CN106833480A - A kind of fire retardant elastic adhesive of double-component normal temperature cure and preparation method thereof - Google Patents
A kind of fire retardant elastic adhesive of double-component normal temperature cure and preparation method thereof Download PDFInfo
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- CN106833480A CN106833480A CN201710032475.2A CN201710032475A CN106833480A CN 106833480 A CN106833480 A CN 106833480A CN 201710032475 A CN201710032475 A CN 201710032475A CN 106833480 A CN106833480 A CN 106833480A
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- 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
- C09J171/00—Adhesives 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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- 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
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- 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
- C09J11/06—Non-macromolecular additives organic
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- 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
- C09J11/08—Macromolecular additives
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- 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
- C09J163/00—Adhesives based on epoxy resins; Adhesives based on derivatives of epoxy resins
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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
- C08K2201/00—Specific properties of additives
- C08K2201/011—Nanostructured additives
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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
- C08K2201/00—Specific properties of additives
- C08K2201/014—Additives containing two or more different additives of the same subgroup in C08K
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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
- C08L2201/00—Properties
- C08L2201/02—Flame or fire retardant/resistant
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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
- C08L2205/00—Polymer mixtures characterised by other features
- C08L2205/02—Polymer mixtures characterised by other features containing two or more polymers of the same C08L -group
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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
- 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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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- 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
- C08L2205/035—Polymer mixtures characterised by other features containing three or more polymers in a blend containing four or more polymers in a blend
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Abstract
The present invention discloses a kind of fire retardant elastic adhesive of double-component normal temperature cure, and it is made up of component A and B component in mass ratio 3~4: 1；Wherein component A includes the component of following parts by weight：Silane-terminated polyether, epoxy resin, plasticizer, inorganic powder material, ultra-violet absorber, fire retardant；The B component includes the component of following parts by weight：Organotin catalysts, organic amine, inorganic powder material, diluent.Two ingredient elastic adhesive of the invention, due to having used silane-terminated polyether performed polymer, the material such as adapted bisphenol A epoxide resin, Polyamines Curing Agents of Epoxy Resins is adjustable with solidification temperature, hardening time is adjustable, after solidification adhesive strength it is high, it is elastic good the characteristics of.There is excellent fire-retardant and ageing-resistant performance simultaneously.Need not heat up dehydrating operations in adhesive A of the invention, B component preparation process, simple production process less demanding to filler water content, and product shelf life is more than 6 months, meets actual demand.
Description
Technical field
The present invention relates to adhesive area, more particularly to a kind of double-component normal temperature containing silane-terminated polyether performed polymer is consolidated
The fire retardant elastic adhesive of change.
Background technology
Before the sixties in last century, polyurethane is mainly in the widely used liquid sealant of building trade, polythiaether and
Organosilicon.It is more excellent that later stage seventies Japan's clock deep pool chemical industry (being now renamed as KANEKA Co., Ltd) develops performance
Polyether-type fluid sealant, input industrial production in 1978, obtaining within 1980 Japanese polymer science can approve that nineteen eighty-two puts on market i.e.
Cause great concern.Its base polymer because of end for methoxy silane is referred to as terminal groups modification silane polymer, its main chain knot
Structure is polyoxypropylene, i.e. PPE (Polypropylene ether) (also having referred to as PPO or PPG), also has referred to as MS to gather at present
Compound.Because its excellent performance is widely popularized in Japanese architecture industry.Its usage amount occupies more than organosilicon sealant within 1992
Second, nineteen ninety-five exceedes the kind that polyurethane turns into consumption maximum in building sealant first.Start within 1997 in Europe and U.S.
State is set up factories production, and its production technology, formula technique is increasingly mature, and in industry, building materials, the field such as automobile is developed on an unprecedented scale.
With polyurethane, organosilicon is compared with polythiaether material, and MS polymer has advantage following prominent：
(1) stability is preserved fabulous.
(2) viscosity is relatively low compared with the polyurethane of equivalent molecule amount, can not use or use plasticizer less, in equivalent viscosities
Under can fill more fillers, reduces cost.
(3) there is good adhesive force to many materials, it is applied widely.
(4) against weather is good, and the physical property at initial stage is maintained in the outdoor exposure fluid sealant of 20 years, without obvious
Deterioration, experienced the test of time.
(5) surface has coating character (Paintability) after solidifying, unlike organosilicon sealant repels coating.
(6) environment-friendly, the micromolecular compound for not discharging pollution environment (can gradually discharge after silicone sealant adhesive curing
Cyclic dimethylsiloxane, so that the greasy dirt in adsorbing air is caused formed around fluid sealant obvious black pollution thing).
(7) curing rate is fast, and will not being bubbled in solidification process, (reaction of moisture in polyurethane and air can usually be discharged
Blown with carbon dioxide).
(8) low temperature operability is good, with good thixotropy, is easily extruded from coating gun, it might even be possible to sprayed using spray gun
Apply (Spray).
