CN101298545A - Heat resisting anti-aging adhesive for construction - Google Patents
Heat resisting anti-aging adhesive for construction Download PDFInfo
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- CN101298545A CN101298545A CNA2008101229173A CN200810122917A CN101298545A CN 101298545 A CN101298545 A CN 101298545A CN A2008101229173 A CNA2008101229173 A CN A2008101229173A CN 200810122917 A CN200810122917 A CN 200810122917A CN 101298545 A CN101298545 A CN 101298545A
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Abstract
The invention relates to a heat resistant and aging resistant epoxy resin adhesive used for buildings, which is an epoxy resin adhesive modified by rosin resin; the invention also relates to a preparation method of the adhesive. The adhesive designed by the invention has good aging resistant and heat resistant properties.
Description
Technical field
The present invention relates to heat-resisting anti-aging epoxide resin type tackiness agent for building.
Background technology
The tackiness agent that is applicable to building trade should have following characteristics usually: 1) shearing resistance, compressive strength, tensile strength height; 2) can be at-40 ℃ of-+80 ℃ of following life-time service; 3) wet and heat ageing resistant is excellent, water tolerance is excellent; 4) easy to operate, curing speed is moderate.And in the building trade construction process, because envrionment temperature difference is bigger, generally change in 0-40 ℃, therefore, tackiness agent must adopt warm curing type.
Epoxyn has heat-resisting, weather-proof, water-fast, ageing-resistant, corrosion-resistant and unique characteristics such as bonding force, is widely used in building reinforce (for example all kinds of concrete structure reparations, reinforcing etc.), building slab gluing (for example bonding ceramic tile, wood floors, metal, decorative glass board etc.) etc. in the civil construction industry.But present epoxyn can not satisfy the above-mentioned requirements of building trade fully.
Though the coventional type epoxyn belongs to warm curing tackiness agent, very responsive to envrionment temperature, in the time of 0 ℃, most of adhesive solidifications are very slow, even do not solidify, and in the time of 30 ℃-40 ℃, curing speed is too fast again, and gel time only at tens minutes, can't be constructed usually at all.In addition, common room temperature curing epoxy resin adhesive stick exists cured article fragility big, and curing speed is with shortcomings such as temperature sensitives.For improving the fragility of epoxyn, the method for toughening of present common employing is to add softening agent in epoxy resin ingredient, because softening agent and solidifying agent can not crosslinking reactions, softening agent is free in the epoxy curing systems, can show preferably toughness in a short time but cohesive strength is low, behind life-time service, softening agent is secreted, cause that bonding failure and tackiness agent shrink, toughness descends, and ageing resistance is poor.Modal method for toughening is to add nbr carboxyl terminal (CTBN), thiorubber.The CTBN toughened epoxy resin adhesive has toughening effect and higher bonding strength preferably, but cost is higher.The poly-toughness reinforcing rubber-toughened epoxy resin tackiness agent of sulphur, bonding strength is relatively poor and have very big irritating smell, uses extremely inconvenient.The adding of above-mentioned in addition two kinds of toughner all makes the activity of Resins, epoxy reduce, and solidifies slowly, and prolong set time, solidifies not exclusively.The urethane resin also is used to increase the toughness of Resins, epoxy as toughner, but polyurethane toughened epoxy resin exists equally under the normal temperature and to solidify slowly, solidifies shortcomings such as incomplete.In addition, used toughner all is to be spiked in the epoxy resin ingredient at present, toughner has very big molecular weight, the reactive behavior of epoxy resin ingredient is reduced, thereby make tackiness agent be difficult to completion of cure at normal temperatures, during its life-time service, ageing resistance and thermotolerance can not satisfy the civil construction requirement.
With Resins, epoxy and urethane is the tackiness agent of skeleton, existing at present many reports.
