CN1244660C - Preparation method of room temperature cured high temperature tolerant flexible epoxy adhesive - Google Patents
Preparation method of room temperature cured high temperature tolerant flexible epoxy adhesive Download PDFInfo
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- CN1244660C CN1244660C CN 200310111085 CN200310111085A CN1244660C CN 1244660 C CN1244660 C CN 1244660C CN 200310111085 CN200310111085 CN 200310111085 CN 200310111085 A CN200310111085 A CN 200310111085A CN 1244660 C CN1244660 C CN 1244660C
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Abstract
The present invention discloses a room-curing high-temperature resistant flexible epoxy adhesive and a preparation method thereof. The adhesive is composed of an adhesive component and a curing component, wherein the adhesive component also comprises a toughening component, a temperature-resistant component and a plasticizing agent; the curing component is composed of a main curing agent and a curing accelerating agent; the curing accelerating agent is a mixture of multiple components; the adhesive component and the curing component are respectively prepared and are respectively packaged; when used, the adhesive component and the curing component are proportionally mixed and modulated in place. The epoxy adhesive prepared by the method has the advantages of excellent flexibility and high adhesive strength; the impact strength at room temperature is not lower than 30MPa, using temperature is high, and the epoxy adhesive can be used at the temperature of 300 DEG C. for a long time.
Description
One, technical field
The present invention relates to technical field of adhesive, more particularly, relating to Resins, epoxy is base mateiral, by adhesive component and the curing component epoxy adhesive and the preparation method that become of hybrid modulation in use.
Two, background technology
The epoxy adhesive that with Resins, epoxy is main ingredient has very high cohesive strength, can be used for the bonding between metal, pottery, glass, timber, plastic or other material member.Prior art has been developed the different epoxy adhesive of multiple performance according to the environment for use difference of bonding piece, for social economy's construction contributes.But the performance of the epoxy adhesive of prior art is desirable not enough, and the snappiness that promptly has is better, and resistance to impact shock is higher, but temperature tolerance is relatively poor, can only use under 100～150 ℃ of environment, at high temperature life-time service; Otherwise the high thermal resistance that has is better, can use under hot environment, but snappiness is very poor, the not enough 20MPa of resistance to impact shock under the normal temperature, can not satisfy the requirement of intensity, the heat resistance and the flexility that also have in addition are all right, but can not solidify down in room temperature (25 ± 5 ℃).Therefore the epoxy adhesive of prior art can't be applicable to the operation that bonds at normal temperatures, and use temperature and resistance to impact shock require than higher environment, as the member bonding in fields such as a lot of civilian structures, train rail signal shielding, aerospacecraft structure, borer brake sheet.
Three, summary of the invention
Deficiency at the prior art epoxy adhesive exists the purpose of this invention is to provide a kind of operation that can at room temperature bond, and use temperature can reach 300 ℃, and the resistance to impact shock under the room temperature can reach epoxy adhesive of 30MPa and preparation method thereof.
Room curing and high temperature resistant type flexible epoxy tackiness agent provided by the invention, by in use just phase blended adhesive component and curing component form, the ratio of weight and number of two kinds of components is 100 parts of adhesive components, 30～100 parts of curing components.What of curing component proportion are depended on the requirement to adhesive solidification speed.The ratio height that curing component accounts for, the adhesive solidification speed of tackiness agent is fast, otherwise then slow.But the ratio that curing component accounts for is too high, can influence the bond effect of tackiness agent.