(9) solidfied material has good physical and mechanical properties.
Although MS polymer has the advantages that so many, it is widely applied in fluid sealant field, as adhesive
Still the industrial rigors to adhesive strength can not be met.As industrial adhesive except that must have good bonding strong
Degree (including shearing strength and peel strength), shock resistance, to the engineering plastics commonly used, rubber, metal, ceramics are waited with good
Good adhesive force, it is impossible to produce interface peel, in addition it is also necessary to high-temp resisting high-humidity resisting environment, cold-resistant thermal cycle is water-fast, solvent resistant and chemistry
Product corrode.Polyethers non-polar conformations in MS polymer determine that its cohesive energy is relatively low, though take inorganic filler reinforcement and
The means such as addition adhesion promoter cannot still obtain the elastic attachment adhesive of high intensity.
To solve this problem, MS polymer is modified using epoxy resin.Its principle is using epoxy resin
The highly polar deficiency to make up MS polymer cohesive energys.There is two kinds of reaction mechanisms (Dual-cure), i.e. ring when the method solidifies
The curing reaction of oxygen tree fat and the moisture-curing of MS polymer, island phase separation structure can be formed after solidification has excellent physics
Mechanical performance.In traditional handicraft the two component adhesive be using MS resins and epoxy resin as a main body for component,
The curing catalysts of MS polymer add in the epoxy and the curing agent of epoxy resin is added in MS resins.Due to MS polymer
Reaction can be produced with the curing agent of most of epoxy resin, so as to directly solidify, and then influence the storage of MS polymers compositions steady
It is qualitative.For example, number of patent application is CN201410553164.7, patent name is《A kind of epoxy resin modification double-component end silicon
Alkyl, polyether adhesive》Patent of invention, it discloses using epoxy resin modification MS polymer thinking.In that patent,
The curing agent of epoxy resin is curing agent diethylenetriamine etc., after the curing agent and MS mixed with polymers, resulting MS polymerizations
Thing component is only capable of preserving 2-3 days time.And the method for also finding no effect at present can solve MS polymer in Bi-component adhesive
The preservation problem of component.
As can be seen here, the selection of dual-component silicane end capped polyether performed polymer adhesive preparation process epoxy resin curing agent
It is particularly important key technology, i.e., ensures that product stability meets the requirement of cold curing again, its characteristic is limited significantly
The range of choice of curing agent.
In addition, be added in for the curing agent of epoxy resin by existing adhesive is prepared into a kind of component in MS resins, in order to ensure
The stability of storage, need to carry out dehydrating operations under elevated temperature in vacuo, and operating condition is harsh, high cost, be difficult to realize big rule
The production of mould.
The content of the invention
To solve prior art problem, present invention offer is a kind of to ensure that product stability can meet wanting for cold curing again
Fire retardant elastic adhesive of double-component normal temperature cure asked and preparation method thereof.
Therefore, inventor providing following technical scheme：
A kind of fire retardant elastic adhesive of double-component normal temperature cure, it is by 3~4: 1 group in mass ratio of component A and B component
Into；Wherein component A includes the component of following parts by weight：
The B component includes the component of following parts by weight：
The present invention uses above-mentioned technical proposal, and silane-terminated polyether and epoxy resin are placed in component A, and asphalt mixtures modified by epoxy resin
The curing agent organic amine of fat and the curing catalysts organotin catalysts of silane-terminated polyether are placed in another B component, by silane
End capped polyether separates in different component with the curing agent organic amine of epoxy resin, so as to avoid the curing agent of epoxy resin organic
Amine solidifies silane-terminated polyether, it is ensured that the stability of silane-terminated polyether, and then ensures the stability of component A.
Meanwhile, the present invention also innovatively adds fire retardant in elastic attachment adhesive, hinders modified elastic attachment adhesive
Combustion property is greatly reinforced, and can be applied in the building trade material higher to flame-retardancy requirements, greatly expand the application of elastic attachment adhesive
Scope.
Further, the silane-terminated polyether is：Relative molecular mass in 12000~30000 one or two with
The mixture of upper silane-terminated polyether.In the present invention, in order to realize the optimum performance of elastic attachment adhesive, not only consider only to use one
Plant silane-terminated polyether of the relative molecular mass in 12000~30000, it is also contemplated that by two or more relative point
Silane-terminated polyether of the protonatomic mass in 12000~30000 be mixed with elastic attachment adhesive, the elasticity of regulation adhesive and
Intensity, makes the properties of elastic attachment adhesive reach most preferably.
Further, the epoxy resin is one of the following or two kinds of mixing：Bisphenol A epoxide resin or phenol aldehyde type ring
The epoxide equivalent of oxygen tree fat, the bisphenol A epoxide resin or phenol aldehyde type epoxy resin is 210~240g/eq or 184~190g/
eq。
Further, the inorganic particle filler in the component A is one of the following or two or more mixing：Lightweight carbon
Sour calcium, nanometer grade silica, titanium dioxide and carbon black；Inorganic particle filler in the B component for one of the following or
Two or more mixing：Precipitated calcium carbonate, titanium dioxide or nanometer grade silica.By the filling of inorganic particle filler,
In the case of not influenceing elastic attachment adhesive performance, the cost of elastic attachment adhesive can be substantially reduced.
