CN102453458A - Nano rubber modified room temperature cured high temperature resistant structure adhesive - Google Patents
Nano rubber modified room temperature cured high temperature resistant structure adhesive Download PDFInfo
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- CN102453458A CN102453458A CN201010521945XA CN201010521945A CN102453458A CN 102453458 A CN102453458 A CN 102453458A CN 201010521945X A CN201010521945X A CN 201010521945XA CN 201010521945 A CN201010521945 A CN 201010521945A CN 102453458 A CN102453458 A CN 102453458A
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Abstract
The invention provides a nano rubber modified room temperature cured high temperature resistant structure adhesive, which consists of 90 to 120 parts of nano rubber modified epoxy resin (XH), 15 to 40 parts of multifunctional epoxy resin (DH), 35 to 55 parts of high temperature resistant modified aromatic amine curing agent, 70 to 110 parts of high temperature resistant filler (FZX), 1 to 10 parts of promoter and 1 to 10 parts of coupler. The nano rubber modified room temperature cured high temperature resistant structure adhesive is cured at normal temperature, can meet the requirement of high temperature application, and is convenient to use in engineering.
Description
Technical field
The invention belongs to the structural adhesive field, be specifically related to a kind of can the room temperature completely solidified, and can be at the Nano powder rubber modified epoxide resin adhesive of life-time service under the hot conditions.。
Background technology
Existing high-temperature resistance adhesive is mainly formulated by pressed powder solidifying agent and high viscosity resins, but is mostly middle temperature or high-temperature curing agent, needs heating unit, and application art is complicated, and the proportioning consumption is big, is difficult for simply mixing.
Chinese patent 03116358.0 report: a kind of composition comprises 5-50% (weight part) polyimide precursor; 95-50% (weight part) 4; 4 '-diaminodiphenyl-methane type, four sense epoxy compoundss and plant the 2-30 weight part that mixture 100 weight of material are the basis with the first two and gather methyl (3; 3,3-trifluoro propyl) the tackiness agent constituent of silicone rubber stirs to mix in tetrahydrofuran solvent in 20-40 ℃ and obtains adhesive solvent.This kind adhesive solvent is 200 ℃ of 12-14MPa of shearing resistance to bonding its intensity of duraluminum; 250 ℃ of 4.87MPa; 270 ℃ of 3.93Mpa; Inhomogeneous stripping strength room temperature 40KN/m; To bonding its intensity of titanium alloy be: shearing resistance room temperature 24.5MPa; 250 ℃ of 4.9MPa; 270 ℃ of 4.15MPa.
Chinese patent 85100135 reports: 100 parts of two or more blending epoxies < weight>that have two end epoxy group(ing) in each molecule of this epoxy binder modified mainly including (1) heating curable at least; Preferably wherein having at least a kind of is solid epoxy; Have at least another kind to be 25 ℃ and be the epoxy resin of liquid down, (2) number-average molecular weight is at 3000--4000, and acrylonitrile content is at 20%--32%; Average functionality is the carboxyl end of the liquid acrylonitrile-butadiene rubber 5--35 part more than 1.7; (3) to stablize down at 25 ℃ on a small quantity, be heated to 120 ℃ of ability solidified latent curing agents and promotor and an amount of thixotropic agent. this kind tackiness agent is a single component glue, can be made into glued membrane; Glue or glue rod are one type of intermediate temperature setting HS modified epoxy sqtructural adhesives.
Chinese patent 200610151171.X report: the invention discloses a kind of novel fire resistant epoxyn and preparation method thereof; It is made up of first, second two-pack; The first component comprises fluorenyl epoxy resin, E-51 epoxy resin and E-44 epoxy resin; The second component comprises anhydride curing agent, and the mass ratio of each component is: 100 parts of fluorenyl epoxy resin, 0～50 part of E-51 epoxy resin, 0～50 part of E-44 epoxy resin, 30～80 parts of anhydride curing agents.The present invention processes fluorenyl epoxy resin by bisphenol fluorene and epoxy chloropropane through polycondensation; With resin and solidifying agent heating blend; Process epoxyn; This tackiness agent is after solidifying under 150～200 ℃, and its high temperature (200 ℃) shearing resistance reaches more than the 8MPa, can be used for the occasion higher to the shear at high temperature requirement of strength.
