CN106497502A - A kind of silane end capped polyurethane modified silicone seal gum with mould proof net taste effect and preparation method thereof - Google Patents

A kind of silane end capped polyurethane modified silicone seal gum with mould proof net taste effect and preparation method thereof Download PDF

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Publication number
CN106497502A
CN106497502A CN201610947747.7A CN201610947747A CN106497502A CN 106497502 A CN106497502 A CN 106497502A CN 201610947747 A CN201610947747 A CN 201610947747A CN 106497502 A CN106497502 A CN 106497502A
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nano
meter sio
end capped
parts
preparation
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吴传兴
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Maanshan Jiechuang Plastic Science & Technology Co Ltd
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Maanshan Jiechuang Plastic Science & Technology Co Ltd
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    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
    • C08G18/00—Polymeric products of isocyanates or isothiocyanates
    • C08G18/06—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen
    • C08G18/28—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen characterised by the compounds used containing active hydrogen
    • C08G18/2805—Compounds having only one group containing active hydrogen
    • C08G18/288—Compounds containing at least one heteroatom other than oxygen or nitrogen
    • C08G18/289—Compounds containing at least one heteroatom other than oxygen or nitrogen containing silicon
    • C—CHEMISTRY; METALLURGY
    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
    • C09J11/00—Features of adhesives not provided for in group C09J9/00, e.g. additives
    • C09J11/02—Non-macromolecular additives
    • C09J11/04—Non-macromolecular additives inorganic
    • C—CHEMISTRY; METALLURGY
    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
    • C09J183/00—Adhesives based on 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; Adhesives based on derivatives of such polymers
    • C09J183/04—Polysiloxanes
    • C09J183/06—Polysiloxanes containing silicon bound to oxygen-containing groups
    • C—CHEMISTRY; METALLURGY
    • 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
    • C08K2201/00—Specific properties of additives
    • C08K2201/011—Nanostructured additives

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  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Inorganic Chemistry (AREA)
  • Health & Medical Sciences (AREA)
  • Medicinal Chemistry (AREA)
  • Polymers & Plastics (AREA)
  • Sealing Material Composition (AREA)

Abstract

The present invention discloses a kind of silane end capped polyurethane modified silicone seal gum with mould proof net taste effect, is made up of the raw material of following weight portion：α, ω dialkyl polydimethylsiloxane 55 70, Nano-meter SiO_2258, epoxy prapanol 10 17, polyether polyol 18 30,2,4 toluene di-isocyanate(TDI)s 13 18, dibutyl tin laurate 12, γ aminopropyl triethoxysilanes 8 16, appropriate absolute methanol, 0.4mol/L sodium methoxide solutions are appropriate, appropriate amount of ethanol, tetra-n-butyl titanate esters 24, hydroxyl scavenger 13, nano-Ag particles 0.2 1, anion powder 13, tourmaline powder 0.5 1.The present invention is in SiO2The poly- epoxy prapanol of nanoparticle surface situ-formed graft, is compound in base polyurethane prepolymer for use as afterwards so that compound seal glue has the advantage of polyurethane and both silicone sealants concurrently, improves low temperature flexibility, the anti-yellowing property of colloid.