Further, the fire retardant in the component A is one of the following or two or more mixing：Trichloroethyl phosphoric acid
Ester, triaryl phosphate, trichlorine propyl phosphate or methyl-phosphoric acid dimethyl ester.The present invention adds above-mentioned anti-flammability, can be with silicon
Alkane end capped polyether performed polymer, epoxy resin are mixed with adhesive so that adhesive possesses anti-flammability, meet the spy of some industries
It is different to require, expand range of application.
Further, the organotin catalysts in the B component are one of the following：Stannous octoate, the fourth of tin dilaurate two
Ji Xi, dibutyltin diacetate or two (octadecyl sulphur) dibutyl tins.Organotin catalysts of the present invention, in component A
After being mixed to form adhesive with B component, adhesive can be promoted to solidify, shorten the hardening time of adhesive.
Further, the organic amine in the B component is one of the following or two or more mixing：N, N- dimethyl benzene
Amine, 2- dimethylaminomethylphenols (DMP-10), 2,4- bis- (dimethylamino methyl) phenol (DMP-20), (diformazans of 2,4,6- tri-
Amino methyl) phenol (DMP-30) or low molecular polyamides.In the present invention, selected above-mentioned organic amine catalyst is non-
Volatile organic amine catalyst, so as to avoid the volatile shortcoming of low-molecular weight amines, it is to avoid in production and work progress
The middle penetrating odor caused by low-molecular weight amines volatility.The present invention uses non-volatile organic amine catalyst, system
Standby adhesive is applied for production and provides good working environment with workman person without any excitant taste.
Further, the plasticizer in the component A is one of the following or two kinds of mixing：Aliphatic dibasic acid ester
Or phenyl alkylsulf class.
Further, the diluent in the B component is PPG of the molecular weight more than 2000.
Further, the ultra-violet absorber in the component A is commercially available prod, is bought in German BASF joint-stock company,
Product grade is Tinuvin327 or Tinuvin765.In the present invention, add ultra-violet absorber can avoid adhesive due to light,
The degraded that weather causes.
The present invention also provides a kind of preparation method of the fire retardant elastic adhesive of double-component normal temperature cure, the preparation method
Comprise the following steps：
Prepare component A：By silane-terminated polyether, epoxy resin, plasticizer, inorganic powder material, ultraviolet absorber and resistance
Combustion agent is added in planet stirring kettle, is stirred at room temperature uniformly, and discharging is packaged to be component A；
Prepare B component：By organotin catalysts, organic amine, inorganic particle filler and diluent in agitator at room temperature
Well mixed, discharging is packaged to be B component；
Mixing：Component A and B component in mass ratio 3~4: 1 are well mixed and obtain adhesive.
The solidification temperature of invention adhesive is 0-25 DEG C, and hardening time is 0.5-24 hours.During according to specific solidification
Environment temperature, adjusts hardening time.
The present invention is individually enclosed in difference and deposits in a device after component A and B component is prepared, when it is desired to be used,
Just carry out blend step.
In the present invention, due to silane-terminated polyether, epoxy resin are placed in same component i.e. component A, such component A
In preparation process, silane-terminated polyether and epoxy resin are greatly simplified without carrying out dehydrating operations under elevated temperature in vacuo
Operating procedure, reduces the requirement of preparation condition (such as temperature and vacuum), need to only be stirred at room temperature and uniformly can obtain A groups
Point, substantially reduce production cost.And the curing agent and other auxiliary material components of silane-terminated polyether and epoxy resin also need to only pass through
Another component i.e. B component is formed by being stirred at room temperature so that the preparation condition of whole adhesive is simple, product cost reduction, and
It is convenient to realize big expansion large-scale production.
Advantages of the present invention has：
1st, be placed in same component i.e. component A for silane-terminated polyether and epoxy resin by the present invention, by silane-terminated polyether
Curing catalysts and the curing agent of epoxy resin be placed in another set point i.e. B component, so as to avoid silane in the prior art
End capped polyether is solidified by the curing agent of epoxy resin and causes the not enough problem of stability, so as to improve product elasticity of the present invention
The stability of adhesive.
2nd, the present invention adds anti-flammability in elastic attachment adhesive, assigns elastic attachment adhesive fire resistance so that elasticity is gluing
Agent meets the requirement of some special industries, greatly expands the range of application of elastic attachment adhesive.
3rd, elastic attachment adhesive preparation condition of the invention is simple, without carrying out high-temperature vacuum dehydrating operations, in room temperature normal pressure
It is lower to prepare, the production cost of product is substantially reduced, and large-scale production is expanded greatly in convenient realization.
