CN1088604A - Heat-resistant building structure adhesives of amino multi-function epoxy resins - Google Patents
Heat-resistant building structure adhesives of amino multi-function epoxy resins Download PDFInfo
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- CN1088604A CN1088604A CN 92113860 CN92113860A CN1088604A CN 1088604 A CN1088604 A CN 1088604A CN 92113860 CN92113860 CN 92113860 CN 92113860 A CN92113860 A CN 92113860A CN 1088604 A CN1088604 A CN 1088604A
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Abstract
A kind of heat-resistant building structure adhesives of amino multi-function epoxy resins, be to select p-aminophenol 2-glycidyl epoxy or 4 for use, 4 '-diamino ditan four glycidyl epoxy are host, adopt the mixed type solidifying agent of aromatic amine and phenol, formaldehyde, amine condenses and the two component tackiness agent that are mixed with.Its preparation use of this tackiness agent is easy, and raw material is easily synthetic, at room-temperature-curable.It is good to be used for the bonding not only adhesiveproperties of material of construction, and thermotolerance height (can use at 150～180 ℃ of environment), so this tackiness agent is specially adapted to the maintenance and the reinforcing of building structures such as thermal environment high temperature factory building, workshop.
Description
The present invention relates to a kind of organic structure tackiness agent, provide specifically that a kind of to adopt multifunctional aminoepoxy resin be the heat-resistant structural adhesive that host is used for construction industry.
The sqtructural adhesive development is very fast, now has been widely used in industries such as space flight, aviation, electronics, automobile, water power, metallurgy, machinery, petrochemical industry, building.According to different metal construction glue, nonmetal structure glue, construction structure glue, the special construction glue etc. of can being divided into again in its use field with adhesives.Can be divided into coventional type (below～82 ℃) by its heatproof situation again, heat-resistance type (82～149 ℃), 280 ℃ of heat resistant type (150～260 ℃) and high temperature modifications (〉) sqtructural adhesive.Hundreds of heat-resistant structural adhesives have been applied to building structural element, bonding Steel Concrete of self-vulcanizing or steel.But the heat-resistant building structure glue at energy life-time service more than 150 ℃ the report of discovery.U.S. Pat P4,841,010 technology were once mentioned a kind of polyfunctional epoxy resin tackiness agent, it need use the high organic aromatic anhydride of complicated process of preparation cost as solidifying agent, solidifies at normal temperatures, is applied under 120 ℃ of temperature.Though 150 ℃ of fashion certain intensity is arranged, does not see and make heat-resistant building structure glue aspect report.Domestic also once had a report hot setting epoxy construction adhesive of anti-the high-strong toughness, it is that host adds carboxyl butyronitrile reaction and is composited with the bisphenol epoxy, use imidazole curing agent, and be added with the organo-siloxane auxiliary agent, can in metal, plastics, pottery, rubber structure reparation and the assembling of electronics, motor, instrument, automobile, machinery, petroleum industry, use at-55～150 ℃ of life-time service.But this structure glue can not be used as heat-resistant building structure glue.
The building structure adhesive that the purpose of this invention is to provide a kind of heat resistant type, it can at room temperature solidify, and has resistance to elevated temperatures, and low, the raw material of the major ingredient cost of this tackiness agent is easy to get simultaneously.
Heat-resistant building structure tackiness agent provided by the invention improves on the prior art basis and makes, and it still belongs to the gluing formulation of two components, when practical application each component is concocted evenly in proportion.It is host that this tackiness agent adopts amino polyfunctional epoxy resin, and mate corresponding solidifying agent, toughner, promotor, auxiliary agent and filler, it is characterized in that amino polyfunctional epoxy resin adopt p-aminophenol 2-glycidyl epoxy or 4,4 '-diamino ditan four glycidyl epoxy; Solidifying agent adopts the mixed type solidifying agent of aromatic amine and phenolic aldehyde amine condenses, and the content of phenolic aldehyde amine condenses accounts for 60～75%(wt) of mixed type solidifying agent, and its adhesive formulation is:
Amino polyfunctional epoxy resin: 100(part is heavy, below identical)
Toughner: 5～30
Mixed type solidifying agent: 20～45
Promotor: 0.05～5;
Auxiliary agent: 0.5～6;
Mixed fillers: 150～350;
Said components is deployed into two-pack, and the weight percent content of various compositions is in its every component: the first component:
Amino polyfunctional epoxy resin: 25～40
Toughner 3～7
Thinner 1～3
All the other are filler.