Described adhesive component contains multiple component again, has plenty of to belong to the toughness reinforcing component that improves the tackiness agent flexility in these components, has plenty of to belong to the heatproof component that improves the tackiness agent heat resistance.These two kinds of components are as follows respectively in the composition with a kind of weight unit umber:
Toughness reinforcing component:
100 parts of toughness reinforcing discharge ring epoxy resins
30～50 parts of liquid acrylonitrile butadiene rubber toughner
5～12 parts of polyfunctional epoxy resin toughness reinforcing accelerants
The heatproof component:
80～100 parts of heatproof discharge ring epoxy resins
50～60 parts of silicone resin heatproof properties-correcting agent
40～50 parts of resol heatproof properties-correcting agent
Described curing component is the main body solidifying agent with the polyetheramine, is curing catalyst with the organic amine.Curing component composed as follows in a kind of weight unit umber:
100 parts in polyetheramine main body solidifying agent
20～30 parts of organic amine curing catalysts
Described toughness reinforcing discharge ring epoxy resins is selected from the Resins, epoxy that the trade mark is E51, and described heatproof discharge ring epoxy resins is selected from the Resins, epoxy that the trade mark is E20.
In the adhesive component preparation process of above-mentioned tackiness agent, can add a certain amount of thinner to silicone resin as required, dilute as methyl alcohol etc., so that toughness reinforcing component is mixed with the heatproof component.
Also can contain with the dibutyl phthalate in the above-mentioned adhesive component is the component of softening agent, and to improve the use properties of tackiness agent, the weight content of plasticizer components is not more than 5 parts.
Liquid acrylonitrile butadiene rubber in the above-mentioned adhesive component can be selected from liquid nbr carboxyl terminal and liquid hydroxy'terminated butadiene nitrile rubber, promptly can be wherein a kind of be toughner, can be toughner with two kinds simultaneously also.
Polyfunctional epoxy resin in the above-mentioned adhesive component is the promotor that is used to improve the liquid acrylonitrile butadiene rubber toughening effect, can be selected from 4, polyfunctional epoxy resins such as 4 '-diaminodiphenylmethane, four sense Resins, epoxy, Resorcinol difunctional epoxy resin.Containing this composition toughening effect in the toughness reinforcing component of adhesive component can be better, but this composition does not have tangible toughening effect yet, and promptly this composition is not must composition.This composition can be a kind of in the above-mentioned polyfunctional epoxy resin, also can be their mixture.
As the silicone resin of heatproof properties-correcting agent, can purchase from the market in the above-mentioned adhesive component, also can oneself synthesize preparation.When taking a kind of mode in back, 40～50 parts of available diphenyl dichlorosilanes, 8～10 parts of dimethyldichlorosilane(DMCS)s and 3～5 parts of synthetic preparations of boric acid.
In the above-mentioned curing component as the organic amine of curing catalyst, can select several as curing catalyst from organic amines such as hexanediamine, Dyhard RU 100,2-ethyl monomethyl imidazoles, mphenylenediamine and m-xylene diamine, the kind of selection mainly be to consider contained composition in the adhesive component.The preferential mixture of at least 4 kinds of components in 2.5～5.0 parts of 3.0～7.0 parts of hexanediamines, 4.0～7.0 parts of Dyhard RU 100s, 3.5～6.0 parts of 2-ethyl monomethyl imidazoles, 2.5～5.0 parts of mphenylenediamines and the m-xylene diamines of selecting is as curing catalyst in invention.
Self-vulcanizing heat-resistance type flexible epoxy tackiness agent provided by the invention, the preferential scheme of selecting is, it is the Resins, epoxy of E51 that toughness reinforcing discharge ring epoxy resins adopts the trade mark, it is the Resins, epoxy of E20 that heatproof discharge ring epoxy resins adopts the trade mark, and adopting the trade mark as the resol of heatproof properties-correcting agent is the resol of F648.
Adopt the epoxy adhesive of technical scheme preparation of the present invention to have very high heat resistance and fabulous flexility, excellent in cushion effect.Experiment shows, epoxy adhesive of the present invention, resistance to impact shock under normal temperature condition is not less than 30MPa, and flexural strength is not less than 90MPa, and the rate of stretching is not less than 8%, shearing resistance is not less than 20MPa, even under 300 ℃ condition, its shearing resistance also is not less than 8MPa, and can be under 300 ℃ condition life-time service, therefore can under cohesive strength and the demanding environment of use temperature, use, can solve the inadhesive technical problem of prior art epoxy resin binder.