Specific embodiment
To describe technology contents of the invention, structural feature, the objects and the effects in detail, below in conjunction with implementation method
It is explained in detail.
The present invention provides a kind of fire retardant elastic adhesive of double-component normal temperature cure, its by component A and B component in mass ratio
3~4: 1 composition；Wherein component A includes the component of following parts by weight：
The B component includes the component of following parts by weight：
The present invention also provides a kind of preparation method of the fire retardant elastic adhesive of double-component normal temperature cure, the preparation method
Comprise the following steps：
Prepare component A：By silane-terminated polyether, epoxy resin, plasticizer, inorganic powder material, ultraviolet absorber and resistance
Combustion agent is added in planet stirring kettle, is stirred at room temperature uniformly, and discharging is packaged to be component A；
Prepare B component：By organotin catalysts, organic amine, inorganic particle filler and diluent in agitator at room temperature
Well mixed, discharging is packaged to be B component；
Mixing：Component A and B component in mass ratio 3~4: 1 are well mixed and obtain adhesive, the solidification temperature of adhesive
It it is 0-25 DEG C, hardening time is 0.5-24 hours.
Embodiment 1
A kind of preparation method of the fire retardant elastic adhesive of double-component normal temperature cure, it is comprised the following steps：
1) component A is prepared：First each component is weighed by formula as below：
The relative molecular mass of the silane-terminated polyether is 12000 methyl dimethoxy epoxide silicyl polyethers.
The epoxy resin is bisphenol A epoxide resin E-44, and the epoxide equivalent of the bisphenol A epoxide resin is 210g/eq.
The plasticizer is phenyl alkylsulf, specially pentadecyl sulphonyl phenyl ester (T-50 petroleum esters).
The inorganic particle filler is precipitated calcium carbonate.
The fire retardant is trichloroethyl phosphate.
The ultra-violet absorber is purchased in German BASF joint-stock company, and product grade is Tinuvin327.
Silane-terminated polyether, epoxy resin, plasticizer, inorganic powder material, ultraviolet absorber and fire retardant are added again
In planet stirring kettle, it is stirred at room temperature uniformly, discharging is packaged to be component A；
2) B component is prepared：First each component is weighed by formula as below：
The organotin catalysts are dibutyl tin laurate.
The organic amine is N, accelerine.
The inorganic particle filler is precipitated calcium carbonate.
The diluent is the PPG of molecular weight 2500, specially DL-2000D.
Organotin catalysts, organic amine, inorganic particle filler and diluent are well mixed at room temperature in agitator again,
Discharging is packaged to be B component；
The component A and B component are prepared and finish packaging preservation respectively, when it is desired to be used, then the mixing behaviour for carrying out step 3
Make.
3) mix：Component A and B component in mass ratio 4: 1 are well mixed and obtain adhesive.
Embodiment 2
A kind of preparation method of the fire retardant elastic adhesive of double-component normal temperature cure, it is comprised the following steps：
1) component A is prepared：First each component is weighed by formula as below：
The relative molecular mass of the silane-terminated polyether is 30000 trimethoxysilyl polyethers.
The epoxy resin is phenol aldehyde type epoxy resin F-44, and the epoxide equivalent of the phenol aldehyde type epoxy resin is 240g/
eq。
The plasticizer is aliphatic dibasic acid ester, specially dioctyl adipate.
The inorganic particle filler is precipitated calcium carbonate and titanium dioxide in mass ratio 2:1 mixture.
The fire retardant is triaryl phosphate.
The ultra-violet absorber is purchased in German BASF joint-stock company, and product grade is Tinuvin327.
Silane-terminated polyether, epoxy resin, plasticizer, inorganic powder material, ultraviolet absorber and fire retardant are added again
In planet stirring kettle, it is stirred at room temperature uniformly, discharging is packaged to be component A；
2) B component is prepared：First each component is weighed by formula as below：
The organotin catalysts are stannous octoate.
The organic amine is 2- dimethylaminomethylphenols (DMP-10).
The inorganic particle filler is precipitated calcium carbonate and titanium dioxide in mass ratio 2:1 mixture.
The diluent is the PPG of molecular weight 3000.
Organotin catalysts, organic amine, inorganic particle filler and diluent are well mixed at room temperature in agitator again,
Discharging is packaged to be B component；
The component A and B component are prepared and finish packaging preservation respectively, when it is desired to be used, then the mixing behaviour for carrying out step 3
Make.
3) mix：Component A and B component in mass ratio 3: 1 are well mixed and obtain adhesive.
Embodiment 3
A kind of preparation method of the fire retardant elastic adhesive of double-component normal temperature cure, it is comprised the following steps：
1) component A is prepared：First each component is weighed by formula as below：
The relative molecular mass of the silane-terminated polyether is 20000 dimethoxy triethoxy mixing end-blocking monosilane
Base polyethers；
The epoxy resin is bisphenol A epoxide resin E-54, and the epoxide equivalent of the bisphenol A epoxide resin is 184g/eq.
