CN110205073A - A kind of high-strength ageing MS glue and preparation method thereof - Google Patents

A kind of high-strength ageing MS glue and preparation method thereof Download PDF

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Publication number
CN110205073A
CN110205073A CN201910373443.8A CN201910373443A CN110205073A CN 110205073 A CN110205073 A CN 110205073A CN 201910373443 A CN201910373443 A CN 201910373443A CN 110205073 A CN110205073 A CN 110205073A
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China
Prior art keywords
glue
strength ageing
plasticizer
silane
ageing
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Inventor
陆林森
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DINGLI NEW MATERIAL TECHNOLOGY Co.,Ltd.
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SHANGHAI DONGHE ADHESIVE CO Ltd
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Priority to CN201910373443.8A priority Critical patent/CN110205073A/en
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    • CCHEMISTRY; METALLURGY
    • C09DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09JADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
    • C09J11/00Features of adhesives not provided for in group C09J9/00, e.g. additives
    • C09J11/02Non-macromolecular additives
    • C09J11/06Non-macromolecular additives organic
    • CCHEMISTRY; METALLURGY
    • C09DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09JADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
    • C09J171/00Adhesives based on polyethers obtained by reactions forming an ether link in the main chain; Adhesives based on derivatives of such polymers

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  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Adhesives Or Adhesive Processes (AREA)
  • Compositions Of Macromolecular Compounds (AREA)

Abstract

The invention discloses a kind of high-strength ageing MS glue, by weight, prepare raw material and include at least: 80~120 parts of silane modified polyether performed polymer, 100~180 parts of plasticizer, 70~100 parts of filler, 0.2~5 part of catalyst, 1~10 part of deicer;The invention also discloses a kind of preparation methods of high-strength ageing MS glue, the following steps are included: a. mixing: weighing plasticizer, filler, deicer investment and be stirred kettle, it is stirred 0.5~1 hour, silane modified polyether performed polymer is added to continue to be stirred until homogeneous, it vacuumizes, it is warming up to 90~110 DEG C under agitation, is kept for 1~3 hour;B. it reacts: temperature in the kettle is down to 40~50 DEG C, be filled with nitrogen, catalyst is added, vacuumizes again, after material is sufficiently stirred, releases vacuum to normal pressure, discharge filling to get finished product.The present invention is nontoxic, without any organic solvent and isocyanate prepolymer composition, has good workability, intensity is high, elasticity is good, ageing-resistant performance is strong.

Description

A kind of high-strength ageing MS glue and preparation method thereof
Technical field
The present invention relates to adhesive areas more particularly to a kind of high-strength ageing MS glue and preparation method thereof.
Background technique
MS glue, the i.e. abbreviation of silane modified polyether glue are that a new generation to grow up after silicone adhesive, polyurethane adhesive builds Sealant is built, the fields such as bonding, joint filling, seam, sealing, waterproof, the reinforcement of architectural engineering and decorations are widely used in, Sealant is often used compared to other two, MS glue has excellent on the properties such as caking property, weatherability, the feature of environmental protection, storage characteristics Performance.
Plasticizer is one of indispensable additive in sealant, and the flexibility of high polymer can be substantially improved after use, The workability of sealant is improved, the mechanism of action is that plasticizer molecule can enter between the high-polymer molecule chain, weakens strand Between active force, reduce the crystallinity of high polymer.Phthalic ester plasticizer is industrial the most widely used plasticising One of agent, but its harm increasingly attracts people's attention, if using excessive phthalic acid in adhesive for building Ester is a kind of environmental hormone substance and has carcinogenicity, and people, which is chronically at this environment, can seriously affect health, adult Reproductive disease, infertile can be suffered from, or even suffer from cancer, and children can generate sex premature.Currently, more and more low toxicities or nothing Malicious plasticizer has appeared on the market, but the plasticization effect of new plasticizer used also far away from phthalate There is situations such as migration, exudation in journey, does not simply fail to the flexibility for improving high molecular material when serious, can also reduce its mechanical property Energy.
Summary of the invention
To solve the above-mentioned problems, the first aspect of the present invention provides a kind of high-strength ageing MS glue, by weight Meter, prepares raw material and includes at least: 80~120 parts of silane modified polyether performed polymer, 100~180 parts of plasticizer, filler 70~ 100 parts, 0.2~5 part of catalyst, 1~10 part of deicer.
As a kind of perferred technical scheme, the pressure stream viscosity of the silane modified polyether performed polymer is 10~30s/10g.
As a kind of perferred technical scheme, the silane modified polyether performed polymer has 2 or 3 end alkoxies.