The second component:
Mixed type solidifying agent: 20～35;
Promotor: 0.5～4;
Auxiliary agent: 1～6
All the other are filler.
First component concentration (wt) is 60～80% in tackiness agent, and the second component is 20～40%.In the heat-resistant building structure tackiness agent provided by the invention, its toughner can be held carboxyl nitrile (HTBN) or liquid acrylonitrile butadiene rubber with random carboxyl nitrile (HTBN); Thinner adopts the low molecule epoxy compounds that contains epoxy group(ing), as diglycidylether (660, trade(brand)name is as follows), and epoxy propane butyl ether (660A) or ethylene glycol diglycidylether (669); Mixed type solidifying agent is made up of two class solidifying agent, and a class is an aromatic amine curing agent, as two amido ditanes, mphenylenediamine, benzene dimethylamine etc.; Another kind of is phenol, formaldehyde, appropriate class condenses, as phenol, formaldehyde, hexanediamine condenses (701), phenol, formaldehyde, benzene dimethylamine condenses (702), phenol, formaldehyde, quadrol condenses (703) or phenol, formaldehyde, mphenylenediamine condenses etc.Aromatic amine curing agent can account for 25～40%(wt) in mixed type solidifying agent, and phenolic aldehyde amine condenses class solidifying agent accounts for 60～75%.Promotor can be Resorcinol and tertiary amines, as 2,4, and 6-trisphenol (DMP-30).Coupling agent is an auxiliary agent, improves bonding strength, organo-silicon coupling agent commonly used, and as 7-aminopropyl triethoxysilane (KH-550), r-glycidyl ether propyl trimethoxy silicane (KH-560) or anilino Union carbide A-162; The filler that adopts in the tackiness agent is that quartz sand and mineral fillers such as titanium dioxide, talcum powder, lime carbonate, silicon-dioxide and/or carbon black mix, wherein to account for the weight percent of filler be 60～70% to the content of quartz sand, and filler should be ground into certain particle size before use on request.
Heat-resistant building structure tackiness agent provided by the invention, because selecting the aminoepoxy resin of above-mentioned polyfunctionality for use is host, make tackiness agent after the curing have the space reticulated structure of height interlinkage, thereby guaranteed the high heat resistance of tackiness agent, it adopts phenol again, formaldehyde, the mixture of amine condenses and aromatic amine has solved the low worn-out end of self-vulcanizing thermotolerance preferably as solidifying agent, resin and solidifying agent molecule reactive behavior had at room temperature both been improved, make polar functionality and cross-linking density that suitable ratio is arranged again, thereby solved heat-resisting, the contradiction of mechanical property and self-vulcanizing, be that tackiness provided by the invention is at room temperature used, and have higher heat resistance.In addition, introduce an amount of coupling auxiliary agent in the tackiness agent of the present invention again, overcome the internal stress that the resin elastic modulus change causes when producing volumetric shrinkage stress or high low temperature alternation after amino polyfunctional epoxy resin system is solidified and change on macromolecule layer (glue-line) or splicing face, make it maintain higher bonding strength.Simultaneously, introducing such as coupling auxiliary agent also helps to improve structure glue moisture-proof, heat aging performance.
The preparation process of tackiness agent of the present invention can be undertaken by the preparation method of common two component type tackiness agent, promptly the proportioning by above-mentioned tackiness agent takes by weighing material, be mixed with first component and second component respectively, during use, two components mixed by a certain percentage be modulated into tackiness agent of the present invention again.The basic physical properties of this tackiness agent is:
Viscosity: 80,000～90,000 centipoise, modulus of compression: 2.5～3.2 * 10
3MPa; Compressive strength: 70～135MPa, flexural strength: 29～65MPa.Guaranteeing under the bonding strength that this tackiness agent is used for that building slab is bonding can be at 150～180 ℃ of following life-time service.Below by embodiment technology of the present invention is given to illustrate further.
Example 1, the preparation 1 of heat-resistant building structure tackiness agent
(1) first component preparation: with 23 parts of p-aminophenol three-glycidyl epoxies (weight is as follows), 4 parts of nitrile (HTBN)-40 rubber, 1 part of 660A thinner, 30 parts of quartz sands (110 ℃ of drying treatment), 7 parts of titanium dioxides (110 ℃ of drying treatment), 7 parts of talcum powder (110 ℃ of drying treatment) fully mix.