The plasticizer is aliphatic dibasic acid ester and phenyl alkylsulf class in mass ratio 1:1 mixture, specifically
It is dioctyl adipate and pentadecyl sulfonic acid toluene ester (M-50).
The inorganic particle filler is titanium dioxide and carbon black in mass ratio 1:1 mixture.
The fire retardant is triaryl phosphate.
The ultra-violet absorber is purchased in German BASF joint-stock company, and product grade is Tinuvin327.
Silane-terminated polyether, epoxy resin, plasticizer, inorganic powder material, ultraviolet absorber and fire retardant are added again
In planet stirring kettle, it is stirred at room temperature uniformly, discharging is packaged to be component A；
2) B component is prepared：First each component is weighed by formula as below：
The organotin catalysts are two (octadecyl sulphur) dibutyl tins.
The organic amine is 2,4- bis- (dimethylamino methyl) phenol (DMP-20).
The inorganic particle filler is precipitated calcium carbonate and nanometer grade silica in mass ratio 1:1 mixture.
The diluent is the PPG of molecular weight 3500, specially polyethers 3050.
Organotin catalysts, organic amine, inorganic particle filler and diluent are well mixed at room temperature in agitator again,
Discharging is packaged to be B component；
The component A and B component are prepared and finish packaging preservation respectively, when it is desired to be used, then the mixing behaviour for carrying out step 3
Make.
3) mix：Component A and B component in mass ratio 3: 1 are well mixed and obtain adhesive.
Embodiment 4
A kind of preparation method of the fire retardant elastic adhesive of double-component normal temperature cure, it is comprised the following steps：
1) component A is prepared：First each component is weighed by formula as below：
The relative molecular mass of the silane-terminated polyether is 18000 triethoxysilyl polyethers；
The epoxy resin is phenol aldehyde type epoxy resin F-51, and the epoxide equivalent of the phenol aldehyde type epoxy resin is 190g/
eq。
The plasticizer is phenyl alkylsulf class, specially pentadecyl sulphonyl phenyl ester (T-50 petroleum esters).
The inorganic particle filler is nanometer grade silica；
The fire retardant is trichlorine propyl phosphate.
The ultra-violet absorber is purchased in German BASF joint-stock company, and product grade is Tinuvin765.
Silane-terminated polyether, epoxy resin, plasticizer, inorganic powder material, ultraviolet absorber and fire retardant are added again
In planet stirring kettle, it is stirred at room temperature uniformly, discharging is packaged to be component A；
The component A and B component are prepared and finish packaging preservation respectively, when it is desired to be used, then the mixing behaviour for carrying out step 3
Make.
2) B component is prepared：First each component is weighed by formula as below：
The organotin catalysts are dibutyltin diacetate.
The organic amine is 2,4,6- tri- (dimethylamino methyl) phenol (DMP-30).
The inorganic particle filler is nanometer grade silica.
The diluent is the PPG of molecular weight 4000, specially PPG-4000.
Organotin catalysts, organic amine, inorganic particle filler and diluent are well mixed at room temperature in agitator again,
Discharging is packaged to be B component；
3) mix：Component A and B component in mass ratio 4: 1 are well mixed and obtain adhesive.
Embodiment 5
A kind of preparation method of the fire retardant elastic adhesive of double-component normal temperature cure, it is comprised the following steps：
1) component A is prepared：First each component is weighed by formula as below：
The silane-terminated polyether is two kinds of mixing of different relative molecular mass silane-terminated polyethers.Specifically, described
Silane-terminated polyether is by methyl dimethoxy epoxide silicyl polyethers that relative molecular mass is 12000 and relative molecular mass
25000 trimethoxysilyl polyethers in mass ratio 1:1 is mixed.
The epoxy resin is bisphenol A epoxide resin E-44B and phenol aldehyde type epoxy resin F-51 in mass ratio 1:1 mixing
Thing, the epoxide equivalent of the bisphenol A epoxide resin is 220g/eq；The epoxide equivalent of the phenol aldehyde type epoxy resin is 186g/
eq。
The plasticizer is aliphatic dibasic acid ester, specially dioctyl adipate.
The inorganic particle filler precipitated calcium carbonate and nanometer grade silica in mass ratio 2:1 mixture.
The fire retardant is methyl-phosphoric acid dimethyl ester.
The ultra-violet absorber is purchased in German BASF joint-stock company, and product grade is Tinuvin765.
Silane-terminated polyether, epoxy resin, plasticizer, inorganic powder material, ultraviolet absorber and fire retardant are added again
In planet stirring kettle, it is stirred at room temperature uniformly, discharging is packaged to be component A；
2) B component is prepared：First each component is weighed by formula as below：
The organotin catalysts are dibutyl tin laurate.
The organic amine is low molecular polyamides, specially polyamide 6 50.
The inorganic particle filler is titanium dioxide.