As a kind of perferred technical scheme, the plasticizer is selected from phthalic acid ester, fatty group dibasic acid, epoxy One of acid esters, citrate, phosphate or a variety of mixing.
As a kind of perferred technical scheme, the citrate is selected from triethyl citrate, tributyl citrate, lemon One of sour three monooctyl esters, tributyl 2-acetylcitrate, acetyl tributyl citrate or a variety of mixing.
As a kind of perferred technical scheme, the filler be selected from nanometer calcium carbonate, gas-phase silica, powdered whiting, One of carbon black, silica white, titanium dioxide, nano aluminium oxide or a variety of mixing.
As a kind of perferred technical scheme, the catalyst be selected from stannous octoate, butyric acid tin, dibutyltin diacetate, One of two sad dibutyl tins, chelating tin, dibutyl tin dilaurate, trialkylamine or a variety of mixing.
As a kind of perferred technical scheme, the deicer is selected from vinyltrimethoxysilane, three ethoxy of vinyl One of base silane, vinyl three (2- methoxy ethoxy) silane, 3- (methacryloxypropyl) propyl trimethoxy silicane Or a variety of mixing.
It is as a kind of perferred technical scheme, by weight, described that prepare raw material also include 1~10 part of pigment, ultraviolet 0.1~5 part of absorbent, 0.1~5 part of light stabilizer.
The second aspect of the present invention provides a kind of preparation method of above-mentioned high-strength ageing MS glue, including following step It is rapid:
A. mixing: plasticizer, filler, deicer investment are weighed and is stirred kettle, is stirred 0.5~1 hour, silicon is added Alkane modified polyether performed polymer continues to be stirred until homogeneous, and vacuumizes, and is warming up to 90~110 DEG C under agitation, holding 1~3 is small When;
B. it reacts: temperature in the kettle is down to 40~50 DEG C, be filled with nitrogen, catalyst is added, vacuumizes, is sufficiently stirred again After material, vacuum is released to normal pressure, is discharged filling to get finished product.
The utility model has the advantages that a kind of high-strength ageing MS glue provided by the present application has used environment-protecting and non-poisonous plasticizer, and gram Problem is oozed out in the defect for having taken novel environment-friendlyplasticizer plasticizer, the migration as caused by the poor compatibility with high molecular material, soft after addition Property increase, strength reduction the problem of etc..The present invention is suitable for a variety of substrates, and intensity is high, resistance to ag(e)ing is good, uses safe letter Just.
Specific embodiment
In conjunction with preferred implementation method of the invention below detailed description and including embodiment can be further understood that this hair Bright content.Unless otherwise indicated, all technologies used herein and scientific term all have general with the application fields Logical technical staff's is generally understood identical meaning.If mentioned in the definition and the application of the concrete term disclosed in the prior art Any definition supplied is inconsistent, then term provided herein of being subject to defines.
It is used in the present context, unless being clearly dictated in context, otherwise without the spy of the single plural form of restriction Sign is also intended to the feature including plural form.It will also be appreciated that term as used herein " by ... preparation " it is synonymous with "comprising", " comprising ", " including ", " having ", "comprising" and/or " including " indicate stated group when used in this manual Object, step, method, product or device are closed, but does not preclude the presence or addition of one or more of the other composition, step, method, system Product or device.In addition, using " preferred ", " preferably ", " preferred " etc. to be when describing presently filed embodiment Refer to, can provide the embodiment of the present invention of certain beneficial effects in some cases.However, under identical circumstances or other feelings Under condition, other embodiments are also likely to be preferred.In addition to this, not dark to the statement of one or more preferred embodiments Show that other embodiments are unavailable, is also not intended to exclude other embodiments except the scope of the present invention.
To solve the above-mentioned problems, the first aspect of the present invention provides a kind of high-strength ageing MS glue, by weight Meter, prepares raw material and includes at least: 80~120 parts of silane modified polyether performed polymer, 100~180 parts of plasticizer, filler 70~ 100 parts, 0.2~5 part of catalyst, 1~10 part of deicer.
In some preferred embodiments, by weight, the high-strength ageing MS glue prepares raw material at least Include: 100 parts of silane modified polyether performed polymer, 150 parts of plasticizer, 75 parts of filler, 1 part of catalyst, 7.5 parts of deicer.
Silane modified polyether performed polymer
Silane modified polyether is initially succeeded in developing by Japanese Zhong Yuan chemical industrial company, is by that will contain hydrolyzable base Made from the silane compound of group is connected on the polyethers end group with bifunctionality, so also known as silane-terminated polyether.Silane The synthesis of modified polyether is divided into two steps: (1) with allyl polyether alcohol, end hydroxy polyether etc. for raw material, using methylene halide as chain extension The polyether intermediate of allyl capped is made by chain extending reaction using caustic alkali as catalyst for agent;(2) in platinum group catalyst In the presence of, the intermediate of purification is reacted with methyl dimethoxysilane by end-silicane-groupization reaction and is made silane-modified poly- Ether.