Description

A kind of silane end capped polyurethane modified silicone seal gum with mould proof net taste effect and Its preparation method
Technical field
The present invention relates to silicone rubber preparing technical field, and in particular to a kind of Silante terminated poly- with mould proof net taste effect Urethane modified silicone seal gum and preparation method thereof.
Background technology
Silicone sealant be with polydimethylsiloxane as primary raw material, be aided with cross-linking agent, filler, plasticizer, coupling agent, The paste that catalyst is mixed under vacuum conditions, at room temperature by occurring to solidify to form elasticity with the water in air Silicone rubber.Alcohol is discharged in single-component dealcoholization-type room temperature vulcanized silicone rubber sulfidation, compared to deacidification type and ketoxime removing type, There is environmental protection, free from corrosion advantage, can be widely applied to the industries such as building, electric, space flight and aviation, auto industry, as A kind of adhesive alcohol type fluid sealant of environmental protection will be the trend of future market application.
Xie Guirong, Jiang Hongwei et al. are at which《The research of polyurethane-modified end silylated polyether fluid sealant》In one text, have studied Isocyanate terminated based polyurethanes and end silane epoxide polyurethane and end silylated polyether are combined the fluid sealant of preparation, through polyurethane-modified Sealant material afterwards has the preferably transparency and mechanical property, while also showing good low temperature pliability, yellowing resistance Energy.
The present invention adopts anionic polymerization, in SiO2The poly- epoxy prapanol of nanoparticle surface situ-formed graft, improves which Adhesion between sizing material, is compound in base polyurethane prepolymer for use as, afterwards by using gamma-aminopropyl-triethoxy-silane With the polyurethane prepolymer precursor reactant of-NCO end-blockings, base polyurethane prepolymer for use as is introduced in sizing material so that compound seal glue has poly- ammonia concurrently Ester and the advantage of both silicone sealants, fluid sealant have higher mechanical strength and adhesion strength, while improving the low of colloid Temperature flexibility, anti-yellowing property.
Content of the invention
For the deficiencies in the prior art, it is modified that the present invention provides a kind of silane end capped polyurethane with mould proof net taste effect Silicone sealant and preparation method thereof.
A kind of silane end capped polyurethane modified silicone seal gum with mould proof net taste effect, by the raw material of following weight portion Composition：α, alpha, omega-dihydroxy polydimethyl siloxane 55-70 parts, Nano-meter SiO_225-8 parts, epoxy prapanol 10-17 parts, polyether polyols Alcohol 18-30 parts, 2,4 toluene diisocyanate 13-18 parts, dibutyl tin laurate 1-2 parts, gamma-aminopropyl-triethoxy silicon Alkane 8-16 parts, appropriate absolute methanol, 0.4mol/L sodium methoxide solutions are appropriate, appropriate amount of ethanol, tetra-n-butyl titanate esters 2-4 part, hydroxyl Base scavenger 1-3 part, nano-Ag particles 0.2-1 parts, anion powder 1-3 parts, tourmaline powder 0.5-1 parts.
Comprise the following steps that：
（1）Nano-meter SiO_22The poly- epoxy prapanol of surface grafting：
1. 0.4mol/L sodium methoxide solutions, are taken, Nano-meter SiO_2 is added2, ultrasonic vibration 8-14 minutes, continue reaction 50-70 minutes, After stopped reaction, washed using absolute methanol, then drying, grinding obtain the Nano-meter SiO_2 that surface sodium alkoxide is processed2；
2., by the Nano-meter SiO_2 of above-mentioned surface sodium alkoxide process2, in the epoxy prapanol addition there-necked flask that molecular sieve eliminating water is crossed, control Mixing speed 300-500r/min, temperature 105-115 DEG C, nitrogen are protected, centrifugation after reaction 40-55 minutes, and use ethanol Washing, drying obtain the Nano-meter SiO_2 of the poly- epoxy prapanol of surface grafting2；
（2）Nano-meter SiO_22The preparation of composite polyurethane performed polymer：
Polyether polyol, under the conditions of 100-120 DEG C, vacuum decompression is added in the there-necked flask equipped with agitator and thermometer Dehydration 1-3 hours, are cooled to less than 60 DEG C, use mechanical agitation instead, add step（1）Modified Nano-meter SiO_22Stir, Add 2,4 toluene diisocyanate and dibutyl tin laurate afterwards, be passed through N2, it is warming up to 70-90 DEG C of back flow reaction 6-8 Hour, obtain Nano-meter SiO_22Composite polyurethane performed polymer；
（3）The synthesis of silane end capped polyurethane performed polymer：
Above-mentioned composite polyurethane performed polymer, three ethoxy of γ-aminopropyl are added in the there-necked flask equipped with agitator and thermometer 65-75 DEG C is heated under base silane, vacuum protection, and the lower reaction 1-3 hours of stirring are obtained silane end capped polyurethane performed polymer；
（4）The preparation of fluid sealant：
By α, alpha, omega-dihydroxy polydimethyl siloxane and step（3）The silane end capped polyurethane performed polymer of preparation, tetra-n-butyl titanium Acid esters, hydroxyl scavenger, add in planetary mixer, are kept for vacuum 0.08-0.09MPa stirring 35-45 minutes, add nanometer Argent grain, anion powder, tourmaline powder, stirring reaction 40-60 minute under rotating speed 40-60rpm, obtain and there is mould proof net taste effect Silicone sealant, the fluid sealant is loaded by sealing preserve in plastic rubber bottle by platen.