Epoxy adhesive provided by the invention uses very simple and convenient.Adhesive component that will encapsulate respectively during use and the curing component scene under room temperature (25 ± 5 ℃) condition are in proportion fully modulated mixing, promptly can be used for the bonding between structural part, bonded structural part just can reach best solid state through 5～7 hours, just can reach enough intensity through 24 hours.
Epoxy adhesive of the present invention has the use temperature height simultaneously, good toughness, excellent in cushion effect, the multiple excellent properties of solidified at ambient temperature, overcome the problem that the prior art epoxy adhesive exists, can be widely used in the bonding between facility structural parts such as civilian structure, train rail signal shielding, aerospacecraft structure, borer brake sheet.
Four, embodiment
Below umber among each embodiment be parts by weight.
Embodiment 1
The toughness reinforcing component in A, the adhesive component and the composition of heatproof component are in a kind of weight unit umber.
The composition of a, toughness reinforcing component:
100 parts of Resins, epoxy E51
20 parts of liquid nbr carboxyl terminals
30 parts of liquid hydroxy'terminated butadiene nitrile rubbers
4,10 parts of 4 '-diaminodiphenylmethane, four sense Resins, epoxy
The composition of b, heatproof component:
80 parts of Resins, epoxy E20
50 parts of heatproof properties-correcting agent
50 parts of silicone resins
48 parts of resol F648
Wherein the synthetic preparation of silicone resin oneself is by 40 parts of diphenyl dichlorosilanes, 10 parts of dimethyldichlorosilane(DMCS)s and 3 parts of synthetic making of boric acid.
Composed as follows in a kind of weight unit umber of B, curing component:
A, main body solidifying agent
100 parts of polyetheramines
B, curing catalyst
4 parts of hexanediamines
7 parts of Dyhard RU 100s
3.5 parts of 2-ethyl-Methylimidazoles
5.0 parts of mphenylenediamines
The composition of C, tackiness agent
Tackiness agent is counted by weight, is formed by the curing component hybrid modulation of 100 parts adhesive components and 40 parts.
The preparation method of tackiness agent is as follows:
Producing of A, adhesive component:
Earlier produce toughness reinforcing component and heatproof component respectively,, promptly make the adhesive component of tackiness agent then with two kinds of component hybrid package.
Producing of toughness reinforcing component: Resins, epoxy-E51 that proportioning is good, liquid nbr carboxyl terminal, liquid hydroxy'terminated butadiene nitrile rubber are heated to about 120 ℃, stirring reaction is about 2 hours under this temperature, after reaction finishes to be cooled to room temperature, add again proportioning good 4,4 '-diaminodiphenylmethane, four sense Resins, epoxy, behind the thorough mixing, promptly made the toughness reinforcing component in the adhesive component.
Producing of heatproof component: first synthetic silicone resin.The diphenyl dichlorosilane that proportioning is good, dimethyldichlorosilane(DMCS) and boric acid are heated to about 90 ℃, and reaction is about 1.5 hours under this temperature condition, promptly makes silicone resin.After silicone resin prepared, Resins, epoxy-E20 that proportioning is good, silicone resin, resol were heated to about 80 ℃, and reaction is about 1.5 hours under this temperature, is cooled to room temperature and promptly makes the heatproof component.
The toughness reinforcing component of producing is respectively mixed the back encapsulation with the heatproof component, promptly make the adhesive component of tackiness agent.
Producing of B, curing component:
The polyetheramine as the main body solidifying agent that proportioning is good mixes under room temperature (25 ± 5 ℃) as hexanediamine, Dyhard RU 100,2-ethyl-Methylimidazole, the mphenylenediamine of solidifying agent promotor, encapsulates behind the thorough mixing, promptly makes the curing component of tackiness agent.
C, use preparation:
Adhesive component and the curing component produced are carried out hybrid modulation in given ratio at the use scene, promptly make self-vulcanizing heat-resistance type flexible epoxy tackiness agent, be used for the bonding of structural part.