The subject matter of aforementioned techniques is that material require solidifies under heating condition, will occur the difficulty that is difficult to overcome on the large foundation facility if be applied in large quantities, needs expensive heating unit and complicated control techniques, is uneconomic in most of occasions.
Summary of the invention
In order to solve tackiness agent still keeps higher-strength when under hot conditions, using after the ambient cure a difficult problem; The invention provides a kind of nano-rubber modification room curing and high temperature resistant structural adhesive; Reach ambient cure and just can satisfy the high temperature use properties, make things convenient for practical applications.
A kind of nano-rubber modification room curing and high temperature resistant structural adhesive of the present invention, directly mixed by following parts by weight of component and to form:
90 ~ 120 parts of nano-rubber modified epoxies (XH),
15 ~ 40 parts of multiple functionality epoxide resins (DH),
35 ~ 55 parts of heat resist modification aromatic amine curing agents,
70 ~ 110 parts of high temperature resistant fillers (FZX),
1 ~ 10 part of promotor,
1 ~ 10 part of coupling agent;
Said nano-rubber modified epoxy is in the active nano level rubber of 5 ~ 50 parts of per 100 parts of E-51/E44 epoxy resin addings, obtains the epoxy resin toughened of modification at 15 ~ 75 ℃ of uniform mixing; Said heat resist modification aromatic amine curing agent is that 80 ~ 100 parts mphenylenediamine is heated to 45 ~ 50 degree; Add 1 ~ 7 part of imidazoles; Be warming up to 65 ℃ after adding, add 30 ~ 45 parts aliphatic cyclic amine methyl ring pentamethylene diamine and 2,3-(dimethyl-) two butylidene triamines are pressed the mixed mixture of mass ratio 2:1 ~ 3:1; Reacted 3 ~ 4 hours, discharging makes the modified aromatic amine hardener that viscosity is 2000 ~ 3000mpa.s.
Said active nano level rubber can adopt the nano level full vulcanized powdered rubber with controllable particle diameter of record in the number of patent application 00816450.9.
Wherein the screening formulation proportioning is made up of following parts by weight of component:
Nano-rubber modified epoxy 100-110 part,
Multiple functionality epoxide resin 25-35 part,
Heat resist modification aromatic amine curing agent 40-50 part,
High temperature resistant filler 80-100 part,
Promotor 5-7 part,
Coupling agent 3-7 part.
Above-mentioned multiple functionality epoxide resin is phenolic multi-functional epoxy, 4,5-epoxy cyclohexyl-1,2-dioctyl phthalate 2-glycidyl ester (TDE85) or MDA four glycidyl ethers (AG80)
Above-mentioned high temperature resistant filler be with one or several of silicon powder or aluminum oxide powder or asbestos powder or blaue fixe in 80% ~ 85% vitriol oil in 120 ~ 135 ℃ of following pickling of high temperature 2 ~ 3 hours, using pure water to be washed till PH again is 7, after high temperature is removed moisture, makes.
Above-mentioned promotor is phenol, Resorcinol, ortho-cresol, NP or two phenolic group propane.
Above-mentioned coupling agent is γ-An Bingjisanyiyangjiguiwan (KH-550), 3-(2,3-epoxy third oxygen) propyl trimethoxy silicane (KH-560), γ-methacryloxypropyl trimethoxy silane (KH-570) or anilinomethyl triethoxysilane (Nanjing University-42).