Wherein, the hydroxyl scavenger is hexamethyldisiloxane.
Compared with prior art, the present invention has advantages below：
（1）The polyurethane prepolymer precursor reactant that the present invention is blocked with-NCO using gamma-aminopropyl-triethoxy-silane, polyurethane is pre- - NCO bases in aggressiveness are all blocked and become-Si (OC2H5)3, on the one hand by the use of Silante terminated hydrolysis property as crosslinking When agent, dampness in air is contacted, rapid there is the Si-OH bases that hydrolysis are generated in silanol, with rubber that condensation occurs be anti- Should, so as to cause the solidification of single-component room-temperature vulcanized silicone rubber to be crosslinked, on the other hand introduce base polyurethane prepolymer for use as so that compound close Sealing has the advantage of polyurethane and both silicone sealants concurrently, and fluid sealant has higher mechanical strength and adhesion strength, while Improve low temperature flexibility, the anti-yellowing property of colloid.
（2）The present invention adopts anionic polymerization, in SiO2Nanoparticle surface causes epoxy prapanol ring-opening polymerisation, in situ Poly- epoxy prapanol is grafted, Nano-meter SiO_2 after grafting2Particle still in regular spherical, is compound in base polyurethane prepolymer for use as afterwards, with It is added in fluid sealant by the modification of base polyurethane prepolymer for use as afterwards, increases SiO2Nanoparticle and the compatibility of colloid so as to Even be dispersed stably in reaction system, improve the adhesion between sizing material, make the percentage elongation of colloid, tensile strength, storage The combination properties such as stability are improved.
（3）The present invention adds nano-Ag particles as antifungus agent, improves fluid sealant in the wet environments such as bathroom, kitchen Lasting fungicidal properties, add anion powder, tourmaline powder, can sustained release anion, for air can be improved during interior Quality.
Specific embodiment
A kind of silane end capped polyurethane modified silicone seal gum with mould proof net taste effect, by the raw material of following weight portion Composition：α, alpha, omega-dihydroxy polydimethyl siloxane 65, Nano-meter SiO_226, epoxy prapanol 14, polyether polyol 24,2,4- toluene two Isocyanates 13, dibutyl tin laurate 2, gamma-aminopropyl-triethoxy-silane 12, appropriate absolute methanol, 0.4mol/L first Alcohol sodium solution is appropriate, appropriate amount of ethanol, tetra-n-butyl titanate esters 3, hydroxyl scavenger 2, nano-Ag particles 0.6, anion powder 2, electricity Gas stone powder 0.8.
Comprise the following steps that：
（1）Nano-meter SiO_22The poly- epoxy prapanol of surface grafting：
1. 0.4mol/L sodium methoxide solutions, are taken, Nano-meter SiO_2 is added2, ultrasonic vibration 10 minutes, continuation reaction 60 minutes stop anti- Ying Hou, is washed using absolute methanol, then drying, grinding obtain the Nano-meter SiO_2 that surface sodium alkoxide is processed2；
2., by the Nano-meter SiO_2 of above-mentioned surface sodium alkoxide process2, in the epoxy prapanol addition there-necked flask that molecular sieve eliminating water is crossed, control Mixing speed 400r/min, 110 DEG C of temperature, nitrogen are protected, centrifugation after reacting 45 minutes, and use washing with alcohol, drying Obtain the Nano-meter SiO_2 of the poly- epoxy prapanol of surface grafting2；
（2）Nano-meter SiO_22The preparation of composite polyurethane performed polymer：
Polyether polyol is added in the there-necked flask equipped with agitator and thermometer, under the conditions of 110 DEG C, vacuum decompression is dehydrated 2 hours, less than 60 DEG C are cooled to, use mechanical agitation instead, add step（1）Modified Nano-meter SiO_22Stir, Zhi Houjia Enter 2,4 toluene diisocyanate and dibutyl tin laurate, be passed through N2, it is warming up to 80 DEG C of back flow reaction 7 hours, is received Rice SiO2Composite polyurethane performed polymer；
（3）The synthesis of silane end capped polyurethane performed polymer：
Above-mentioned composite polyurethane performed polymer, three ethoxy of γ-aminopropyl are added in the there-necked flask equipped with agitator and thermometer 70 DEG C are heated under base silane, vacuum protection, and the lower reaction of stirring 2 hours is obtained silane end capped polyurethane performed polymer；
（4）The preparation of fluid sealant：
By α, alpha, omega-dihydroxy polydimethyl siloxane and step（3）The silane end capped polyurethane performed polymer of preparation, tetra-n-butyl titanium Acid esters, hydroxyl scavenger, add in planetary mixer, keep vacuum 0.08-0.09MPa to stir 40 minutes, add nanometer silver Granule, anion powder, tourmaline powder, stirring reaction 50 minutes under rotating speed 60rpm obtain and have the silicone of mould proof net taste effect close The fluid sealant is loaded sealing preserve in plastic rubber bottle by platen by sealing.
Wherein, the hydroxyl scavenger is hexamethyldisiloxane.
The performance test results：
Tensile strength：2.25MPa, shear strength：2.08MPa, elongation at break：249%, hardness：44A；
Yellowing resistance specific performance is：Fluid sealant is immediately placed into 120 DEG C of baking ovens from after sebific duct extrusion sizing material, and 24 hours non-yellowing.

