CN103421464A - Anti-vibration adhesive resistant to high and low temperature - Google Patents
Anti-vibration adhesive resistant to high and low temperature Download PDFInfo
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- CN103421464A CN103421464A CN2013103708898A CN201310370889A CN103421464A CN 103421464 A CN103421464 A CN 103421464A CN 2013103708898 A CN2013103708898 A CN 2013103708898A CN 201310370889 A CN201310370889 A CN 201310370889A CN 103421464 A CN103421464 A CN 103421464A
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Abstract
The invention provides an anti-vibration adhesive resistant to high and low temperature, and aims to provide an anti-vibration adhesive which is good in electric-appliance resistance, good in temperature change resistance, capable of bearing high and low temperature alternating change and pressure of vibration pieces, and not prone to falling off in a using process. According to the technical scheme, the anti-vibration adhesive resistant to the high and low temperature comprises, by weight percentage, 46%-55% of base material which is modified epoxy organic silicon resin, 8%-14% of a curing agent which is low-molecular-weight polyimide, 8%-20% of plasticizer which comprises at least one of dibutyl phthalate, dioctyl phthalate and dioctyl maleate, and 20-30% of filler which comprises at least one of aluminium chloride anhydrous and titanium dioxide. The anti-vibration adhesive resistant to the high and low temperature is good in electric-appliance resistance, good in temperature change resistance, capable of bearing high and low temperature alternating change and pressure of the vibration pieces, not prone to falling off in the using process, and applicable to sealing and fastening screws and nuts of heat-resisting anti-vibration annunciators of various novel engines.
Description
Technical field
The present invention relates to a kind of anti-electric property good, temperature-change resistance is good, can bear the pressure of high low temperature alternation variation and vibrating plate, the high-low temperature resistant antidetonation tackiness agent of difficult drop-off in use procedure.
Background technology
Along with the development of the new and high technologies such as space flight, electronics, nuclear technique, high performance tackiness agent demand is increasing.Under application circumstances, adhesive solidification time, solidification value, temperature tolerance, shearing resistance etc. are all had higher requirement.The fundamental research of domestic high-low temperature resistant high-performance adhesive and product development aspect are all weaker, very large with external difference.As a kind of tackiness agent, general most important quality standard has: A, bonding strength (tack); B, high thermal resistance; C, lower temperature resistance; D, ageing resistance; The retentivity of E, bonding strength.It is bonding not firm that general common tackiness agent occurs, or product embrittlement in for some time, more common.Therefore any caking agent is not omnipotent, and a kind of tackiness agent can only be applicable to certain or the specific adherend matter of a certain class.Blindly very harmful with glue, because adhesive products has hysteresis quality, many coming unstuck is all even just to display after several months at several days, so must be cautiously with glue.Such as the heat-resistant extensively adopted on the engine force signal device MCTB series of jolt-squeezing, need carry out fastening high-low temperature resistant antidetonation tackiness agent with a kind of screw rod to annunciator, nut.This high-low temperature resistant antidetonation tackiness agent plays fixed action, prevents screw rod, nut in use, because the change of vibration or the extraneous factor such as temperature variation produces loosening.Requirement at overload pressure from 0.588 Mpa～6.86 Mpa, the antidetonation tackiness agent that can work in the environment of-60 ℃～220 ℃.Because the two-phase linear expansivity of tackiness agent bonded metal differs too large, bonding difficulty, glue-line easily produces internal stress; The metal bonding position easily produces galvanic corrosion because of the water effect in addition.Therefore require the high-low temperature resistant antidetonation tackiness agent of development, need bear the variation of high low temperature alternation, vibrations and pressure, in use procedure, can not come off and anti-electric property good, temperature-change resistance is good.
The stick of anti-Ultra-Low-Temperature Epoxy Adhesive formula adopted on the market at present mainly contains by mass parts:
1. E-51 epoxy resin 100, base polyurethane prepolymer for use as (NCO=4%～5%) 10, dibutyl phthalate 10, m-xylene diamine 20,30,60 ℃/4h of talcum powder solidify.Use temperature-120 ℃～80 ℃.
2. DW-3 cryogenic, tetrahydrofuran (THF) polyethers epoxy resin+D44 epoxy resin 100,590 solidifying agent, KH-550 4.60 ℃/8h or 100 ℃/2h or 130 ℃/1h solidify.The shearing resistance room temperature 17.7MPa of bonding aluminium alloy ,-196 ℃ of time >=17.7MPa ,-269 ℃ of time >=17.7MPa.Use temperature-269 ℃～60 ℃.