In some preferred embodiments, the pressure stream viscosity of the silane modified polyether performed polymer is 10~30s/10g; It is further preferred that the pressure stream viscosity of the silane modified polyether performed polymer is 20s/10g.
Pressure stream viscosity refers to that pressure stream viscosmeter can be used and measured with the time used in certain pressure extrusion 10g performed polymer, Test parameter includes: that nozzle bore is 3 millimeters, nitrogen pressurization 0.5MPa.
In some preferred embodiments, the silane modified polyether performed polymer has 2 or 3 end alkoxies;Into one Step is preferred, and the silane modified polyether performed polymer has 2 end alkoxies.
The viscosity of silane modified polyether performed polymer can influence the tensile strength, shear strength, extension at break of final finished glue The performances such as rate, if viscosity is excessive, MS glue can generate very long wire drawing when in use, and constructing operation difficulty increases, and sagging resistance It reduces, cannot keep contoured after gluing, intensity substantially reduces;If viscosity is too small, quality is very hard after MS adhesive curing, flexibility Difference, time long situations such as will appear crackle.The curing mechanism category moisturecuring of silane modified polyether seal glue, under moist conditions, End alkoxy first hydrolyzes to be condensed again, forms Si-O-Si key crosslinking points, final to realize solidification.The number of end alkoxy determines close The solidification rate and solidification effect of sealing, end the more then solidification rates of alkoxy number it is fast, the crosslinking points of formation are more, product it is soft Toughness reduces, and displacement capacity is poor, and alkyl number is held solidification rate to be made to slow down less.
Silane modified polyether performed polymer (No. CAS: 75009-88-0) in the application is purchased from Shanghai Mai Ruier chemical technology Co., Ltd.
Plasticizer
The interaction of polymer molecule interchain will lead to entanglement or crystallization, and then influence the mobility of polymer, displacement Ability, droop etc., plasticizer can weaken the Van der Waals force between polymer molecule, increase the mobility of strand after being added, The crystallinity for reducing polymer, so that the flexibility of product glue, flexibility, elongation are improved.
In some embodiments, the plasticizer be selected from phthalic acid ester, fatty group dibasic acid, epoxy acid ester, One of citrate, phosphate or a variety of mixing.
In some embodiments, the phthalic acid ester can enumerate repefral, phthalic acid two Ethyl ester, dibutyl phthalate, dioctyl phthalate, dibenzyl phthalate, diisooctyl phthalate.
In some embodiments, the fatty group dibasic acid can enumerate dioctyl adipate, dioctyl azelate, the last of the ten Heavenly stems Adipate, dibutyl adipate, dibutyl azelate, dibutyl sebacate.
In some embodiments, it is stearic can to enumerate epoxidized soybean oil, epoxidised linseed oil, epoxy for the epoxy acid ester Misery ester, epoxyoleic acid monooctyl ester, epoxyoleic acid butyl ester, epoxyoleic acid last of the ten Heavenly stems ester.
In some embodiments, the phosphate can enumerate tricresyl phosphate, triphenyl phosphate, trioctyl phosphate, Tributyl phosphate, tridecyl phosphate.
In some preferred embodiments, the plasticizer is citrate.
In some preferred embodiments, the citrate is selected from triethyl citrate, tributyl citrate, lemon One of sour three monooctyl esters, tributyl 2-acetylcitrate, acetyl tributyl citrate or a variety of mixing.
In some preferred embodiments, the citrate is trioctyl lemon acid.
Trioctyl lemon acid in the application is purchased from Jiangsu Lei Meng new material Co., Ltd.
Phthalic ester plasticizer is one of industrial the most widely used plasticizer, but its harm is more next It more attracts people's attention, therefore more environmentally friendly plasticizer should be selected, such as citric acid ester type, epoxyeicosatrienoic acid ester plasticizer. However, excellent plasticization effect may be implemented as a kind of solvent-type plasticizer in phthalic acid ester, if using other plasticizer instead It is poor that matrix polymer compatibility can be resulted from, and then migrated, exudation, so that plasticization effect reduces the mechanical property for even influencing product Energy, adhesion property etc..
Filler
Filler is added in adhesive, discord material of main part reacts, the properties of also changeable adhesive, drop Low production cost.According to different needs, the selection of filler is varied, such as increase hardness and compressive property can add quartz Powder, boron carbide, metal oxide powder etc.;The filler for increasing thermal conductivity has aluminium powder, copper powder, iron powder, graphite powder etc.;Increase heat-resisting Property flake asbestos, titanium dioxide, phenolic resin etc. can be used.