Embodiment 2
The toughness reinforcing component in A, the adhesive component and the composition of heatproof component and softening agent are all in a kind of weight unit umber.
The composition of a, toughness reinforcing component:
100 parts of Resins, epoxy-E50
40 parts of liquid nbr carboxyl terminals
4,5 parts of 4 '-diaminodiphenylmethane, four sense Resins, epoxy
6 parts of Resorcinol official energy Resins, epoxy
The composition of b, heatproof component:
90 parts of Resins, epoxy E20
60 parts of silicone resins
40 parts of resol F648
C, softening agent
2 parts of dibutyl phthalates
Composed as follows in a kind of weight unit umber of B, curing component:
A, main body solidifying agent
100 parts of polyetheramines
B, curing catalyst
6 parts of hexanediamines
6 parts of Dyhard RU 100s
4 parts of 2-ethyl-Methylimidazoles
8 parts of mphenylenediamines
The composition of C, tackiness agent
Tackiness agent is counted by weight, is formed by the curing component hybrid modulation of 100 parts adhesive components and 100 parts.
The preparation method of tackiness agent:
The adhesive preparation method of present embodiment is substantially the same manner as Example 1, and difference only is, because the used feed composition silicone resin of present embodiment is to be obtained by market purchasing, has therefore lacked the silicone resin synthetic method among the embodiment 1.
Embodiment 3
The toughness reinforcing component in A, the adhesive component and the composition of heatproof component and softening agent are all in a kind of weight unit umber.
The composition of a, toughness reinforcing component:
100 parts of Resins, epoxy-E51
25 parts of liquid nbr carboxyl terminals
20 parts of liquid hydroxy'terminated butadiene nitrile rubbers
4,7 parts of 4 '-diaminodiphenylmethane, four sense Resins, epoxy
4 parts of Resorcinol difunctional epoxy resin
The composition of b, heatproof component:
100 parts of Resins, epoxy (E20)
60 parts of silicone resins (synthetic certainly)
45 parts in resol (F648)
Wherein the synthetic voluntarily preparation of silicone resin is by 50 parts of diphenyl dichlorosilanes, 10 parts of dimethyldichlorosilane(DMCS)s and 5 parts of synthetic making of boric acid.
C, softening agent
5 parts of dibutyl phthalates
Composed as follows in a kind of weight unit umber of B, curing component:
A, main body solidifying agent
100 parts of polyetheramines
B, curing catalyst
5 parts of hexanediamines
4 parts of Dyhard RU 100s
6 parts of 2-ethyl-Methylimidazoles
2.5 parts of mphenylenediamines
5.0 parts of m-xylene diamines
The composition of C, tackiness agent
Tackiness agent is counted by weight, is formed by the curing component hybrid modulation of 100 parts adhesive components and 60 parts.
The preparation method of tackiness agent:
The adhesive preparation method of present embodiment is substantially the same manner as Example 1, just will add softening agent in the producing of adhesive component.
The specific embodiment of the present invention is not limited to the form of the foregoing description, and the content that those skilled in the art discloses according to the present invention is easy to implement with different proportionings.
Claims (7)
1, a kind of room curing and high temperature resistant type flexible epoxy tackiness agent is made up of phase blended adhesive component and curing component in use, it is characterized in that the weight ratio of two kinds of components is, 100 parts of adhesive components, and 30～100 parts of curing components, two kinds of components composed as follows:
A, adhesive component contain toughness reinforcing component and heatproof component, composed as follows in a kind of weight unit umber of two kinds of components:
A, toughness reinforcing component:
100 parts of toughness reinforcing discharge ring epoxy resins
30～50 parts of liquid acrylonitrile butadiene rubber toughner
5～12 parts of polyfunctional epoxy resin toughness reinforcing accelerants
B, heatproof component:
80～100 parts of heatproof discharge ring epoxy resins
50～60 parts of silicone resin heatproof properties-correcting agent
40～50 parts of resol heatproof properties-correcting agent
B, curing component are composed as follows in parts by weight:
100 parts in polyetheramine main body solidifying agent
20～30 parts of organic amine curing catalysts
Described toughness reinforcing discharge ring epoxy resins is selected from the Resins, epoxy that the trade mark is E51, described heatproof discharge ring epoxy resins is selected from the Resins, epoxy that the trade mark is E20, and described silicone resin heatproof properties-correcting agent is by 40～50 parts of diphenyl dichlorosilanes, 8～10 parts of dimethyldichlorosilane(DMCS)s and 3～5 parts of synthetic making of boric acid.