3. E-51 epoxy resin 100, QS-2 (epoxy-terminated polyurethane ether) toughner 20, Amino Terminated polyether(ATPE) 30.Ask benzene dimethylamine 10,2,80 ℃/2h of KH-560 solidifies.(18～33) MPa during shearing resistance of bonding aluminium alloy-269 ℃, 20MPa in the time of 140 ℃.The cold-hot impact property is good.Lasting heatproof generally can reach 500 ℃ of 350 ℃ to 400 ℃ ， Duan Time heatproofs, moment 600 ℃ of heatproofs.To ABS, the various plastics such as PVC, devitrified glass, coated glass and metal and oxide compound have good cementability and bonding strength high, electrical insulation capability is superior.Can produce to react with moisture in air rapidly and be solidified into durable, the resilient colloid of high-performance; Cementability is good, protection against the tide, antidetonation, anti-corona, anti-electric leakage and ageing-resistant performance, water-tolerant, moistureproof and waterproof superior performance.
But the antidetonation tackiness agent of these components can not bear the variation of high low temperature alternation, vibrations and pressure, in use procedure, easily come off, temperature-change resistance is poor, under utmost point low temperature, bonding strength is low, bonding not firm, or embrittlement in for some time, embrittlement and can not using, even cause serious quality accident and very large loss.
Summary of the invention
The objective of the invention is the weak point existed for above-mentioned prior art, provide a kind of anti-electric property good, temperature-change resistance is good, can bear the pressure of high low temperature alternation variation and vibrating plate, difficult drop-off in use procedure, particularly can prevent screw rod on annunciator, nut in use, because the change of extraneous factor produces loosening high-low temperature resistant antidetonation tackiness agent.
A kind of high-low temperature resistant antidetonation tackiness agent provided by the invention, by weight percentage, this high-low temperature resistant antidetonation tackiness agent contains 46%～55% modified epoxy organosilicon resin binder, 8%～14% low molecular weight polycaprolactone imide solidifying agent, in 8%～20% dibutyl phthalate (DBP), dioctyl phthalate (DOP), dioctyl maleate, at least one is as softening agent, and in 20%～30% aluminum trichloride (anhydrous), titanium dioxide, at least one is as filler.
In above-mentioned heat-resisting antidetonation tackiness agent,
1. the modified epoxy organosilicon resin is base-material.Owing to containing aliphatic hydroxyl in epoxy resin structural, ehter bond reaches the cause of very active epoxy group(ing), the polarity of hydroxyl and ehter bond makes epoxy resin molecule and adjacently situated surfaces produce gravitation, and epoxy group(ing) can react with the metallic surface containing reactive hydrogen, generate chemical bond, thus sticking power especially by force, the performance such as stability and sticking power preferably.Due to the existence of siloxane bond, there is high temperature resistant, scale resistance, hydrophobic nature, solidity to corrosion and good electric property, mildew resistance, weather resistance in silicone resin, but its sticking power, bad mechanical strength.Epoxy modified silicone resin integrates epoxy resin and silicone resin good characteristic, have the advantage of epoxy resin and silicone resin concurrently, there is good mechanical property and the excellent performances such as thermostability, non-corrosibility, electrical insulating property, resistant of high or low temperature, anti-corona, radiation hardness, humidity and resistant to chemical media, sticking power is splendid, but room temperature or low-temperature curing.
The present invention has selected the varnish in H61-1 epoxy organosilicon heat-resisting varnish, varnish in H61-1 epoxy organosilicon heat-resisting varnish is to be dissolved in the modified epoxy organosilicon resin in dimethylbenzene with oxyethyl group organosilicon prepolycondensate and intermediate molecular weight epoxy resin after Copolymerization at high temperature.Epoxy resin coordinates thermotolerance, the temperature resistance sex change that has improved base-material, shock resistance with the silicone resin modification.Its content preferred amounts is 48%～50%.
