alkoxysilanes or trifunctional alkoxy silane.
5. antimildew and antibacterial polysiloxane sealing material according to claim 3, it is characterised in that: one or more in the preferred γ-glycidyl ether oxygen propyl trimethoxy silicane of organosilan, trimethoxy silane containing hydrogen, triethoxy silane containing hydrogen, dimethoxy silane containing hydrogen, diethoxy silane containing hydrogen, dimethyl silane containing hydrogen, γ-r-chloropropyl trimethoxyl silane, γ-chloropropyl triethoxysilane.
6. antimildew and antibacterial polysiloxane sealing material according to claim 2, it is characterised in that: the structural formula of long-chain alkyl tertiary amine is N (CH3)2CnH2n+1, n is span is the positive integer of 6～18.
7. antimildew and antibacterial polysiloxane sealing material according to claim 2, it is characterised in that: reaction promoter is C1～6The mixture of one or more in positive structure or isomery small molecular alcohol, dioxane, ethylene glycol monomethyl ether, ethylene glycol, butyl glycol ether, propylene glycol monomethyl ether, propylene-glycol ethyl ether, propandiol butyl ether, oxolane, ethyl acetate, monocarboxylic acid, dicarboxylic acids or tricarboxylic acid, reaction promoter consumption is 0.2～5 times of organosilan quality.
8. antimildew and antibacterial polysiloxane sealing material according to claim 1, it is characterised in that: organic additive includes polyethers, viscosity is the polydimethylsiloxane of 100～5000mPa.S, (C2H5O)3SiC3H6Cl、Me3SiCH2COOC2H5、(CH3O)3SiC3H6Cl, aminopropyl triethoxysilane, γ-glycidyl ether oxygen propyl trimethoxy silicane, γ-(methacryloxypropyl) propyl trimethoxy silicane, N-(β-aminoethyl)-γ-aminopropyltrimethoxysilane, isocyanatopropyl triethoxysilane, N-(normal-butyl)-gamma-aminopropyl-triethoxy-silane, N-(normal-butyl)-γ-aminopropyltrimethoxysilane, N-methyl-γ-aminopropyltrimethoxysilane, urea propyl trimethoxy silicane, one or more mixture in anilinomethyl trimethoxy silane or anilinomethyl triethoxysilane.
9. antimildew and antibacterial polysiloxane sealing material according to claim 1, it is characterised in that: silane crosslinker includes EtSi (OAc)3、ViSi(OAc)3、(BuO)2Si(OAc)2、Si(OAc)4-Me2Si(OAc)2、MeSi(OMe)3、ViSi(OMe)3、MeSi(ON=CMeEt)3、ViSi(ON=CMeEt)3、Me2Si(NEtAc)2、MeViSi(NEtAc)2、MeSi(OCMe=CH2)3、ViSi(OCMe=CH2)3、(C2H5O)3SiC3H6Cl, aminopropyl triethoxysilane, γ-glycidyl ether oxygen propyl trimethoxy silicane, γ-(methacryloxypropyl) propyl trimethoxy silicane, N-(β-aminoethyl)-γ-aminopropyltrimethoxysilane, isocyanatopropyl triethoxysilane, N-(normal-butyl)-gamma-aminopropyl-triethoxy-silane, N-(normal-butyl)-γ-aminopropyltrimethoxysilane, N-methyl-γ-aminopropyltrimethoxysilane, urea propyl trimethoxy silicane, one or more mixture in anilinomethyl trimethoxy silane or anilinomethyl triethoxysilane.
10. the preparation method of an antimildew and antibacterial polysiloxane sealing material as in one of claimed in any of claims 1 to 9, carry out as follows: by formula, hydroxy-end capped polydimethylsiloxane, antibacterial components, inorganic filler, organic additive are added mixing in kneader, heat treatment is carried out under vacuumized conditions, then grinding with three-roll grinder is placed in planet stirring still, it is separately added into silane crosslinker, organic additive and catalyst again, moves to swager after evacuation mixing and pack.
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| CN116574441A (en) * | 2023-04-28 | 2023-08-11 | 湖南中能新材料技术有限公司 | Water-based UV (ultraviolet) coating and preparation method and application thereof |
| CN116574441B (en) * | 2023-04-28 | 2024-03-29 | 湖南中能新材料技术有限公司 | Water-based UV (ultraviolet) coating and preparation method and application thereof |
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