CN101235269B - Double-component epoxy resin embedding adhesive and its preparation method and can sealing technique - Google Patents
Double-component epoxy resin embedding adhesive and its preparation method and can sealing technique Download PDFInfo
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Abstract
Bi-component epoxy resin pouring sealant and the preparation and the potting technology are disclosed, which comprises an epoxy resin A component and a cursing agent B component, wherein the curing agent B component at least comprises the mixing curing agent of cashew shell oil modified amine curing agent and fatty amine curing agent. The potting technology comprises mixing and stirring evenly the epoxy resin A component and the curing agent B agent to conduct the potting, and spraying a layer of absolute alcohol on the surface of the pouring sealant after 10-15 minutes. The advantages are that gel time is prolonged through adopting the mixing curing agent of cashew shell oil modified amine curing agent and fatty amine curing agent, the requirement of operation time is fulfilled, and the operation time can reach 20-30 minutes, thereby being beneficial for the encapsulation of housing with large capacity, and the pouring sealant of the invention has the effect of fast curing, wherein the curing time is 1-3 hours, and defoaming is accelerated through spraying a layer of absolute alcohol on the surface of colloid after pouring, thereby making the solid gel surface bright and flat after curing.
Description
Technical field
The present invention relates to a kind of double-component epoxy resin embedding adhesive and preparation method thereof and can sealing technique, especially a kind of a kind of component that adopts cashew nut oil modified amine as solidifying agent is with the double-component epoxy resin embedding adhesive that is combined into mixed curing agent of aliphatic amide and other solidifying agent.
Background technology
Concerning most of double-component epoxy resin embedding adhesives, the operating time is long, correspondingly set time also long, vice versa.Requiring short occasion set time, because the operating time is short, then can not satisfy a big housing embedding of glue consumption, often encapsulating work is not also finished, gel has taken place in the glue of first watering, can not flow, the glue that the later stage is irritated can not fully flow in the slit of housing, solidifies the easy cavity that forms in the middle of the back.
If prolong gel time simply, also will prolong corresponding set time, and its completely solidified time of the two-pack glue of gel time about 1 hour was greater than 24 hours usually, and for the construction occasion that operation efficiency has higher requirements, this time is oversize.
Another problem that fast type glue admittedly in use occurs is that because gel time is short, the bubble that produces in the whipping process also has little time to eliminate, glue has lost flowability, the surface residual bubble can not be eliminated fully, causes the adhesive curing rear surface that a large amount of small bubbles are arranged, and influences surface luster.In recent years, all carried out research both at home and abroad to cashew nut shell oil, the cashew nut shell oil epoxy curing agent is mainly made by cashew nut oil modified, China Patent No. ZL02116454.1 has reported a kind of synthetic method of cashew nut shell oil epoxy curing agent, by cashew nut shell oil, formaldehyde and aliphatic amide make long-chain through mannich reaction and replace phenolic aldehyde amine---cashew nut amine, contain phenolic hydroxyl group and Armeen and secondary amine in the molecular structure, when reacting with Resins, epoxy, amido in the molecule and epoxy group(ing) generation polyaddition reaction, hydrogen on the phenolic hydroxyl group has then played promotor, this solidifying agent curing speed is accelerated, and can satisfy the requirement of low-temperature curing.
Can make the two-pack joint sealant with cashew nut oil modified amine to the solidification of Resins, epoxy, China Patent No. ZL200410047913.5 discloses a kind of like this joint sealant, mention cashew nut oil modified amine separately as the B component of joint sealant, this joint sealant has quick-setting characteristics, but does not mention the surface luster property problem of cured glue.Applicant of the present invention is through finding after the experiment repeatedly, cashew nut shell oil is used as the solidifying agent of joint sealant separately, solidifying the rear surface all has a large amount of bubbles not eliminate, this mainly contains the reason of two aspects: the one, and the viscosity of cashew nut oil modified amine hardener is bigger, often to reach several thousand to several ten thousand cps, be unfavorable for the elimination of open bubble; The 2nd, because, there is the defective that encapsulating rear surface tension force is big, be not easy froth breaking as epoxy curing agent in existing cashew nut oil modified amine, also need to carry out some aftertreatment work, so that mixed epoxy resin solidifying system has lower surface tension.
Summary of the invention
Technical problem to be solved by this invention is to provide that a kind of to satisfy the operating time long, fast setting, and solve cured glue surface glossy double-component epoxy resin embedding adhesive.
Another technical problem to be solved by this invention is to provide the preparation method of above-mentioned double-component epoxy resin embedding adhesive.
A technical problem more to be solved by this invention is to provide the can sealing technique of above-mentioned double-component epoxy resin embedding adhesive.