2. solidifying agent is to impel adhesive substance to accelerate curing component by chemical reaction.Because modified epoxy is thermosetting resin, and solidifying agent is the indispensable composition of heat-resisting antidetonation sealing agent, it and main polymer react and enter in molecular structure, can improve bond strength, cohesive strength, chemical stability, water-fast and resistance to medium, thermotolerance and creep resistance etc.In order to solve the matching of high-low temperature resistant antidetonation tackiness agent low-temperature curing and high heat resistance, solidifying agent adopt aliphatic amide that reactive behavior is higher and thermotolerance preferably aromatic amine mix, solidifying agent in H61-1 epoxy organosilicon heat-resisting varnish can reach requirement, and the preferred amounts of its content is 8%～12%.
3. toughner is toughness in order to improve adhesive linkage, the component that improves its resistance to impact shock.In the epoxy silicone resin bonded adhesives, the content of toughner is most important on the impact of its performance, toughner content is very few, and the shearing resistance of material is poor, when toughner content surpasses certain value, along with the increase of toughner content, the thermotolerance of bonded adhesives and shearing resistance all have decline.Toughner, when in tackiness agent, content is suitable (mass ratio 20%), can fully react with solidifying agent, and organosilicon and epoxy resin also can obtain intermiscibility preferably, and the over-all properties of the epoxy organosilicon tackiness agent of preparation is more excellent.Having selected dibutyl phthalate (DBP), dioctyl phthalate (DOP), dioctyl maleate for fragility, shock resistance and the lower temperature resistance of improving high-low temperature resistant antidetonation tackiness agent is softening agent, and the preferred amounts of its content is 10%～20%.
4. chemical reaction does not generally occur in filler in tackiness agent, and it can make the denseness of tackiness agent increase, thermal expansivity reduces, shrinkability reduces.Shrinking percentage while solidifying in order to reduce, improve dimensional stability, thermotolerance and physical strength, influence liquidity, improve the effects such as manufacturability and weather resistance and selected the fillers such as aluminum trichloride (anhydrous), titanium dioxide, it can make the denseness of tackiness agent increase, thermal expansivity reduces, shrinkability reduces, the enhancing shock resistance.The preferred amounts of its content is 22%～26%.Can also add silane coupling agent in case of necessity, silane coupling agent can improve the Joint strength of glued membrane interfacial layer, improves the shearing resistance of epoxy organosilicon tackiness agent.The alkane coupling agent is by trichlorosilane (HSiCl3) with unsaturated olefin addition under the catalysis of platinum chloric acid of reactive group, then obtains through alcoholysis.The organic radical of connecting band functional group on Siliciumatom normally, simultaneously again with an one type of silane of hydrolysable group phase bonding.Silane coupling agent is in fact the silane that a class has organo-functional group, has energy and the chemically combined reactive group of inanimate matter material (as glass, silica sand, metal etc.) and and the chemically combined reactive group of organic material (synthetic resins etc.) in its molecule simultaneously.Can improve bonding strength between resin and solid surface and an one type of silane of weather resistance.Mainly contain KH550, KH560, KH570, KH792, DL602, these several models of DL171.Such as amino silicane coupling agent KH550 molecule contains 2 groups, a close organic group can react with epoxy resin, the other end parent inorganic group is in the reaction of glued membrane system, move to bonding plane from glue, improved the Joint strength of interfacial layer, and KH550, in epoxy organosilicon System forming transition phase, has improved the consistency of epoxy resin and silicone resin, thus the shearing resistance of raising material.
The above-mentioned percentage range of each component of high-low temperature resistant antidetonation tackiness agent is determined by lot of experiments, the anti-electric property of high-low temperature resistant antidetonation tackiness agent that the above-mentioned percentage range of the present invention forms is good, temperature-change resistance is good, can bear the pressure of high low temperature alternation variation and vibrating plate, difficult drop-off in use procedure, be applicable to the sealing, fastening of screw rod, nut on the heat-resisting antidetonation annunciator of many moneys new work engine.
The specific embodiment mode
Further illustrate the present invention below by embodiment and Comparative Examples.In the following Examples and Comparative Examples, can 46%～55% modified epoxy organosilicon resin binder be arranged high-low temperature resistant antidetonation tackiness agent according to the present invention, 8%～14% low molecular weight polycaprolactone imide solidifying agent, at least one softening agent such as 8%～20% dibutyl phthalate (DBP), dioctyl phthalate (DOP), dioctyl maleate, at least one filler in 20%～30% aluminum trichloride (anhydrous), titanium dioxide etc.Any one concrete numerical value in weight percent content, at normal temperatures and pressures, by each component of appointment in table 1 and table 2, by the varnish in H61-1 epoxy organosilicon heat-resisting varnish, be that solidifying agent in base-material, H61-1 epoxy organosilicon heat-resisting varnish is that solidifying agent, dibutyl phthalate (DBP) are that softening agent, aluminum trichloride (anhydrous) are that filler is poured in container and mixed respectively, in stirring at normal temperature extremely evenly, form uniform high-low temperature resistant antidetonation tackiness agent, list test result in table 1.