The diluent is the PPG of molecular weight 3000, specially polyethers 3050.
Organotin catalysts, organic amine, inorganic particle filler and diluent are well mixed at room temperature in agitator again,
Discharging is packaged to be B component；
The component A and B component are prepared and finish packaging preservation respectively, when it is desired to be used, then the mixing behaviour for carrying out step 3
Make.
3) mix：Component A and B component in mass ratio 3: 1 are well mixed and obtain adhesive.
Embodiment 6
A kind of preparation method of the fire retardant elastic adhesive of double-component normal temperature cure, it is comprised the following steps：
1) component A is prepared：First each component is weighed by formula as below：
The silane-terminated polyether is mixture, specifically, silane-terminated polyether is for relative molecular mass is 15000 three
Triethoxysilyl polyethers and relative molecular mass be 30000 trimethoxysilyl polyethers by quality 2:1 mixing
Thing.
The epoxy resin is bisphenol A epoxide resin WSR634 and phenol aldehyde type epoxy resin F-51 in mass ratio 2:1 it is mixed
Close, the epoxide equivalent of the bisphenol A epoxide resin is 230g/eq, and the epoxide equivalent of the phenol aldehyde type epoxy resin is 190g/
eq。
The plasticizer is aliphatic dibasic acid ester, specially Dioctyl Glutaricate.
The inorganic particle filler is precipitated calcium carbonate；
The fire retardant is trichloroethyl phosphate and triaryl phosphate in mass ratio 2:1 mixture.
The ultra-violet absorber is purchased in German BASF joint-stock company, and product grade is Tinuvin765.
Silane-terminated polyether, epoxy resin, plasticizer, inorganic powder material, ultraviolet absorber and fire retardant are added again
In planet stirring kettle, it is stirred at room temperature uniformly, discharging is packaged to be component A；
2) B component is prepared：First each component is weighed by formula as below：
The organotin catalysts are stannous octoate.
The organic amine is 2- dimethylaminomethylphenols (DMP-10) and (dimethylamino methyl) phenol of 2,4- bis- DMP-
20 in mass ratio 1:1 mixture.
The inorganic particle filler is precipitated calcium carbonate.
The diluent is the PPG of molecular weight 3000, specially polyethers 303.
Organotin catalysts, organic amine, inorganic particle filler and diluent are well mixed at room temperature in agitator again,
Discharging is packaged to be B component；
Component A and B component are prepared and finish packaging preservation respectively, when it is desired to be used, then the married operation for carrying out step 3.
3) mix：Component A and B component in mass ratio 3: 1 are well mixed and obtain adhesive, it is adaptable to the elasticity of structural member
Sealing and bonding.
The solidification temperature of adhesive prepared by the present invention is 0-25 DEG C, and hardening time is 0.5-24 hours.Work as solidification temperature
When higher, then hardening time shortening, when solidification temperature is relatively low, hardening time extension.Specifically can according to it is actually used when ring
Border temperature is adjusted hardening time.For example, when solidification temperature is 0 DEG C, hardening time can be 24 hours, when solidification temperature is
At 25 DEG C, hardening time can be 0.5 hour；When solidification temperature is 15 DEG C, hardening time can be 10 hours.Therefore, Yong Hu
During use, hardening time can be adjusted according to specific environment temperature.
Embodiment 7
The embodiment be with reference to embodiment, the number of patent application mentioned with background technology as CN201410553164.7,
Patent name is《A kind of epoxy resin modification double-component silyl-terminated polyether adhesive》Patent of invention embodiment 10 for ginseng
According to.
Each component is weighed by the data of table 1：
The each component addition of 1 embodiment of table 7
By in mass ratio the 1 of component A and B component:1 mixing, obtains adhesive, and the specific surface area of aerosil is：
200m2/g.Experiment finds the component A for being prepared (without vacuum dehydration) in this way, and viscosity is significantly increased after placing 12 hours,
24 was as a child self-curing, into rubber-like.Afterwards it has been investigated that silyl-terminated polyether is in simple and diethylenetriamine, triethylene four
After the mixing such as amine, the short time after significant change, but a couple of days without itself reacting solidification, it is impossible to preservation for a long time.
Analysis of test results
1st, component A tenability time is detected.
As shown in Table 1, the fire retardant elastic adhesive component A for being prepared by the inventive method has good storage stability,
Can at least preserve more than 210 days, meet the requirement of product marketization.
2nd, adhesive prepared by embodiment 1-7 is carried out into performance detection respectively, the performance of detection has：Tensile strength, fracture
Elongation, tensile shear strength, 180 ° of peel strengths, hardness and anti-flammabilitys.
Wherein, tensile strength and elongation at break are tested with reference to GB GB/T 528-2009；Tensile shear strength is joined
GB GB/T 7124-2008 are examined to be tested；180 ° of peel strengths are tested with reference to GB GB/T 2790-1995；Burning
Performance is tested with reference to GB GB/T10707-2008, using vertical combustion；Hardness refers to GB GB/T 3398.2-
2008 are tested.Specific testing result is shown in Table 2.