The present invention solves the problems of the technologies described above the technical scheme of being taked: a kind of double-component epoxy resin embedding adhesive, comprise Resins, epoxy A component and solidifying agent B component, wherein, described solidifying agent B component is for comprising the mixed curing agent of cashew nut oil modified amine hardener and fatty amine curing agent at least.
The present invention is by using cashew nut oil modified amine and aliphatic amide with, the operating time of gained curing system can reach 20～30 minutes, foreshorten to 1～3 hour set time, compare with simple aliphatic amide curing system, mixing cured system of the present invention, change comparatively smooth in time in initial stage viscosity, the twice required time that the viscosity of curing system increases to initial viscosity is respectively more than 20 minutes, and this illustrates that the used mixing cured system of the present invention is longer than the independent aliphatic amide curing system operating time.In addition, adopt the mixture solidified agent, reduced the viscosity of cashew nut oil modified amine, weakened the problem of independent cashew nut oil modified amine curing system inherent deaeration difficulty simultaneously.
Further, solidifying agent B component of the present invention is preferably 10～15 parts of fatty amine curing agents, the mixed curing agent of 2～6 parts of cashew nut oil modified amine and 2～6 parts of polyetheramines; Or be the mixed curing agent of 12～15 parts of fatty amines and 12～15 parts of cashew nut oil modified amine.
On the basis of such scheme, described double-component epoxy resin embedding adhesive comprises:
Resins, epoxy A component is 100 parts of bisphenol A epoxide resins, 120～180 parts of fillers, 1～5 part of thixotropic agent, 15～30 parts of reactive thinners, 0.8～3 part of defoamer, 1～3 part of mineral black;
And solidifying agent B component, be 10～15 parts of fatty amine curing agents, the mixed curing agent of 2～6 parts of cashew nut oil modified amine and 2～6 parts of polyetheramines, or be the mixed curing agent of 12～15 parts of fatty amines and 12～15 parts of cashew nut oil modified amine;
Wherein, the blending ratio of described Resins, epoxy A component and solidifying agent B component is 4～5: 1.
On the basis of such scheme, the filler in the Resins, epoxy A component is 90～130 parts of precipitator method barium sulfate and 30～50 parts of lime carbonate.
Thixotropic agent in the Resins, epoxy A component is a thermal silica, and reactive thinner is a benzyl glycidyl ether, and defoamer is a polysiloxane defoamers.
A kind of preparation method at above-mentioned double-component epoxy resin embedding adhesive, prepare A, B component respectively, the preparation of described Resins, epoxy A component comprises: add reactive thinner, defoamer and mineral black, add filler and thixotropic agent then, normal pressure stirred after 2～5 minutes in stirrer, vacuumize, improve stirring velocity, vacuum stirring 20～40 minutes;
The preparation of solidifying agent B component comprises: the preparation of solidifying agent B component comprises: each component was stirred in the high-speed stirring still 5～20 minutes;
Concrete step is:
The preparation of Resins, epoxy A component comprises: earlier successively with bisphenol A epoxide resin, reactive thinner, defoamer and mineral black join in the planet stirring tank that has vaccum-pumping equipment, add barium sulfate then, the white carbon black of the lime carbonate and the precipitator method, cover kettle cover, do not vacuumize, stirring at low speed 2～5 minutes, open vacuum apparatus then, improve mixing speed, vacuum stirring 20～40 minutes, wherein, it is 5～30rpm that normal pressure stirs the revolution rotating speed, the rotation rotating speed is 100～400rpm, vacuum stirring revolution rotating speed is 10～40rpm, and the rotation rotating speed is 200～800rpm, and vacuum tightness is 0.05～0.10Mpa;
The preparation of described solidifying agent B component comprises: will successively aliphatic amide, cashew nut oil modified amine, polyetheramine (also can not adding) be joined in the high-speed stirring still of 300ml, rotating speed 200～800rpm stirred 5～20 minutes down.
Can sealing technique at above-mentioned double-component epoxy resin embedding adhesive, described solidifying agent B component comprises the mixed curing agent of cashew nut oil modified amine hardener and fatty amine curing agent at least, with Resins, epoxy A component and solidifying agent B component mixing and stirring, carry out potting, spray one deck raw spirit on the joint sealant surface after 10～15 minutes.
The embedding time of described Resins, epoxy A component and solidifying agent B component is 20～30 minutes, and be 1～3 hour the set time after the embedding, is not less than 80 to solidifying back shore hardness D.