For example, CN1091129C discloses a kind of structure glue of forming with Resins, epoxy, base polyurethane prepolymer for use as and polymeric amide, have advantages such as adhesive power is strong, stripping strength is high, solidification value is low, set time is short, be mainly used in travelling belt, transmission belt is connected with gluing, but its weather-proof and ageing-resistant performance can not satisfy the civil construction requirement.
CN100355816C discloses a kind of mesh subaqueous patching material of interpenetrating polymer of epoxy/polyurethane, it adopts acrylic acid epoxy resin, base polyurethane prepolymer for use as is the network structure tackiness agent that bone structure structure feedstock production goes out, be mainly used in underwater repair, still there are deficiency in its bonding strength and ageing-resistant performance.
The present inventor adopts the rosin series resin that Resins, epoxy is carried out modification and prepares epoxyn by discovering, has overcome the defective of prior art, so finished the present invention.
Summary of the invention
The invention provides a kind of heat-resisting anti-aging epoxide resin type tackiness agent for building, it is made up of component A and component B two-pack, it is raw material that component A serves as reasons with Resins, epoxy, base polyurethane prepolymer for use as and rosin series resin, in the presence of curing catalysts and solvent, the pre-polymerization component that prepared in reaction forms, component B is solidifying agent and solvent, and wherein the ingredients by weight of each gel component is such as following:
Resins, epoxy 100
Base polyurethane prepolymer for use as 10-30
Rosin series resin 1-40
Curing catalysts 0.1-2
Solidifying agent 1-100
In the embodiment preferred, the component and the content of the present composition are as follows:
Resins, epoxy 100
Base polyurethane prepolymer for use as 15-25
Rosin series resin 5-30
Curing catalysts 0.1-0.5
Solidifying agent 2-25
Solvent 10-100
In the preferred embodiment, also contain silane coupling agent in the present composition B component, its consumption is the 1-10 weight part with respect to 100 parts by weight of epoxy resin.
In the preferred embodiment, can contain inorganic filler in the present composition B component.
As the compound that has 2 epoxide groups in preferred 1 molecule of the Resins, epoxy that uses among the present invention at least.As such epoxy compounds, can exemplify bisphenol f type epoxy resin, bisphenol A type epoxy resin, for example trade(brand)name Resins, epoxy E-12, E-20, E21, E44, E-51, DER331, F44 and TDE-85.Preferred epoxy E system commodity.
Base polyurethane prepolymer for use as is Polyether-Polyol Polyurethane Prepolymer or PAUR performed polymer, for example, preferably has-polyester prepolymer of NCO end group, and NCO/OH=about 2.5.The molecular weight of base polyurethane prepolymer for use as (MW) can be selected for use between 2,000 to 50,000, and preferred 2,000 to 8,000.
Base polyurethane prepolymer for use as can adopt following method preparation: remove the contained small amount of moisture of oligomer polyol (polyether glycol or polyester polyol etc.) earlier, then under the atmosphere of nitrogen, oligomer polyol is added drop-wise in the excessive slightly polyisocyanates while stirring, and in time remove the heat that reaction produces, temperature of reaction is controlled in the certain limit.Sometimes according to the needs of reaction, can add the viscosity of appropriate solvent, add the speed of catalyzer with the control prepolymerization reaction with regulation system.
The base polyurethane prepolymer for use as of all size can be buied in market.The base polyurethane prepolymer for use as that the present invention selects for use can directly be buied on demand from the market.
With respect to 100 weight part Resins, epoxy, adopt the poly-propylhomoserin performed polymer of 10-30 weight part, preferred 15-25 weight part.
When base polyurethane prepolymer for use as mixes with solidifying agent, under the solidifying agent effect, can further react, generate the macromolecule network shaped polymer.
The rosin series resin for example is, resin, toll oil rosin, wood rosin etc. also can be the rosin that this rosin series is carried out modification, hydrogenation or disproportionation, as modified rosin, staybelite or disproportionation rosin.Can exemplify the 138# Gum Rosin, pensel AD, Super Ester T-125 etc.