In some preferred embodiments, the filler be selected from nanometer calcium carbonate, gas-phase silica, powdered whiting, One of carbon black, silica white, titanium dioxide, nano aluminium oxide or a variety of mixing.
In some preferred embodiments, the filler is silica white;It is further preferred that the mesh number of the silica white For 1000 mesh.
Silica white in the application is purchased from the clever Trade Co., Ltd. in Shanghai.
In some preferred embodiments, the plasticizer and the weight ratio of filler are (1~3): 1;Further preferably , the weight ratio of the plasticizer and filler is 2:1.
The properties of MS glue are superior to polyurethane adhesive, are covering with paint property compared to silicone adhesive biggest advantage, but resistance to Slightly inadequate on hot, it is found by the applicant that silica white helps to improve the heat resistance of MS glue, reason is the main of silica white Ingredient is the silica of very high purity, and the heat resisting temperature of its own is up to 1000 DEG C or more;In addition, silica white reacts work with water Property it is high, there is excellent hygroscopicity, the case where MS glue meets moisturecuring during storage can be effectively reduced, guarantee its performance not It can change.
Applicant further found that plasticization effect is deteriorated after phthalic ester plasticizer is changed to other plasticizer, increase Modeling agent migration, exudation situation are serious, but silica white can be obviously improved this case, it is possible to increase the dosage of plasticizer, and make it It will not migrate, ooze out, the performance of MS glue improves, especially flexibility and displacement capacity.This is because the partial size of silica white it is small and With micro hole structure, sizable specific surface area can generate physisorption to plasticizer, and silica white is as plasticizer Carrier enter the internal structure of high polymer, plasticizer, which plays a role, weakens intermolecular force, reduces the crystallinity of high polymer; Applicant it has surprisingly been found that, select citric acid ester plasticizer that can realize more preferably effect, that is, migrate, ooze out situation into one Step is reduced, and after reason is silica white water suction, surface is formed with the hydroxyl on activity hydroxy, with citric acid ester plasticizer Hydrogen bond, more closely, plasticizer is preferably fixed on inside high polymer the connection between plasticizer and filler.
Catalyst
Catalyst can accelerate the crosslinking curing of MS glue at room temperature, shorten curing time, it is good can also to assign sizing material Good storage stability.
In some preferred embodiments, the catalyst be selected from stannous octoate, butyric acid tin, dibutyltin diacetate, One of two sad dibutyl tins, chelating tin, dibutyl tin dilaurate, trialkylamine or a variety of mixing;It is further excellent Choosing, the catalyst is dibutyl tin dilaurate.
Dibutyl tin dilaurate (No. CAS: 77-58-7) in the application is purchased from the limited public affairs of Shanghai Mai Ruier chemical technology Department.
Deicer
Deicer can rapidly deplete the moisture absorbed in sealant system, make MS glue will not be wet because occurring within storage period Solidify and influences using effect.
In some preferred embodiments, the deicer is selected from vinyltrimethoxysilane, three ethoxy of vinyl One of base silane, vinyl three (2- methoxy ethoxy) silane, 3- (methacryloxypropyl) propyl trimethoxy silicane Or a variety of mixing;It is further preferred that the deicer is vinyltrimethoxysilane.
Vinyltrimethoxysilane (No. CAS: 2768-02-7) in the application has purchased from Shanghai Mai Ruier chemical technology Limit company.
In some preferred embodiments, the weight ratio of the filler and deicer is (8~12): 1;Further preferably , the weight ratio of the filler and deicer is 10:1.
It has been found that selecting silane as deicer, especially containing there are three the silane of methoxyl group with very high anti- Activity is answered, the water consumption in system is fallen by the hydrolysis of silane, improves the storage stability of sealant;In addition, silane Deicer is also used as silane coupling agent, for that can increase caking property in MS colloid system, after reason is silane hydrolyzate The alkoxy of one end generates active silicone hydroxyl, and the hydroxyl condensation of silicone hydroxyl and substrate surface forms stable chemical bond, and The vinyl of the other end of silane coupling agent is equally reactive functional groups, can be in conjunction with polymer, between MS glue and substrate Form bridge.
Applicant further found that the addition of silane coupling agent can further improve migration of plasticizer, exudation.This be by Interaction between silane coupling agent and silica white increases compatibility of the silica white in polymeric system, makes it more Evenly dispersed in system well, the compatibility of the plasticizer loaded enhances therewith, and finally obtained MS glue has good Flexibility, displacement capacity, however the excessively good compatible dispersibility of plasticizer can be such that the mechanical property of MS glue substantially reduces, and silane The addition of coupling agent can balance this defect just, the reason is that, its crosslinking agent that can be used as MS adhesive curing reaction, three Methoxyl group provides more crosslinking nodes, increases crosslink density, and the silica white evenly spread out by silane coupling agent can also be with Certain support is provided to high polymer.