Each performance test results of embodiment 1-7 of table 2
The made elastic attachment adhesive main purpose of the present invention be in order to be applied to the bonding of sizing variable building, in order to
Increase elasticity, formula epoxy resin content is on the low side.With reference to elastic binder relevant criterion (JC/T 881-2001) tensile strength
>0.6MPa can meet requirement.From the testing result of table 2, the fire retardant elastic binding agent prepared by the present invention has good
Elasticity and fire resistance, disclosure satisfy that the use demand of association area.
The component A and B component prepared to embodiment 1 by preset ratio be mixed to form gluing after preserving 180 days
Agent, the performance detection of its work progress is as shown in table 3.The detection method of its each performance is same as mentioned above.
Adhesive work progress performance detection prepared by 3 embodiment of table 1
As shown in Table 3, the adhesive that prepared by the present invention is keeping normally using for 180 days, its performance and immediately after preparation 1-3
It is consistent, illustrates adhesive good stability of the invention, can at least stablize and preserve more than half a year.
Two ingredient elastic adhesive of the invention, due to having used silane-terminated polyether performed polymer, adapted bisphenol-A epoxy
The materials such as resin, Polyamines Curing Agents of Epoxy Resins, inorganic powder material, plasticizer, adjustable with solidification temperature, hardening time can
Adjust, after solidification adhesive strength it is high, it is elastic good the characteristics of.There is excellent fire-retardant and ageing-resistant performance simultaneously.It is of the invention gluing
Need not heat up dehydrating operations in agent A, B component preparation process, simple production process less demanding to filler water content, produce
Product Storage period is more than 6 months, meets actual demand.
Embodiments of the invention are the foregoing is only, scope of patent protection of the invention, every utilization is not thereby limited
Equivalent structure or equivalent flow conversion that present specification is made, or directly or indirectly it is used in other related technologies
Field, is included within the scope of the present invention.
Claims (10)
1. a kind of fire retardant elastic adhesive of double-component normal temperature cure, it is characterised in that：It is by component A and B component in mass ratio 3
~4: 1 composition；Wherein component A includes the component of following parts by weight：
The B component includes the component of following parts by weight：
2. the fire retardant elastic adhesive of double-component normal temperature cure according to claim 1, it is characterised in that：The silane envelope
End polyethers be：The mixture of one or more silane-terminated polyethers of the relative molecular mass in 12000~30000.
3. the fire retardant elastic adhesive of double-component normal temperature cure according to claim 1, it is characterised in that：The asphalt mixtures modified by epoxy resin
Fat is one of the following or two kinds of mixing：Bisphenol A epoxide resin or phenol aldehyde type epoxy resin, the bisphenol A epoxide resin
Or the epoxide equivalent of phenol aldehyde type epoxy resin is 210~240g/eq or 184~190g/eq.
4. the fire retardant elastic adhesive of double-component normal temperature cure according to claim 1, it is characterised in that the component A
In inorganic particle filler be one of the following or two or more mixing：Precipitated calcium carbonate, nanometer grade silica, dioxy
Change titanium and carbon black；Inorganic particle filler in the B component is one of the following or two or more mixing：Lightweight carbonic acid
Calcium, titanium dioxide or nanometer grade silica.
5. the fire retardant elastic adhesive of the double-component normal temperature cure described in a claim 1, it is characterised in that in the component A
Fire retardant be one of the following or two or more mixing：Trichloroethyl phosphate, triaryl phosphate, three chloropropyl phosphorus
Acid esters or methyl-phosphoric acid dimethyl ester.
6. the fire retardant elastic adhesive of the double-component normal temperature cure described in a claim 1, it is characterised in that in the B component
Organotin catalysts be one of the following：Stannous octoate, dibutyl tin laurate, dibutyltin diacetate or two (ten
Eight alkyl sulfides) dibutyl tin.
7. the fire retardant elastic adhesive of the double-component normal temperature cure described in a claim 1, it is characterised in that in the B component
Organic amine be one of the following or two or more mixing：N, accelerine, 2- dimethylaminomethylphenols, 2,4-
Two (dimethylamino methyl) phenol, (dimethylamino methyl) phenol of 2,4,6- tri- or low molecular polyamides.
8. the fire retardant elastic adhesive of double-component normal temperature cure according to claim 1, it is characterised in that the component A
In plasticizer be one of the following or two kinds of mixing：Aliphatic dibasic acid ester or phenyl alkylsulf class.
9. the fire retardant elastic adhesive of double-component normal temperature cure according to claim 1, it is characterised in that the B component
In diluent for molecular weight more than 2000 PPG.