With respect to 100 parts of Resins, epoxy, adopt 1-40 part rosin series resin, preferred 5-30 part.
Solidifying agent is selected polyamine for use, particularly fatty amine and aromatic amine, for example diethylenetriamine, Triethylenetetramine (TETA), hexanediamine, mphenylenediamine etc.Solidifying agent can be selected wherein one or more for use.Based on the Resins, epoxy of 100 parts of weight, the consumption of solidifying agent is 1-100 part, is preferably 2-25 part.Be less than 1 part and then can't realize good curing, and normally unwanted more than 100 parts.
Curing catalysts is selected organotin, organic acid tin class catalyzer for use, preferably, and dibutyl tin laurate and stannous octoate.Catalyst levels is a catalytic amount, and for example, the Resins, epoxy employing 0.1-1 part with respect to 100 parts of weight is preferably 0.1-0.5 part.
Solvent is selected organic solvent for use, for example is selected from ethanol, methyl alcohol, toluene, acetone, pimelinketone and the ethyl acetate one or more.The amount of solvent is not crucial, can dissolve combination of the present invention and get final product.During preparation, can optionally add, for example, 100 parts by weight of epoxy resin can add the solvent of 100 weight parts, and few solubilizing agent for example, adds the solvent of 10-50 part, is mixed with the two component adhesive of high solids content or low solvent.
The main colloid raw material of glue paste of the present invention comprises Resins, epoxy, base polyurethane prepolymer for use as, rosin series resin and solidifying agent, curing catalysts, if add, silane coupling agent and mineral filler also constitute the colloid part of raw materials.The solvent part is volatilized after use, does not constitute the colloid part of glue paste of the present invention.
Contain above-mentioned organic solvent in the B component, this organic solvent identical or different in can component A.
Silane coupling agent is selected from a kind of in γ-An Jibingjisanyiyangjiguiwan, γ-epoxypropyl triethoxyl silane, γ-glycidoxy butyl trimethoxy silane and the glycidoxy Union carbide A-162, preferred γ-An Jibingjisanyiyangjiguiwan (KH-550).Silane coupling agent plays function served as bridge on by the interface of adhesives, thereby improves bonding strength.
Inorganic filler is selected from chromium aluminate or phosphate (Al
2O
33P
2O
5XCr
2O
3, x=0.1-10), hydroxyapatite, polynite, wilkinite, clay such as class take off stone clay, clay of laminar silicate etc.Inorganic filler can be one or more in them, preferred chromium aluminate or phosphate and hydroxyapatite.Above-mentioned inorganic filler needs to wear into fine powder with sand milling or grinding before interpolation, and for example fineness is less than 50 microns, and above-mentioned inorganic filler itself or cooperate with Resins, epoxy demonstrates good adhesiveproperties.
The additive of inorganic filler can depend on the needs, and is benchmark with 100 parts by weight of epoxy resin, is generally 10-100 part.
Tackiness agent pre-polymerization component A of the present invention can adopt for example following method preparation: raw material is got described weight part; Resins, epoxy is dissolved in the solvent; be preheated to about 30 ℃-solvent boiling point temperature; slowly add base polyurethane prepolymer for use as and rosin series resin again; add curing catalysts; the addition sequence of poly-propylhomoserin performed polymer, rosin series resin and curing catalysts is not crucial, and 50-90 ℃ of reaction obtained tackiness agent pre-polymerization component after 3-10 hour under nitrogen protection.
Adhesive compound of the present invention can prepare by the following method, and above-mentioned tackiness agent pre-polymerization component A is mixed with B component before use, and the weight ratio in component A and the B component is 50-1: 1-2, and during mixing, the weight ratio of Resins, epoxy and solidifying agent was not less than 100: 1.Perhaps also can when pre-polymerization component A is mixed with B component, add inorganic filler before use, mix the back and placed 5-15 minute, just can be used for bonding.