In some preferred embodiments, by weight, the raw material for preparing of the high-strength ageing MS glue also wraps Containing 1~10 part of pigment, 0.1~5 part of ultraviolet absorber, 0.1~5 part of light stabilizer.
In some preferred embodiments, by weight, the raw material for preparing of the high-strength ageing MS glue also wraps Containing 2 parts of pigment, 2 parts of ultraviolet absorber, 1 part of light stabilizer.
The addition of pigment can increase aesthetics when sealant uses, and especially some inorganic pigments are also used as mending Strong filler improves the performance of sealant;The solidification of luminous energy accelerated stock can be absorbed in ultraviolet absorber;Light stabilizer can not only be adjusted Curing rate is saved, can also slow down MS glue because of aging caused by illumination solarization.
In some preferred embodiments, the pigment can enumerate titanium dioxide, zinc white, carbon black, iron oxide black, oxidation Iron oxide red, iron oxide yellow.
In some preferred embodiments, the pigment is titanium dioxide.
Titanium dioxide (No. CAS: 13463-67-7) in the application is purchased from Shanghai Shu Can Industrial Co., Ltd..
In some preferred embodiments, the ultraviolet absorber can enumerate phenyl salicylate, 2- (2 '-hydroxyls -5 ' - Aminomethyl phenyl) benzotriazole, 2,4-DihydroxyBenzophenone, ESCALOL 567,2- hydroxyl -4- be just pungent Oxygroup benzophenone, 2- (2 '-hydroxyls -3 ', 5 '-two tertiary phenyl) -5- chlorination benzotriazole, single benzoic acid resorcinol, 2, 4,6- tri- (2 ' n-butoxyphenyl) -1,3,5-triazines, hexamethylphosphoramide, 2,2 '-thiobis (4- t-octyl phenol oxygroup) Nickel.
In some preferred embodiments, the ultraviolet absorber is 2-hydroxy-4-n-octoxybenzophenone.
2-hydroxy-4-n-octoxybenzophenone (board name: ultraviolet absorbent UV-531 in the application;No. CAS: 1843-05-6) it is purchased from Shanghai Shu Can Industrial Co., Ltd..
In some preferred embodiments, the light stabilizer can enumerate benzoic acid (2,2,6,6- tetramethyl -4- hydroxyls Piperidines) ester, bis- (2,2,6, the 6- tetramethyl -4- hydroxy piperidine) esters of decanedioic acid, [acetic acid (2,2,6, the 6- tetramethyl -4- hydroxyls of nitrogen base three Phenylpiperidines) ester] and bis- (2,2,6, the 6- tetramethyl-piperidyl) hexamethylene diamines of N, N ' -, (1,2,2,6, the 6- pentamethyl -4- of phosphorous acid three Hydroxy piperidine) ester, bis- (1,2,2,6, the 6- pentamethyl -4- hydroxy piperidine) esters of decanedioic acid and 2- ethyl -2- (4- hydroxyl -3,5- tri- Grade butyl benzyl) bis- (1,2,2,6, the 6- pentamethyl -4- hydroxy piperidine) esters of malonic acid.
In some preferred embodiments, the light stabilizer is bis- (2,2,6, the 6- tetramethyl -4- hydroxyl piperazines of decanedioic acid Pyridine) ester.
Bis- (2,2,6,6- tetramethyl -4- hydroxy piperidine) ester (the board names: light stabilizer 770 of decanedioic acid in the application;CAS Number: 52829-07-9) it is purchased from Shanghai Shu Can Industrial Co., Ltd..
The second aspect of the present invention provides a kind of preparation method of above-mentioned high-strength ageing MS glue, including following step It is rapid:
A. mixing: plasticizer, filler, deicer investment are weighed and is stirred kettle, is stirred 0.5~1 hour, silicon is added Alkane modified polyether performed polymer continues to be stirred until homogeneous, and vacuumizes, and is warming up to 90~110 DEG C under agitation, holding 1~3 is small When;
B. it reacts: temperature in the kettle is down to 40~50 DEG C, be filled with nitrogen, catalyst is added, vacuumizes, is sufficiently stirred again After material, vacuum is released to normal pressure, is discharged filling to get finished product.