The present technique principal feature is to use the distinctive heatproof toughner of polymer nano-scale elastomeric material; Guarantee that colloid has enough toughness to be unlikely and breaks under high temperature and stress; Modification alicyclic ring/aromatic amine curing agent has stable internal structure and is difficult for receiving heat collapse; High crosslinked cubic network space structure is guaranteed the colloid excessive person's movements and expression of at high temperature unlikely generation and is caused the glue-line autoclasia; Particle in the filler has played the effect that reduces cure shrinkage and high temperature rate of expansion, and the fiber in the filler has played the effect that increases breaking tenacity, and coupling agent has played crucial bridge linking effect between the organic and inorganic phase; To bonding strength and heat shock resistance, corrosion-resistant have a strong resistant function.
Nano-rubber modification room curing and high temperature resistant structural adhesive of the present invention, self-vulcanizing 24h, room temperature is drawn and is cut intensity 14Mpa.Completely solidified after three days, room temperature are drawn and are cut intensity and reach more than 18 Mpa.150 ℃ are drawn and cut intensity more than 6 Mpa, in the time of 180 ℃ greater than 2.5 Mpa.
The invention has the beneficial effects as follows: common sizing agent need solidify under heating condition; The difficulty that is difficult to overcome will appear on the large foundation facility if be applied in large quantities; Needing expensive heating unit and complicated control techniques, is uneconomic in most of occasions; And the present invention can be solidified at normal temperatures and still keep higher-strength when under hot conditions, using, and cost is practiced thrift in easy construction.
Embodiment
Following umber is weight part;
1, the preparation of nano-rubber modified epoxy:
In the active nano level rubber that per 100 parts of E44 epoxy resin adding is 15 parts, obtain the epoxy resin toughened of modification at 55 ℃ of uniform mixing, subsequent use;
2, the preparation of heat resist modification aromatic amine curing agent:
90 parts mphenylenediamines are added in the reactor drum, be heated to 45 degree, add 4 parts of imidazoles; Be warming up to 65 ℃ after adding; The aliphatic cyclic amine methyl ring pentamethylene diamine TAC/TAB that adds 40 parts reacted 3.85 hours, and discharging makes the modified aromatic amine hardener that viscosity is 2500mpa.s, and is subsequent use;
3, the preparation of high temperature resistant filler:
With silicon powder, aluminum oxide powder, asbestos powder, blaue fixe respectively in 85% vitriol oil in 130 ℃ of following pickling of high temperature 2.5 hours, using pure water to be washed till PH again is 7, subsequent use after high temperature is removed moisture;
Instance one
Composition of raw materials is following:
95 parts of nano-rubber modified epoxies,
20 parts of multiple functionality epoxide resins,
40 parts of heat resist modification aromatic amine curing agents,
3 parts of Resorcinols
KH-550 3 part
25 parts of asbestos powders
50 parts of aluminum oxide powders
Mix the back in self-vulcanizing three days, shearing stress was before test stretched: room temperature 18.5Mpa, 150 6.2Mpa when spending, 180 2.6MPa when spending
Instance two
Composition of raw materials is following:
100 parts of nano-rubber modified epoxies,
30 parts of multiple functionality epoxide resins,
50 parts of heat resist modification aromatic amine curing agents,
Nanjing University-42 5 part
5 parts of ortho-cresols
30 parts of asbestos powders
60 parts of aluminum oxide powders
Mix the back in self-vulcanizing three days, shearing stress was before test stretched: room temperature 18.7Mpa, 150 6.3Mpa when spending, 180 2.7MPa when spending
Instance three
Composition of raw materials is following:
115 parts of nano-rubber modified epoxies
40 parts of multiple functionality epoxide resins
55 parts of heat resist modification aromatic amine curing agents
KH-560 8 part
7 parts of ortho-cresols
28 parts of asbestos powders
65 parts of aluminum oxide powders
15 parts in permanent white
Mix the back in self-vulcanizing three days, shearing stress was before test stretched: room temperature 18.7Mpa, 150 7.6Mpa when spending, 180 3.2Mpa when spending.