25 ℃ of following open hour of adhesive compound of the present invention are 5-90 minute, and 5-7 days set time, long-term long term operation envrionment temperature is-50 ℃ to+70 ℃, is used for building trade.
Because rosin series resin, the functional group of base polyurethane prepolymer for use as and Resins, epoxy carry out chemical reaction in the presence of catalyzer and solidifying agent, generation is the reticulated structure of island structure and urethane-Resins, epoxy IPN with Resins, epoxy, behind life-time service, softening agent can not occur and secrete phenomenon, therefore, epoxyn of the present invention not only has good adhesiveproperties, and overcome life-time service and have the softening agent that causes and secrete phenomenon, therefore, have good ageing resistance and resistance toheat, be suitable for tackiness agent, especially for exterior wall as building trade, it is bonding that air channel and smoke-uptake make up.
Embodiment
Hereinafter provide non-limiting example.
Embodiment 1
100 gram Resins, epoxy E-51 (blue star novel material Wuxi resin processing plant) are dissolved in the 70 gram acetone; be preheated to about 50 ℃; (MW 3 slowly to add 15 gram base polyurethane prepolymer for use as again; 000) and 15 gram Gum Rosin Super Ester T125; add curing catalysts dibutyl tin laurate 0.25 gram; 80-90 ℃ of reaction obtained tackiness agent pre-polymerization component after 5 hours under nitrogen protection.
Embodiment 2
100 gram Resins, epoxy E-51 (blue star novel material Wuxi resin processing plant) are dissolved in the 60 gram acetone; be preheated to about 60 ℃; (MW 3 slowly to add 30 gram base polyurethane prepolymer for use as again; 000) and 10 the gram rosin; add curing catalysts dibutyl tin laurate 0.25 gram; 80-90 ℃ of reaction obtained tackiness agent pre-polymerization component after 4 hours under nitrogen protection.
Embodiment 3
100 gram Resins, epoxy E-12 (Mount Huang Jin Feng Industrial Co., Ltd.) are dissolved in the 60 gram pimelinketone; be preheated to about 50 ℃; (MW 3 slowly to add 25 gram base polyurethane prepolymer for use as again; 000) and 15 gram Gum Rosin Super Ester T125; add curing catalysts dibutyl tin laurate 0.25 gram; 80-90 ℃ of reaction obtained tackiness agent pre-polymerization component after 5 hours under nitrogen protection.
Embodiment 4
100 gram DER331 (Dow Chemical company limited) are dissolved in the 50 gram ethyl acetate; be preheated to about 60 ℃; (MW 3 slowly to add 30 gram base polyurethane prepolymer for use as again; 000) and 20 the gram rosin; add curing catalysts dibutyl tin laurate 0.25 gram; 80-90 ℃ of reaction obtained tackiness agent pre-polymerization component after 4 hours under nitrogen protection.
Embodiment 5
5 gram γ-An Jibingjisanyiyangjiguiwans (KH-550) and 5 gram mphenylenediamines are dissolved in the 10 gram acetone, are mixed with B component.
Embodiment 6
5 gram γ-An Jibingjisanyiyangjiguiwans (KH-550), 2.5 gram diethylenetriamine and 2.5 gram mphenylenediamines are dissolved in the 10 gram acetone, are mixed with B component.
Embodiment 7
5 gram γ-An Jibingjisanyiyangjiguiwans (KH-550), 2.5 gram diethylenetriamine and 2.5 gram mphenylenediamines are dissolved in the 10 gram acetone, add 5 gram fineness less than 400 purpose chromium aluminate or phosphates, high speed dispersion is mixed with B component.
Embodiment 8
The pre-polymerization combination of 100 gram embodiment 1 is mixed with the B component of 10 gram embodiment 5, get adhesive compound of the present invention, 25 ℃ of open hour, 38 minutes.
Embodiment 9
The pre-polymerization combination of 100 gram embodiment 2 is mixed with the B component of 10 gram embodiment 5, get adhesive compound of the present invention, 25 ℃ of open hour, 25 minutes.