According to table 1, table 2 formulated high-low temperature resistant antidetonation tackiness agent.
The formula component property index of table 1 embodiment 1～4
Table 2 Comparative Examples formula forms and performance index
Claims (5)
1. a high-low temperature resistant antidetonation tackiness agent, by weight percentage, this high-low temperature resistant antidetonation tackiness agent contains 46%～55% modified epoxy organosilicon resin binder, 8%～14% low molecular weight polycaprolactone imide solidifying agent, in 8%～20% dibutyl phthalate (DBP), dioctyl phthalate (DOP), dioctyl maleate, at least one is as softening agent, and in 20%～30% aluminum trichloride (anhydrous), titanium dioxide, at least one is as filler.
2. high-low temperature resistant antidetonation tackiness agent as claimed in claim 1, is characterized in that, the modified epoxy organosilicon resin content is 48%～50%.
3. high-low temperature resistant antidetonation tackiness agent as claimed in claim 1, is characterized in that, solidifying agent is the low molecular weight polycaprolactone imide, and its content is 8%～12%.
4. high-low temperature resistant antidetonation tackiness agent as claimed in claim 1, is characterized in that, softening agent is a kind of in dibutyl phthalate (DBP), dioctyl phthalate (DOP), dioctyl maleate, and its content is 10%～20%.
5. high-low temperature resistant antidetonation tackiness agent as claimed in claim 1, is characterized in that, filler is a kind of in aluminum trichloride (anhydrous), titanium dioxide, and its content is 22%～26%.
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| Application Number | Priority Date | Filing Date | Title |
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| CN2013103708898A CN103421464A (en) | 2013-08-23 | 2013-08-23 | Anti-vibration adhesive resistant to high and low temperature |
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| CN2013103708898A CN103421464A (en) | 2013-08-23 | 2013-08-23 | Anti-vibration adhesive resistant to high and low temperature |
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| CN103421464A true CN103421464A (en) | 2013-12-04 |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105086919A (en) * | 2015-08-07 | 2015-11-25 | 东莞市新星有机硅科技有限公司 | Nanometer titanium oxide modified organic silicon bonding agent and preparation method thereof |
| CN112029474A (en) * | 2020-09-18 | 2020-12-04 | 中国航发沈阳黎明航空发动机有限责任公司 | Organic silicon sealing adhesive capable of resisting temperature of 500 ℃ and preparation and use methods thereof |
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| CN1546590A (en) * | 2003-12-04 | 2004-11-17 | 四川大学 | Preparation method of room temperature cured high temperature tolerant flexible epoxy adhesive |
| CN1580172A (en) * | 2003-08-01 | 2005-02-16 | 沈阳黎明航空发动机(集团)有限责任公司 | Epoxy modified organic silicon resin adhesive |
| JP2011132541A (en) * | 2011-03-22 | 2011-07-07 | Sumitomo Electric Ind Ltd | Adhesive composition |
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| CN1546590A (en) * | 2003-12-04 | 2004-11-17 | 四川大学 | Preparation method of room temperature cured high temperature tolerant flexible epoxy adhesive |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105086919A (en) * | 2015-08-07 | 2015-11-25 | 东莞市新星有机硅科技有限公司 | Nanometer titanium oxide modified organic silicon bonding agent and preparation method thereof |
| CN112029474A (en) * | 2020-09-18 | 2020-12-04 | 中国航发沈阳黎明航空发动机有限责任公司 | Organic silicon sealing adhesive capable of resisting temperature of 500 ℃ and preparation and use methods thereof |
| CN112029474B (en) * | 2020-09-18 | 2022-04-22 | 中国航发沈阳黎明航空发动机有限责任公司 | Organic silicon sealing adhesive capable of resisting temperature of 500 ℃ and preparation and use methods thereof |
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Application publication date: 20131204 |