In some preferred embodiments, the preparation method of the high-strength ageing MS glue, comprising the following steps:
A. mixing: plasticizer, filler, deicer investment are weighed and is stirred kettle, is stirred 1 hour, silane is added and changes Property polyethers performed polymer continue to be stirred until homogeneous, vacuumize, be warming up to 100 DEG C under agitation, kept for 2 hours;
B. it reacts: temperature in the kettle is down to 45 DEG C, be filled with nitrogen, catalyst is added, vacuumizes again, material is sufficiently stirred Afterwards, vacuum is released to normal pressure, is discharged filling to get finished product.
Embodiment
Technical solution of the present invention is described in detail by the following examples, but protection scope of the present invention is not limited to In the embodiment, unless otherwise specified, all raw materials are commercially available.
Embodiment 1
Embodiment 1 provides a kind of high-strength ageing MS glue, by weight, prepares raw material and includes at least: silane 100 parts of modified polyether performed polymer, 150 parts of plasticizer, 75 parts of filler, 1 part of catalyst, 7.5 parts of deicer;
The citrate is trioctyl lemon acid;
The filler is silica white, and mesh number is 1000 mesh;
The catalyst is dibutyl tin dilaurate;
The deicer is vinyltrimethoxysilane.
This example additionally provides the preparation method of above-mentioned high-strength ageing MS glue, comprising the following steps:
A. mixing: plasticizer, filler, deicer investment are weighed and is stirred kettle, is stirred 1 hour, silane is added and changes Property polyethers performed polymer continue to be stirred until homogeneous, vacuumize, be warming up to 100 DEG C under agitation, kept for 2 hours;
B. it reacts: temperature in the kettle is down to 45 DEG C, be filled with nitrogen, catalyst is added, vacuumizes again, material is sufficiently stirred Afterwards, vacuum is released to normal pressure, is discharged filling to get finished product.
Embodiment 2
Embodiment 2 provides a kind of high-strength ageing MS glue, difference from example 1 is that, the preparation Raw material also includes 2 parts of pigment, 2 parts of ultraviolet absorber, 1 part of light stabilizer;
The pigment is titanium dioxide;
The ultraviolet absorber is 2-hydroxy-4-n-octoxybenzophenone;
The light stabilizer is bis- (2,2,6, the 6- tetramethyl -4- hydroxy piperidine) esters of decanedioic acid.
This example additionally provides the preparation method of above-mentioned high-strength ageing MS glue, comprising the following steps:
A. mixing: plasticizer, filler, deicer investment are weighed and is stirred kettle, is stirred 1 hour, silane is added and changes Property polyethers performed polymer continue to be stirred until homogeneous, vacuumize, be warming up to 100 DEG C under agitation, kept for 2 hours;
B. it reacts: temperature in the kettle is down to 45 DEG C, be filled with nitrogen, catalyst, pigment, ultraviolet absorber, light is added and stablizes Agent vacuumizes again, after material is sufficiently stirred, releases vacuum to normal pressure, discharges filling to get finished product.
Embodiment 3
Embodiment 3 provides a kind of high-strength ageing MS glue, difference from example 1 is that, the plasticising Agent is dioctyl phthalate.
This example additionally provides the preparation method of above-mentioned high-strength ageing MS glue, and step is similar to Example 1.
Embodiment 4
Embodiment 4 provides a kind of high-strength ageing MS glue, difference from example 1 is that, the plasticising Agent is acetyl tributyl citrate.
This example additionally provides the preparation method of above-mentioned high-strength ageing MS glue, and step is similar to Example 1.
Embodiment 5
Embodiment 5 provides a kind of high-strength ageing MS glue, difference from example 1 is that, the plasticising Agent is tributyl citrate.
This example additionally provides the preparation method of above-mentioned high-strength ageing MS glue, and step is similar to Example 1.
Embodiment 6
Embodiment 6 provides a kind of high-strength ageing MS glue, difference from example 1 is that, the filler For gas-phase silica.
This example additionally provides the preparation method of above-mentioned high-strength ageing MS glue, and step is similar to Example 1.
Embodiment 7
Embodiment 7 provides a kind of high-strength ageing MS glue, difference from example 1 is that, the filler For silica white, mesh number is 500 mesh.
This example additionally provides the preparation method of above-mentioned high-strength ageing MS glue, and step is similar to Example 1.
Embodiment 8
Embodiment 8 provides a kind of high-strength ageing MS glue, difference from example 1 is that, the plasticising The parts by weight of agent are 200 parts.
This example additionally provides the preparation method of above-mentioned high-strength ageing MS glue, and step is similar to Example 1.
Embodiment 9
Embodiment 9 provides a kind of high-strength ageing MS glue, difference from example 1 is that, the plasticising The parts by weight of agent are 100 parts.