(2) second component preparation: with 35 parts in 701 solidifying agent, 3 parts of mphenylenediamines, DMP-300.6 part, 12 parts of quartz sands (with the first component), 3 parts of titanium dioxides (with the A-wire branch), 3 parts of talcum powder (with the first component), 1 part of coupling auxiliary agent KH-550 fully mixes.
(3) first, second component can be used behind the thorough mixing again, effectively under-stream period is 1 hour.
The preparation 2 of example 2 tackiness agent
(1) first component (process for preparation is with example 1) p-aminophenol 2-glycidyl epoxy is 24 parts, nitrile (HTBN)-40 4 part, 1 part of 660A thinner, 30 parts of quartz sands, 8 parts of titanium dioxides, 7 parts of talcum powder.
(2) component B: 5 parts in 701 solidifying agent, 3 parts of mphenylenediamines, 1 part of Resorcinol, 0.6 part of DMP-30,12 parts of quartz sands, 3 parts of titanium dioxides, 3 parts of talcum powder, 1 part of KH-550 (process for preparation is with example 1).
(3) can use after will going up first, second component thorough mixing.
Example 3 tackiness agent preparation 3
(1) first component: 23 parts of p-aminophenol three-glycidyl epoxies, 35 parts of liquid carboxy nitrile rubbers, 1 part of 660A thinner, 30 parts of quartz sands, 7 parts of titanium dioxides, 7 parts of talcum powder.
(2) component B: 4.2 parts in 701 solidifying agent, 2.3 parts of mphenylenediamines, 12 parts of 0.8 part of quartz sands of DMP-30,4 parts of titanium dioxides, 3 parts of talcum powder, 1 part of KH-550.
(3) above-mentioned first, second two components are mixed and can use.
Example 4 tackiness agent preparation 4
(1) first component: 4,4 '-13 parts of diamino-diphenyl first glycidyl epoxy, 12 parts of p-aminophenol three-glycidyl epoxies, nitrile (HTBN)-40 4 part, 30 parts of 1.2 parts of quartz sands of 669 thinners, 7 parts of titanium dioxides, 7 parts of talcum powder.
(2) component B: 2.2 parts of 4 parts of mphenylenediamines of 703 solidifying agent, 12 parts of 0.7 part of quartz sands of DMP-30,4 parts of titanium dioxides, 3 parts of talcum powder, 1 part of anilino Union carbide A-162.
(3) can use after sparing first, second two component thorough mixing evenly.
Example 5 tackiness agent preparation 5
(1) first component: 4,4 '-13 parts of diaminodiphenyl-methane four glycidyl epoxy, 12 parts of p-aminophenol three-glycidyl epoxies, nitrile (HTBN)-40 4 part, 0.8 part of 660 thinner, 28 parts of quartz sands, 8 parts of titanium dioxides, 7 parts of talcum powder.
(2) component B: 4.2 parts in 701 solidifying agent, 2.8 parts of benzene dimethylamines, 1 part of DMP-30,10 parts of quartz sands, 4 parts of titanium dioxides, 3 parts of talcum powder, 1 part of anilino Union carbide A-162.
(3) first, second two component thorough mixing can be used after even.
Example 6 heat-resistant building structure tackiness agent performance tests
Utilize the tackiness agent of the present invention that is made by example 1～5 respectively, be used to do the bonding experiment of material of construction, to test its performance.Its experiment and the means of testing are routinely carried out, and bonding sample solidifies in room temperature (25 ℃) and can use at full capacity after 3 days intensity reaches 80%, 7 day, and solidification process also can be finished at 60 ℃ in following 4 hours, and its test result is as follows:
(1) adhesiveproperties
Steel/steel shearing resistance room temperature 15～17 MPa
60℃ 17～18MPa
80℃ 17～19MPa
100℃ 17.5～19MPa
120℃ 17.5～19MPa
150℃ 14.9～15.7MPa
165℃ 12.2～12.4MPa
180℃ 10.2～10.5MPa
Steel/concrete room temperature 8.6 (doing the C60 concrete member destroys)
(4.5 wet C60 concrete member destroys)
(2) chemical resistance:
After the soaking at room temperature 1 month, survey shearing resistance
Water, seawater, acetone, alcohol, gasoline, lubricating oil, 15%NaCl 10%NaOH10%NH
3The aqueous solution, equal no change, hardness is 15～14MPa.
(3) heat-resisting gas performance:
Self-vulcanizing, aging through 1500 hours hot gas under 150 ℃, shearing resistance slightly improves during than room temperature and reaches shearing resistance 18～19MPa.