2, room curing and high temperature resistant type flexible epoxy tackiness agent as claimed in claim 1 is characterized in that said adhesive component also can contain the dibutyl phthalate softening agent, and its weight content is not more than 5 parts.
3, room curing and high temperature resistant type flexible epoxy tackiness agent as claimed in claim 1 or 2 is characterized in that the liquid acrylonitrile butadiene rubber toughner in the adhesive component is selected from liquid nbr carboxyl terminal and liquid hydroxy'terminated butadiene nitrile rubber.
4, room curing and high temperature resistant type flexible epoxy tackiness agent as claimed in claim 1 or 2, it is characterized in that the polyfunctional epoxy resin toughness reinforcing accelerant in the adhesive component is selected from 4,4 '-diaminodiphenylmethane, four sense Resins, epoxy and Resorcinol difunctional epoxy resin.
5, room curing and high temperature resistant type flexible epoxy tackiness agent as claimed in claim 1 or 2 is characterized in that the organic amine curing catalyst in the curing component is made up of four kinds of components in 2.5～5.0 parts of 3.0～7.0 parts of hexanediamines, 4.0～7.0 parts of Dyhard RU 100s, 3.5～6.0 parts of 2-ethyl monomethyl imidazoles, 2.5～5.0 parts of mphenylenediamines and the m-xylene diamines at least.
6 preparation methods as described any room curing and high temperature resistant type flexible epoxy tackiness agent of claim 1 to 5, its feature is as follows:
Producing of A, adhesive component:
Toughness reinforcing discharge ring epoxy resins and liquid acrylonitrile butadiene rubber toughner that proportioning in each claim in the claim 1 to 5 is good are heated to 100～150 ℃, stirring reaction is 1～2 hour under this temperature, after reaction finishes to be cooled to room temperature, add the good polyfunctional epoxy resin toughner of proportioning again, make toughness reinforcing component
Each claim proportioning is good in the claim 1 to 5 heatproof discharge ring epoxy resins, silicone resin heatproof properties-correcting agent and resol heatproof properties-correcting agent are heated to 50～100 ℃, stirring reaction is 1～2 hour under this temperature, be cooled to room temperature and promptly make the heatproof component
With toughness reinforcing component and the heatproof component hybrid package that makes, promptly make the adhesive component of tackiness agent,
Producing of B, curing component:
With the polyetheramine main body solidifying agent that each claim proportioning is good in the claim 1 to 5, the organic amine curing catalyst at room temperature mixes, and encapsulates behind the thorough mixing, promptly makes the curing component of tackiness agent.
C, adhesive component and the curing component for preparing carried out hybrid modulation in proportion at the use scene, promptly make room curing and high temperature resistant type flexible epoxy tackiness agent.
7, the preparation method of room curing and high temperature resistant type flexible epoxy tackiness agent as claimed in claim 8, it is characterized in that said silicone resin heatproof properties-correcting agent is heated to 80～95 ℃ by the diphenyl dichlorosilane that claim 5 proportioning is good, dimethyldichlorosilane(DMCS) and boric acid, 1～2 hour synthetic making of stirring reaction.
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| CN 200310111085 CN1244660C (en) | 2003-12-04 | 2003-12-04 | Preparation method of room temperature cured high temperature tolerant flexible epoxy adhesive |
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| CN 200310111085 CN1244660C (en) | 2003-12-04 | 2003-12-04 | Preparation method of room temperature cured high temperature tolerant flexible epoxy adhesive |
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| CN1244660C true CN1244660C (en) | 2006-03-08 |
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