This example additionally provides the preparation method of above-mentioned high-strength ageing MS glue, and step is similar to Example 1.
Embodiment 10
Embodiment 10 provides a kind of high-strength ageing MS glue, difference from example 1 is that, the water removal The parts by weight of agent are 5 parts.
This example additionally provides the preparation method of above-mentioned high-strength ageing MS glue, and step is similar to Example 1.
Embodiment 11
Embodiment 11 provides a kind of high-strength ageing MS glue, difference from example 1 is that, the water removal The parts by weight of agent are 10 parts.
This example additionally provides the preparation method of above-mentioned high-strength ageing MS glue, and step is similar to Example 1.
Embodiment 12
Embodiment 12 provides a kind of high-strength ageing MS glue, same as Example 1.
This example additionally provides the preparation method of above-mentioned high-strength ageing MS glue, comprising the following steps:
A. mixing: silane modified polyether performed polymer, plasticizer, filler, deicer investment are weighed and is stirred kettle, stirring is mixed It closes 2 hours, vacuumizes, be warming up to 100 DEG C under agitation, kept for 2 hours;
B. it reacts: temperature in the kettle is down to 45 DEG C, be filled with nitrogen, catalyst is added, vacuumizes again, material is sufficiently stirred Afterwards, vacuum is released to normal pressure, is discharged filling to get finished product.
Performance evaluation
Tensile strength, elongation at break, elasticity is carried out to the obtained high-strength ageing MS glue of embodiment 1~12 to restore Rate, sag, exudative, the special ring performance test of tension-compression, reference standard are GB/T13477-1992 " construction sealing materials Test method ", standard test conditions is 23 ± 2 DEG C of temperature, relative humidity 45%~55%, and each embodiment prepares three examinations Part, test result are averaged, and are shown in Table 1.
Table 1
Example Tensile strength Elongation at break Elastic restoration ratio Sag Exudation amplitude Drawing-pressure performance
1 6.8MPa 996% 94% 0mm 0mm It is without exception
2 6.9MPa 1004% 95% 0mm 0mm It is without exception
3 6.7MPa 992% 93% 0mm 0mm It is without exception
4 5.5MPa 820% 85% 3mm 1.5mm Removing
5 6.0MPa 745% 80% 2mm 0mm Rupture
6 4.8MPa 633% 77% 4mm 3mm Removing rupture
7 5.6MPa 721% 81% 3mm 2mm Removing
8 4.5MPa 880% 86% 4mm 1.5mm It is without exception
9 5.2MPa 703% 78% 1mm 0mm Rupture
10 4.2MPa 755% 70% 1mm 0.5mm Rupture
11 6.3MPa 698% 66% 0mm 0mm Rupture
12 4.0MPa 547% 57% 5mm 3.5mm Removing rupture
By the performance test of embodiment 1~12 it is known that filler, plasticizer, deicer three synergistic effect Under, the MS glue in the present invention also has excellent elasticity, flexibility, resistance to ag(e)ing and displacement energy while ensure that high intensity Power;In addition, the plasticizer being more toxic to be replaced with to nontoxic plasticizer, realize environmentally protective, expands the present invention Use scope.
At last it is pointed out that the foregoing is merely illustrative of the preferred embodiments of the present invention, it is not intended to limit the invention, it is all at this Made any modifications, equivalent replacements, and improvements etc., should be included in protection model of the invention within the spirit and principle of invention Within enclosing.

Claims (10)

1. a kind of high-strength ageing MS glue, which is characterized in that by weight, prepare raw material and include at least: is silane-modified 80~120 parts of polyethers performed polymer, 100~180 parts of plasticizer, 70~100 parts of filler, 0.2~5 part of catalyst, deicer 1~10 Part.
2. high-strength ageing MS glue as described in claim 1, which is characterized in that the pressure of the silane modified polyether performed polymer Stream viscosity is 10~30s/10g.
3. high-strength ageing MS glue as described in claim 1, which is characterized in that the silane modified polyether performed polymer has 2 A or 3 end alkoxies.
4. high-strength ageing MS glue as described in claim 1, which is characterized in that the plasticizer is selected from phthalic acid One of ester, fatty group dibasic acid, epoxy acid ester, citrate, phosphate or a variety of mixing.
5. high-strength ageing MS glue as claimed in claim 3, which is characterized in that the citrate is selected from lemon triethylenetetraminehexaacetic acid One of ester, tributyl citrate, trioctyl lemon acid, tributyl 2-acetylcitrate, acetyl tributyl citrate are a variety of Mixing.
6. high-strength ageing MS glue as described in claim 1, which is characterized in that the filler is selected from nanometer calcium carbonate, gas One of phase white carbon black, powdered whiting, carbon black, silica white, titanium dioxide, nano aluminium oxide or a variety of mixing.