(4) heatproof heat aging performance:
Under 80 ± 2 ℃ of 85 ± 3% humidity, aging through 2000 hours, stable performance, shearing resistance improves when initial, reaches 18～19MPa.
(5) fatigue performance:
Under the normal temperature, steel/steel frequency 200 times/second
ρ=0.1 (out-of-balance load rate) J
b=14.22MPa N=10
7Inferior destruction
ρ=0.1 (out-of-balance load rate) J
b=15.02MPa 7.4 * 10
6Inferior destruction
ρ=0.1 (out-of-balance load rate) J
b=15.34MPa 5.2 * 10
6Inferior destruction
ρ=0.1 (out-of-balance load rate) J
b=16.52MPa 3.2 * 10
6Inferior destruction
Under+100 ℃
ρ=0.1 J
b=3.76〉10
7Inferior destruction
ρ=0.1 J
b=7.12 3.4 * 10
6Inferior destruction
ρ=0.1 J
b=9.33 2.4 * 10
6Inferior destruction
By above-mentioned example, adopt building structure adhesive provided by the invention, its preparation use is easy, and raw material is easily synthetic, and it is bonding to be used for material of construction, and its adhesiveproperties is good, and the thermotolerance height.Therefore, it can be widely used in metallurgy, chemical fertilizer, machinery, chemical industry, oil, power industry building because of long term thermal environment steel-bonded reinforcement to work reinforced concrete member and factory building when impaired, thermal environment (more than 100 ℃) high temperature factory building particularly, the maintenance of workshop building structural member (150～180 ℃) is used during reinforcing.
Claims (4)
1, a kind of amino polyfunctional epoxy resin class building structure adhesive, it is characterized in that Resins, epoxy adopts p-aminophenol 2-glycidyl epoxy or 4,4 '-diamino ditane four glycidyl epoxy, solidifying agent adopts the mixed type solidifying agent of aromatic amine and phenolic aldehyde amine condenses, and the content of phenolic aldehyde amine condenses accounts for 60～75% in the mixed type solidifying agent (wt), and its adhesive formulation is:
Amino polyfunctional epoxy resin: 100 (parts heavy, below identical)
Toughner: 5～30
Mixed type solidifying agent: 20～45
Promotor: 0.05～5;
Auxiliary agent: 0.5～6;
Mixed fillers: 150～350.
2, according to the described tackiness agent of claim 1, it is characterized in that tackiness agent is mixed with two components before use, the weight percent of contained composition is in each component:
The first component:
Amino polyfunctional epoxy resin: 25～40
Toughner 3～7
Thinner 1～3
All the other are filler.
The second component:
Mixed type solidifying agent: 20～35;
Promotor: 0.5～4;
Auxiliary agent: 1～6
All the other are filler; And the first component concentration is 60～80% in the tackiness agent, and the second component is 20～40%.
3, according to the described tackiness agent of claim 1, it is characterized in that adopting organo-silicon coupling agent is auxiliary agent, as γ-An Bingjisanyiyangjiguiwan, and γ-glycidyl ether propyl trimethoxy silicane or anilino Union carbide A-162.
4, according to the described tackiness agent of claim 1, it is characterized in that mixed fillers is that quartz sand and mineral fillers such as titanium dioxide, talcum powder, lime carbonate, silicon-dioxide and/or carbon black mix, and the weight percent that the content of quartz sand accounts for filler is 60～70%.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN92113860A CN1038338C (en) | 1992-12-23 | 1992-12-23 | Heat-resistant building structure adhesives of amino multi-function epoxy resins |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN92113860A CN1038338C (en) | 1992-12-23 | 1992-12-23 | Heat-resistant building structure adhesives of amino multi-function epoxy resins |
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| Publication Number | Publication Date |
|---|---|
| CN1088604A true CN1088604A (en) | 1994-06-29 |
| CN1038338C CN1038338C (en) | 1998-05-13 |
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|---|---|---|---|
| CN92113860A Expired - Fee Related CN1038338C (en) | 1992-12-23 | 1992-12-23 | Heat-resistant building structure adhesives of amino multi-function epoxy resins |
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| CN100532489C (en) * | 2006-01-21 | 2009-08-26 | 邹春林 | Adhesion agent for moist dimension stone |