Claims (3)

1. a kind of silane end capped polyurethane modified silicone seal gum with mould proof net taste effect, it is characterised in that by following heavy The raw material composition of amount part：α, alpha, omega-dihydroxy polydimethyl siloxane 55-70 parts, Nano-meter SiO_225-8 parts, epoxy prapanol 10-17 Part, polyether polyol 18-30 part, 2,4 toluene diisocyanate 13-18 parts, dibutyl tin laurate 1-2 parts, γ-ammonia third Ethyl triethoxy silicane alkane 8-16 parts, appropriate absolute methanol, 0.4mol/L sodium methoxide solutions are appropriate, appropriate amount of ethanol, tetra-n-butyl titanium Acid esters 2-4 parts, hydroxyl scavenger 1-3 part, nano-Ag particles 0.2-1 parts, anion powder 1-3 parts, tourmaline powder 0.5-1 parts.
2. a kind of silane end capped polyurethane modified silicone seal gum with mould proof net taste effect according to claims 1 Preparation method, it is characterised in that comprise the following steps that：
（1）Nano-meter SiO_22The poly- epoxy prapanol of surface grafting：
1. 0.4mol/L sodium methoxide solutions, are taken, Nano-meter SiO_2 is added2, ultrasonic vibration 8-14 minutes, continue reaction 50-70 minutes, stop After only reacting, washed using absolute methanol, then drying, grinding obtain the Nano-meter SiO_2 that surface sodium alkoxide is processed2；
2., by the Nano-meter SiO_2 of above-mentioned surface sodium alkoxide process2, in the epoxy prapanol addition there-necked flask that molecular sieve eliminating water is crossed, control Mixing speed 300-500r/min, temperature 105-115 DEG C, nitrogen are protected, centrifugation after reaction 40-55 minutes, and use ethanol Washing, drying obtain the Nano-meter SiO_2 of the poly- epoxy prapanol of surface grafting2；
（2）Nano-meter SiO_22The preparation of composite polyurethane performed polymer：
Polyether polyol, under the conditions of 100-120 DEG C, vacuum decompression is added in the there-necked flask equipped with agitator and thermometer Dehydration 1-3 hours, are cooled to less than 60 DEG C, use mechanical agitation instead, add step（1）Modified Nano-meter SiO_22Stir, Add 2,4 toluene diisocyanate and dibutyl tin laurate afterwards, be passed through N2, it is warming up to 70-90 DEG C of back flow reaction 6-8 Hour, obtain Nano-meter SiO_22Composite polyurethane performed polymer；
（3）The synthesis of silane end capped polyurethane performed polymer：
Above-mentioned composite polyurethane performed polymer, three ethoxy of γ-aminopropyl are added in the there-necked flask equipped with agitator and thermometer 65-75 DEG C is heated under base silane, vacuum protection, and the lower reaction 1-3 hours of stirring are obtained silane end capped polyurethane performed polymer；
（4）The preparation of fluid sealant：
By α, alpha, omega-dihydroxy polydimethyl siloxane and step（3）The silane end capped polyurethane performed polymer of preparation, tetra-n-butyl titanium Acid esters, hydroxyl scavenger, add in planetary mixer, are kept for vacuum 0.08-0.09MPa stirring 35-45 minutes, add nanometer Argent grain, anion powder, tourmaline powder, stirring reaction 40-60 minute under rotating speed 40-60rpm, obtain and there is mould proof net taste effect Silicone sealant, the fluid sealant is loaded by sealing preserve in plastic rubber bottle by platen.
3. a kind of silane end capped polyurethane modified silicone sealing with mould proof net taste effect according to claims 1,2 The preparation method of glue, it is characterised in that the hydroxyl scavenger is hexamethyldisiloxane.
CN201610947747.7A 2016-10-26 2016-10-26 A kind of silane end capped polyurethane modified silicone seal gum with mould proof net taste effect and preparation method thereof Withdrawn CN106497502A (en)

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Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN107936900A (en) * 2017-12-24 2018-04-20 苏州佳亿达电器有限公司 A kind of fluid sealant for being used to assemble dust catcher
CN109096945A (en) * 2018-06-20 2018-12-28 广州雷斯曼新材料科技有限公司 A kind of tackifier and preparation method thereof applied to silicone sealant
CN109306260A (en) * 2018-08-31 2019-02-05 江苏京展能源科技有限公司 Solar energy evacuated effective glazing compound of one kind and preparation method thereof
CN110511710A (en) * 2019-09-10 2019-11-29 威海成景科技有限公司 A kind of mould proof silane-modified sealant of anion release type and preparation method thereof

Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN107936900A (en) * 2017-12-24 2018-04-20 苏州佳亿达电器有限公司 A kind of fluid sealant for being used to assemble dust catcher
CN109096945A (en) * 2018-06-20 2018-12-28 广州雷斯曼新材料科技有限公司 A kind of tackifier and preparation method thereof applied to silicone sealant
CN109306260A (en) * 2018-08-31 2019-02-05 江苏京展能源科技有限公司 Solar energy evacuated effective glazing compound of one kind and preparation method thereof
CN110511710A (en) * 2019-09-10 2019-11-29 威海成景科技有限公司 A kind of mould proof silane-modified sealant of anion release type and preparation method thereof

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