Embodiment 10
The pre-polymerization combination of 100 gram embodiment 3 is mixed with the B component of 10 gram embodiment 5, get adhesive compound of the present invention, 25 ℃ of open hour, 18 minutes.
Embodiment 11
The pre-polymerization combination of 100 gram embodiment 3 is mixed with the B component of 10 gram embodiment 6, get adhesive compound of the present invention, 25 ℃ of open hour, 15 minutes.
Embodiment 12
The pre-polymerization combination of 100 gram embodiment 3 is mixed with the B component of 10 gram embodiment 7, get adhesive compound of the present invention, 25 ℃ of open hour, 15 minutes.
The tackiness agent comprehensive performance test
Shearing resistance is pressed GB7124-86 and is measured;
Stripping strength is pressed GB/T7122-1996 and is measured.
Get the tackiness agent of embodiment 8-10, the curing of branch room temperature was measured its shearing resistance and stripping strength in 24 hours, 3 days and 10 days, saw Table 1.
Table 1 tackiness agent adhesive test
Embodiment 9 tackiness agent are solidified on room temperature, and in 150 ℃ of following thermal ageings 1000 hours, the test shearing resistance saw Table 2.
The test of table 2 tackiness agent heat aging property
Composition of the present invention has good ageing resistance and resistance toheat as adhesive for building, and it is bonding to be applicable to that particularly exterior wall, air channel and smoke-uptake make up.
Claims (9)
1, a kind of epoxide resin type tackiness agent, it is made up of component A and component B two-pack, it is raw material that component A serves as reasons with Resins, epoxy, base polyurethane prepolymer for use as and rosin series resin, in the presence of curing catalysts and solvent, the pre-polymerization component that prepared in reaction forms, component B is solidifying agent and solvent, and the ingredients by weight of each gel component is such as following in the described tackiness agent:
Resins, epoxy 100
Base polyurethane prepolymer for use as 10-30
Rosin series resin 1-40
Curing catalysts 0.1-2
Solidifying agent 1-100.
2, according to the tackiness agent of claim 1, wherein, its component and content are as follows:
Resins, epoxy 100
Base polyurethane prepolymer for use as 15-25
Rosin series resin 5-30
Curing catalysts 0.1-0.5
Solidifying agent 5-50
Solvent 10-100.
3, according to the tackiness agent of claim 1 or 2, wherein, also contain silane coupling agent in the B component, its consumption is the 1-10 weight part with respect to 100 parts by weight of epoxy resin.
4, according to arbitrary tackiness agent of claim 1-3, wherein, solidifying agent is selected from one or more in diethylenetriamine, Triethylenetetramine (TETA), hexanediamine and the mphenylenediamine.
5, according to arbitrary tackiness agent of claim 1-4, wherein, curing catalysts is dibutyl tin laurate or stannous octoate.
6, according to arbitrary tackiness agent of claim 1-5, wherein, silane coupling agent is selected from one or more in γ-An Jibingjisanyiyangjiguiwan, γ-epoxypropyl triethoxyl silane, γ-glycidoxy butyl trimethoxy silane and the glycidoxy Union carbide A-162.
7, according to arbitrary tackiness agent of claim 1-6, wherein, the weight ratio of component A and B component is 50-1: 1-2.
8, according to arbitrary tackiness agent of claim 7, wherein, also contain inorganic filler among the component B, this inorganic filler is selected from chromium aluminate or phosphate and/or hydroxyapatite.
9, the method for the component A in a kind of arbitrary tackiness agent for preparing claim 1-7; Resins, epoxy is dissolved in the solvent; be preheated to about 30 ℃-solvent boiling point temperature; slowly add base polyurethane prepolymer for use as and rosin series resin again; add curing catalysts; 50-90 ℃ of reaction obtained pre-polymerization component A after 3-10 hour under nitrogen protection.