7. high-strength ageing MS glue as described in claim 1, which is characterized in that the catalyst is selected from stannous octoate, fourth One of sour tin, dibutyltin diacetate, two sad dibutyl tins, chelating tin, dibutyl tin dilaurate, trialkylamine or A variety of mixing.
8. high-strength ageing MS glue as described in claim 1, which is characterized in that the deicer is selected from vinyl trimethoxy Base silane, vinyltriethoxysilane, vinyl three (2- methoxy ethoxy) silane, 3- (methacryloxypropyl) propyl three One of methoxy silane or a variety of mixing.
9. high-strength ageing MS glue as described in claim 1, which is characterized in that by weight, described to prepare raw material also Include 1~10 part of pigment, 0.1~5 part of ultraviolet absorber, 0.1~5 part of light stabilizer.
10. a kind of preparation method of high-strength ageing MS glue as described in claim 1, which is characterized in that including following step It is rapid:
A. mixing: plasticizer, filler, deicer investment are weighed and is stirred kettle, is stirred 0.5~1 hour, silane is added and changes Property polyethers performed polymer continue to be stirred until homogeneous, vacuumize, be warming up to 90~110 DEG C under agitation, kept for 1~3 hour;
B. it reacts: temperature in the kettle is down to 40~50 DEG C, be filled with nitrogen, catalyst is added, vacuumizes again, material is sufficiently stirred Afterwards, vacuum is released to normal pressure, is discharged filling to get finished product.
CN201910373443.8A 2019-05-07 2019-05-07 A kind of high-strength ageing MS glue and preparation method thereof Pending CN110205073A (en)

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Cited By (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN111394035A (en) * 2020-05-08 2020-07-10 湖北回天新材料股份有限公司 High-strength transparent nail-free glue and preparation method thereof
CN111777978A (en) * 2020-05-11 2020-10-16 福建俊达装配材料有限公司 Non-aging green and environment-friendly MS glue and preparation method thereof
CN113637443A (en) * 2020-05-11 2021-11-12 福建俊达装配材料有限公司 High-elongation MS (Murashige & Skoog) adhesive and preparation method thereof
CN114525101A (en) * 2022-02-21 2022-05-24 武汉比邻科技发展有限公司 Silane modified polyether sealant with low modulus and high elastic recovery rate and preparation method thereof
CN115926710A (en) * 2022-11-25 2023-04-07 广州市高士实业有限公司 Preparation of brightening glue

Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US6183593B1 (en) * 1999-12-23 2001-02-06 Closure Medical Corporation 1,1-disubstituted ethylene adhesive compositions containing polydimethylsiloxane
CN104004488A (en) * 2014-04-14 2014-08-27 江苏嘉娜泰有机硅有限公司 Environment friendly silicyl-terminated acrylic ester modified polyurethane electronic sealant
CN106987223A (en) * 2017-04-19 2017-07-28 常熟市恒信粘胶有限公司 Polyether-modified structure sealant of high intensity and preparation method thereof

Patent Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US6183593B1 (en) * 1999-12-23 2001-02-06 Closure Medical Corporation 1,1-disubstituted ethylene adhesive compositions containing polydimethylsiloxane
CN104004488A (en) * 2014-04-14 2014-08-27 江苏嘉娜泰有机硅有限公司 Environment friendly silicyl-terminated acrylic ester modified polyurethane electronic sealant
CN106987223A (en) * 2017-04-19 2017-07-28 常熟市恒信粘胶有限公司 Polyether-modified structure sealant of high intensity and preparation method thereof

Cited By (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN111394035A (en) * 2020-05-08 2020-07-10 湖北回天新材料股份有限公司 High-strength transparent nail-free glue and preparation method thereof
CN111777978A (en) * 2020-05-11 2020-10-16 福建俊达装配材料有限公司 Non-aging green and environment-friendly MS glue and preparation method thereof
CN113637443A (en) * 2020-05-11 2021-11-12 福建俊达装配材料有限公司 High-elongation MS (Murashige & Skoog) adhesive and preparation method thereof
CN114525101A (en) * 2022-02-21 2022-05-24 武汉比邻科技发展有限公司 Silane modified polyether sealant with low modulus and high elastic recovery rate and preparation method thereof
CN114525101B (en) * 2022-02-21 2023-08-01 武汉比邻科技发展有限公司 Low-modulus high-elastic recovery rate silane modified polyether sealant and preparation method thereof
CN115926710A (en) * 2022-11-25 2023-04-07 广州市高士实业有限公司 Preparation of brightening glue

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Application publication date: 20190906