| CN101128504B (en) * | 2004-12-22 | 2011-01-26 | 亨斯迈先进材料（瑞士）有限公司 | Coating system |
| CN102153978A (en) * | 2011-03-11 | 2011-08-17 | 中南林业科技大学 | Room-temperature solidification heat-resistant epoxy adhesive |
| CN101314706B (en) * | 2008-07-11 | 2011-11-16 | 镇江市天益工程科技有限公司 | Preparation of solidification type steel adhesion structure glue in low-temperature and humidity surroundings |
| CN102443371A (en) * | 2011-10-28 | 2012-05-09 | 武钢集团昆明钢铁股份有限公司 | Hard splicing-locking stuffing and preparation method thereof |
| CN102850978A (en) * | 2011-06-28 | 2013-01-02 | 上海市合成树脂研究所 | Room temperature cured high-temperature resistant epoxy adhesive |
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| CN103881635A (en) * | 2012-12-22 | 2014-06-25 | 中航贵州飞机有限责任公司 | Preparation method of adhesive capable of being used at 180 DEG C and adhesive |
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| CN109705784A (en) * | 2018-12-03 | 2019-05-03 | 上海康达新能源材料有限公司 | A kind of high-peeling strength epoxy construction adhesive and preparation method thereof |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| PL133693B1 (en) * | 1982-01-07 | 1985-06-29 | Inst Chemii Przemyslowej | Two-component epoxide adhesive |
| DE3644244A1 (en) * | 1985-12-24 | 1987-06-25 | Toho Rayon Kk | CARBON FIBER CORD FOR RUBBER REINFORCEMENT AND THEIR PRODUCTION |
| US4841010A (en) * | 1987-09-02 | 1989-06-20 | State Of Israel, Ministry Of Defence, Armament Development Authorithy, Rafel | Triglycidyl ether/tetraglycidyl ether/alkadiene rubber/polyalkylene polyamine formulation |
| CN88101121A (en) * | 1988-03-01 | 1988-11-30 | 西北工业大学 | The sqtructural adhesive and the compound method thereof of high temperature resistant, buck |
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- 1992-12-23 CN CN92113860A patent/CN1038338C/en not_active Expired - Fee Related
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| CN100532489C (en) * | 2006-01-21 | 2009-08-26 | 邹春林 | Adhesion agent for moist dimension stone |
| CN101314706B (en) * | 2008-07-11 | 2011-11-16 | 镇江市天益工程科技有限公司 | Preparation of solidification type steel adhesion structure glue in low-temperature and humidity surroundings |
| CN102153978A (en) * | 2011-03-11 | 2011-08-17 | 中南林业科技大学 | Room-temperature solidification heat-resistant epoxy adhesive |
| CN102153978B (en) * | 2011-03-11 | 2013-07-17 | 中南林业科技大学 | Room-temperature solidification heat-resistant epoxy adhesive |
| CN102850978A (en) * | 2011-06-28 | 2013-01-02 | 上海市合成树脂研究所 | Room temperature cured high-temperature resistant epoxy adhesive |
| CN102850978B (en) * | 2011-06-28 | 2015-05-13 | 上海市合成树脂研究所 | Room temperature cured high-temperature resistant epoxy adhesive |
| CN102443371A (en) * | 2011-10-28 | 2012-05-09 | 武钢集团昆明钢铁股份有限公司 | Hard splicing-locking stuffing and preparation method thereof |
| CN103881635A (en) * | 2012-12-22 | 2014-06-25 | 中航贵州飞机有限责任公司 | Preparation method of adhesive capable of being used at 180 DEG C and adhesive |
| CN103881530A (en) * | 2014-02-26 | 2014-06-25 | 施俊杰 | Preparation method of epoxy resin anticorrosive material |
| CN105778842A (en) * | 2016-02-24 | 2016-07-20 | 刘操 | LED package adhesive with high heat conductivity and preparing method and application thereof |
| CN108329876A (en) * | 2018-02-07 | 2018-07-27 | 滕凤琴 | A kind of corrosion-resistant epoxyn and preparation method thereof |
| CN109054787A (en) * | 2018-08-17 | 2018-12-21 | 河北工业大学 | A kind of plugging material of organic/inorganic composite |
| CN109705784A (en) * | 2018-12-03 | 2019-05-03 | 上海康达新能源材料有限公司 | A kind of high-peeling strength epoxy construction adhesive and preparation method thereof |
| CN110330929A (en) * | 2019-07-23 | 2019-10-15 | 潍坊汇胜绝缘技术有限公司 | A kind of application of binder and binder in laminated paper board preparation process |
| CN110437584A (en) * | 2019-08-07 | 2019-11-12 | 威海光威复合材料股份有限公司 | Hot setting resin and the preparation method and application thereof |
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|---|---|
| CN1038338C (en) | 1998-05-13 |
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