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| CNB2008101229173A CN100485009C (en) | 2008-07-01 | 2008-07-01 | Heat resisting anti-aging adhesive for construction |
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|---|---|---|---|
| CNB2008101229173A CN100485009C (en) | 2008-07-01 | 2008-07-01 | Heat resisting anti-aging adhesive for construction |
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Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN102925096A (en) * | 2012-11-12 | 2013-02-13 | 南京海拓复合材料有限责任公司 | Environmental protection inflaming retarding type tackifier |
| WO2013026406A1 (en) * | 2011-08-25 | 2013-02-28 | 北京仁创科技集团有限公司 | Sand-based composition and sand-based product |
| CN104448214A (en) * | 2014-11-29 | 2015-03-25 | 江苏中鹏新材料股份有限公司 | Method for preparing polyurethane-type epoxy resin containing phosphorus and silicon used for flame-retardant packaging material |
| CN104497956A (en) * | 2014-12-18 | 2015-04-08 | 北京天山新材料技术有限公司 | Rapidly-cured double-component polyurethane elastic adhesive and preparation method thereof |
| CN105349078A (en) * | 2015-12-02 | 2016-02-24 | 云南光电辅料有限公司 | Modified epoxy glue easy to separate after being heated and preparation method thereof |
| CN106753188A (en) * | 2016-11-30 | 2017-05-31 | 江苏芯锐传感科技有限公司 | Environment-friendly type repairing joint filling glue composition and preparation method thereof |
| CN113897169A (en) * | 2020-06-22 | 2022-01-07 | 金言实业集团有限公司 | All-purpose adhesive for outer wall and preparation process thereof |
| CN115785904A (en) * | 2021-09-10 | 2023-03-14 | 深圳市德柏斯科技有限公司 | Sealant with high-temperature resistance function and preparation method thereof |
Family Cites Families (2)
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| CN1670109A (en) * | 2005-05-11 | 2005-09-21 | 李洁华 | Modified epoxy resin adhesive and its preparation process |
| CN101182406A (en) * | 2007-12-14 | 2008-05-21 | 华南理工大学 | Method for preparing multiple modified self-crosslinking aqueous polyurethane adhesive agent |
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Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2013026406A1 (en) * | 2011-08-25 | 2013-02-28 | 北京仁创科技集团有限公司 | Sand-based composition and sand-based product |
| CN102925096A (en) * | 2012-11-12 | 2013-02-13 | 南京海拓复合材料有限责任公司 | Environmental protection inflaming retarding type tackifier |
| CN104448214A (en) * | 2014-11-29 | 2015-03-25 | 江苏中鹏新材料股份有限公司 | Method for preparing polyurethane-type epoxy resin containing phosphorus and silicon used for flame-retardant packaging material |
| CN104448214B (en) * | 2014-11-29 | 2018-04-10 | 江苏中鹏新材料股份有限公司 | A kind of preparation method of fire-retardant phosphorous silicon-based polyurethane type epoxy resin used for packing material |
| CN104497956A (en) * | 2014-12-18 | 2015-04-08 | 北京天山新材料技术有限公司 | Rapidly-cured double-component polyurethane elastic adhesive and preparation method thereof |
| CN105349078A (en) * | 2015-12-02 | 2016-02-24 | 云南光电辅料有限公司 | Modified epoxy glue easy to separate after being heated and preparation method thereof |
| CN106753188A (en) * | 2016-11-30 | 2017-05-31 | 江苏芯锐传感科技有限公司 | Environment-friendly type repairing joint filling glue composition and preparation method thereof |
| CN113897169A (en) * | 2020-06-22 | 2022-01-07 | 金言实业集团有限公司 | All-purpose adhesive for outer wall and preparation process thereof |
| CN115785904A (en) * | 2021-09-10 | 2023-03-14 | 深圳市德柏斯科技有限公司 | Sealant with high-temperature resistance function and preparation method thereof |
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