Claims (6)
1. nano-rubber modification room curing and high temperature resistant structural adhesive, simply mixed by following parts by weight of component and to form:
90 ~ 120 parts of nano-rubber modified epoxies,
15 ~ 40 parts of multiple functionality epoxide resins,
35 ~ 55 parts of heat resist modification aromatic amine curing agents,
70 ~ 110 parts of high temperature resistant fillers,
1 ~ 10 part of promotor,
1 ~ 10 part of coupling agent;
Said nano-rubber modified epoxy is in the active nano level rubber of 5 ~ 50 parts of per 100 parts of E-51/E44 epoxy resin addings, obtains the epoxy resin toughened of modification at 15 ~ 75 ℃ of uniform mixing; Said heat resist modification aromatic amine curing agent is that 80 ~ 100 parts mphenylenediamine is heated to 45 ~ 50 degree; Add 1 ~ 7 part of imidazoles; Be warming up to 65 ℃ after adding, add 30 ~ 45 parts aliphatic cyclic amine methyl ring pentamethylene diamine and 2,3-(dimethyl-) two butylidene triamines are pressed the mixed mixture of mass ratio 2:1 ~ 3:1; Reacted 3 ~ 4 hours, discharging makes the modified aromatic amine hardener that viscosity is 2000 ~ 3000mpa.s.
2. a kind of nano-rubber modification room curing and high temperature resistant structural adhesive according to claim 1 is characterized in that, is directly mixed by following parts by weight of component and forms:
Nano-rubber modified epoxy 100-110 part,
Multiple functionality epoxide resin 25-35 part,
Heat resist modification aromatic amine curing agent 40-50 part,
High temperature resistant filler 80-100 part,
Promotor 5-7 part,
Coupling agent 3-7 part.
3. a kind of nano-rubber modification room curing and high temperature resistant structural adhesive according to claim 1 and 2; It is characterized in that; Said multiple functionality epoxide resin is phenolic multi-functional epoxy, 4; 5-epoxy cyclohexyl-1,2-dioctyl phthalate 2-glycidyl ester or MDA four glycidyl ethers.
4. a kind of nano-rubber modification room curing and high temperature resistant structural adhesive according to claim 1 and 2; It is characterized in that; Said high temperature resistant filler be with one or several of silicon powder or aluminum oxide powder or asbestos powder or blaue fixe in 80% ~ 85% vitriol oil in 120 ~ 135 ℃ of following pickling of high temperature 2 ~ 3 hours; Using pure water to be washed till PH again is 7, after high temperature is removed moisture, makes.
5. a kind of nano-rubber modification room curing and high temperature resistant structural adhesive according to claim 1 and 2 is characterized in that said promotor is phenol, Resorcinol, ortho-cresol, NP or two phenolic group propane.
6. a kind of nano-rubber modification room curing and high temperature resistant structural adhesive according to claim 1 and 2; It is characterized in that; Said coupling agent is γ-An Bingjisanyiyangjiguiwan, 3-(2,3-epoxy third oxygen) propyl trimethoxy silicane, γ-methacryloxypropyl trimethoxy silane, anilinomethyl triethoxysilane.