10. the preparation method of the fire retardant elastic adhesive according to the described double-component normal temperature cure of one of claim 1~9, its
It is characterised by：The preparation method is comprised the following steps：
Prepare component A：By silane-terminated polyether, epoxy resin, plasticizer, inorganic powder material, ultraviolet absorber and fire retardant
Add in planet stirring kettle, be stirred at room temperature uniformly, discharging is packaged to be component A；
Prepare B component：Organotin catalysts, organic amine, inorganic particle filler and diluent are mixed at room temperature in agitator
Uniformly, discharging is packaged to be B component；
Mixing：Component A and B component in mass ratio 3~4: 1 are well mixed and obtain adhesive.
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Cited By (10)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN108048015A (en) * | 2017-12-26 | 2018-05-18 | 湖北回天新材料股份有限公司 | Wind electricity blade cover board bonding two-component silane modified polyether seal glue |
| CN108441158A (en) * | 2018-03-27 | 2018-08-24 | 广州机械科学研究院有限公司 | A kind of bi-component epoxy modified silane end capping polypropylene oxide fluid sealant and preparation method thereof |
| CN108795358A (en) * | 2018-07-11 | 2018-11-13 | 合肥同佑电子科技有限公司 | A kind of equipment machine room electronics fluid sealant |
| CN109251714A (en) * | 2018-08-16 | 2019-01-22 | 芮城华纳纳米材料有限公司 | A kind of high-strength bi-component Polyurethane Sealant for Laminated Glass and preparation method thereof |
| CN109266282A (en) * | 2018-09-10 | 2019-01-25 | 广州博邦化学科技有限责任公司 | A kind of compound silane modified polyether heat-conducting glue of one-component and preparation method thereof |
| CN109337630A (en) * | 2018-10-22 | 2019-02-15 | 广州市垠瀚能源科技有限公司 | A kind of two-component room temperature fast-curing antidetonation conductive structure adhesive preparation method |
| CN109467910A (en) * | 2018-10-31 | 2019-03-15 | 深圳市顾康力化工有限公司 | A kind of resistance to thermal-enhanced sealing hybrid material and preparation method thereof |
| CN110157376A (en) * | 2019-06-06 | 2019-08-23 | 广州市白云化工实业有限公司 | Transparent two-component silane modified polyether seal glue and preparation method thereof |
| CN113105860A (en) * | 2021-03-19 | 2021-07-13 | 上海康达化工新材料集团股份有限公司 | Ultrafast-curing flame-retardant bi-component epoxy modified silyl-terminated polymer adhesive, and preparation method and application thereof |
| CN115521739A (en) * | 2022-07-27 | 2022-12-27 | 东方雨虹民用建材有限责任公司 | Water-based water-resistant Bai Huanyang color sand ceramic tile joint mixture and preparation method thereof |
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| CN108048015A (en) * | 2017-12-26 | 2018-05-18 | 湖北回天新材料股份有限公司 | Wind electricity blade cover board bonding two-component silane modified polyether seal glue |
| CN108441158A (en) * | 2018-03-27 | 2018-08-24 | 广州机械科学研究院有限公司 | A kind of bi-component epoxy modified silane end capping polypropylene oxide fluid sealant and preparation method thereof |
| CN108795358A (en) * | 2018-07-11 | 2018-11-13 | 合肥同佑电子科技有限公司 | A kind of equipment machine room electronics fluid sealant |
| CN109251714A (en) * | 2018-08-16 | 2019-01-22 | 芮城华纳纳米材料有限公司 | A kind of high-strength bi-component Polyurethane Sealant for Laminated Glass and preparation method thereof |
| CN109266282A (en) * | 2018-09-10 | 2019-01-25 | 广州博邦化学科技有限责任公司 | A kind of compound silane modified polyether heat-conducting glue of one-component and preparation method thereof |
| CN109337630A (en) * | 2018-10-22 | 2019-02-15 | 广州市垠瀚能源科技有限公司 | A kind of two-component room temperature fast-curing antidetonation conductive structure adhesive preparation method |
| CN109467910A (en) * | 2018-10-31 | 2019-03-15 | 深圳市顾康力化工有限公司 | A kind of resistance to thermal-enhanced sealing hybrid material and preparation method thereof |
| CN110157376A (en) * | 2019-06-06 | 2019-08-23 | 广州市白云化工实业有限公司 | Transparent two-component silane modified polyether seal glue and preparation method thereof |
| CN113105860A (en) * | 2021-03-19 | 2021-07-13 | 上海康达化工新材料集团股份有限公司 | Ultrafast-curing flame-retardant bi-component epoxy modified silyl-terminated polymer adhesive, and preparation method and application thereof |
| CN115521739A (en) * | 2022-07-27 | 2022-12-27 | 东方雨虹民用建材有限责任公司 | Water-based water-resistant Bai Huanyang color sand ceramic tile joint mixture and preparation method thereof |
| CN115521739B (en) * | 2022-07-27 | 2024-02-02 | 东方雨虹民用建材有限责任公司 | Water-based water-resistant white epoxy colored sand tile joint mixture and preparation method thereof |
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