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| CN 201010521945 CN102453458B (en) | 2010-10-28 | 2010-10-28 | Nano rubber modified room temperature cured high temperature resistant structure adhesive |
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Cited By (10)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN102952469A (en) * | 2012-10-27 | 2013-03-06 | 蚌埠凤凰滤清器有限责任公司 | High-strength compound adhesive film for filter |
| CN103965820A (en) * | 2014-05-04 | 2014-08-06 | 武汉建福新材料有限公司 | High-strength underwater structure adhesive and preparation method thereof |
| CN104927737A (en) * | 2015-07-17 | 2015-09-23 | 重庆桥都桥梁技术有限公司 | Bridge support leveling adhesive and preparation method thereof |
| CN107556954A (en) * | 2017-09-12 | 2018-01-09 | 四川力通复合材料科技有限公司 | A kind of aramid fiber cellular composite material epoxy structural rubber and preparation method thereof |
| CN108219300A (en) * | 2018-03-02 | 2018-06-29 | 合肥铭佑高温技术有限公司 | A kind of temperature variation resistant rubber for Air-conditioning Cycle pipe insulation |
| CN110564347A (en) * | 2019-09-09 | 2019-12-13 | 上海汉司实业有限公司 | One-component epoxy structure adhesive for waterproof sealing and preparation method thereof |
| CN111154442A (en) * | 2020-01-13 | 2020-05-15 | 王凤艳 | Environment-friendly high-temperature-resistant modified epoxy resin adhesive and preparation method thereof |
| CN111320957A (en) * | 2020-04-09 | 2020-06-23 | 无锡万亿星新材料科技有限公司 | Epoxy adhesive for aluminum corrugated board and preparation method thereof |
| CN111793450A (en) * | 2020-07-23 | 2020-10-20 | 黑龙江省科学院石油化学研究院 | Medium-high temperature curing epoxy structure adhesive film with thermal breaking performance applied to sound absorption and noise reduction honeycomb plate and preparation method thereof |
| CN112500820A (en) * | 2020-12-17 | 2021-03-16 | 陕西华达科技股份有限公司 | Novel high-temperature-resistant epoxy resin adhesive and preparation method and use method thereof |
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Cited By (15)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102952469A (en) * | 2012-10-27 | 2013-03-06 | 蚌埠凤凰滤清器有限责任公司 | High-strength compound adhesive film for filter |
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| CN103965820A (en) * | 2014-05-04 | 2014-08-06 | 武汉建福新材料有限公司 | High-strength underwater structure adhesive and preparation method thereof |
| CN103965820B (en) * | 2014-05-04 | 2015-09-16 | 武汉建福新材料有限公司 | High strength underwater structure glue and preparation method thereof |
| CN104927737A (en) * | 2015-07-17 | 2015-09-23 | 重庆桥都桥梁技术有限公司 | Bridge support leveling adhesive and preparation method thereof |
| CN104927737B (en) * | 2015-07-17 | 2016-08-24 | 重庆桥都桥梁技术有限公司 | A kind of bridge pad leveling glue and preparation method thereof |
| CN107556954A (en) * | 2017-09-12 | 2018-01-09 | 四川力通复合材料科技有限公司 | A kind of aramid fiber cellular composite material epoxy structural rubber and preparation method thereof |
| CN108219300A (en) * | 2018-03-02 | 2018-06-29 | 合肥铭佑高温技术有限公司 | A kind of temperature variation resistant rubber for Air-conditioning Cycle pipe insulation |
| CN110564347A (en) * | 2019-09-09 | 2019-12-13 | 上海汉司实业有限公司 | One-component epoxy structure adhesive for waterproof sealing and preparation method thereof |
| CN111154442A (en) * | 2020-01-13 | 2020-05-15 | 王凤艳 | Environment-friendly high-temperature-resistant modified epoxy resin adhesive and preparation method thereof |
| CN111154442B (en) * | 2020-01-13 | 2022-05-24 | 王凤艳 | Environment-friendly high-temperature-resistant modified epoxy resin adhesive and preparation method thereof |
| CN111320957A (en) * | 2020-04-09 | 2020-06-23 | 无锡万亿星新材料科技有限公司 | Epoxy adhesive for aluminum corrugated board and preparation method thereof |
| CN111793450A (en) * | 2020-07-23 | 2020-10-20 | 黑龙江省科学院石油化学研究院 | Medium-high temperature curing epoxy structure adhesive film with thermal breaking performance applied to sound absorption and noise reduction honeycomb plate and preparation method thereof |
| CN111793450B (en) * | 2020-07-23 | 2023-01-24 | 黑龙江省科学院石油化学研究院 | Medium-high temperature curing epoxy structure adhesive film with thermal breaking performance applied to sound absorption and noise reduction honeycomb plate and preparation method thereof |
| CN112500820A (en) * | 2020-12-17 | 2021-03-16 | 陕西华达科技股份有限公司 | Novel high-temperature-resistant epoxy resin adhesive and preparation method and use method thereof |
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