This processing step is another emphasis of the present invention, because joint sealant can produce the bubble of upwards emerging in a large number in solidification process, and make joint sealant surface, curing back not bright and clean, so in can sealing technique, one deck dehydrated alcohol is sprayed on colloid demonstration surface outside, to reduce its surface tension, help deaeration, solved the problem of above-mentioned cashew nut shell oil epoxy curing systems deaeration difficulty.
At the purposes of above-mentioned double-component epoxy resin embedding adhesive, can be used for requiring in the mass production fast setting and can not or the embedding of the big-and-middle-sized equipment of inconvenience heating, as the embedding of big-and-middle-sized metal detection equipment etc.
The method of measuring this glue operating time and set time also is one of content of this research, because quick solidifying, gel time is short, the gelation process thermal discharge is big, and the temperature height is easy to occur sudden and violent poly-phenomenon behind the encapsulating, be difficult to the operating time and the set time of more different glue, this research is specially a diameter 8cm, the jerrycan of high 1.5cm by being filled in the jerrycan of will stirring.Because surface-area is big, quickened the heat radiation process like this, reduced colloid temperature in the gelation process, prolonged operating time and set time, made easier compare operation time and set time between the glue of different ingredients.
The invention has the beneficial effects as follows:
1, adopt cashew nut oil modified amine of the present invention and aliphatic amide mixed curing agent, prolonged its gel time, satisfy the demand of operating time, the potting time can reach 20～30 minutes, helps the embedding of big volume housing;
2, joint sealant of the present invention has quick-setting effect, and be 1～3 hour set time;
3, by spraying one deck raw spirit at colloid surface behind the encapsulating, quicken froth breaking, make soon to have bright even curface after the type adhesive curing admittedly.
Description of drawings
Fig. 1 is the viscosity change curve of different ingredients solidifying agent of the present invention.
Embodiment
Embodiment 1
(1) preparation of Resins, epoxy A component:
In the 500ml planetary mixer, add the 200g bisphenol A epoxide resin, add 40g reactive thinner, 1.6g defoamer and 2g black slurry successively, add 210g process white, 90g lime carbonate, the white carbon black of 4g vapor phase process then, at the revolution rotating speed is 5rpm, the rotation rotating speed is under the 100rpm, does not vacuumize, and stirs 5 minutes, stop to stir, open vaccum-pumping equipment, when treating that vacuum tightness reaches 0.09Mpa, begin to stir, the revolution rotating speed is 30rpm, the rotation rotating speed is 300rpm, stirs 30 minutes, stops to stir, remove vacuum, discharging;
(2) preparation of solidifying agent B component:
Take by weighing 48g aliphatic amide, the cashew nut oil modified amine of 20g and 12g polyetheramine respectively in 300ml high-speed stirring still, rotating speed 300rpm stirred 5 minutes down.
Accurately take by weighing above-mentioned A component of 100g and the above-mentioned B component of 20g, stir and make joint sealant.
The mensuration of operating time and set time: pouring the glue that stirs into a diameter is 8cm, height is in the jerrycan of 1.5cm, behind the encapsulating 10 minutes, spray one deck raw spirit with watering can on its surface, observing colloid is meant that herein the middle shore hardness D of colloid reached for 70 used times set time because viscosity increases time and the set time that the wire drawing phenomenon do not occur.
Embodiment 2
(1) preparation of Resins, epoxy A component: with embodiment 1
(2) preparation of solidifying agent B component:
Take by weighing 48g aliphatic amide, the cashew nut oil modified amine of 16g and 16g polyetheramine respectively in 300ml high-speed stirring still, rotating speed 300rpm stirred 5 minutes down.
Accurately take by weighing above-mentioned A component of 100g and the above-mentioned B component of 20g, stir and make joint sealant.
The mensuration of operating time and set time: with embodiment 1
Embodiment 3
(1) preparation of Resins, epoxy A component: with embodiment 1
(2) preparation of solidifying agent B component:
Take by weighing the cashew nut oil modified amine of 30g aliphatic amide and 30g respectively in 300ml high-speed stirring still, rotating speed 300rpm stirred 5 minutes down.
Accurately take by weighing above-mentioned A component of 100g and the above-mentioned B component of 20g, stir and make joint sealant.
The mensuration of operating time and set time: with embodiment 1
Comparative example
(1) preparation of Resins, epoxy A component: with embodiment 1
(2) preparation of solidifying agent B component:
Take by weighing the 80g aliphatic amide respectively in 300ml high-speed stirring still, rotating speed 300rpm stirred 5 minutes down.
The operating time and the set time of different ingredients potting glue are as shown in table 1:
Table 1
| Numbering | Aliphatic amide/g | Cashew nut oil modified amine/g | Polyetheramine/g | Operating time/min | Set time/min |
| Embodiment 1 | 12 | 5 | 3 | 30 | 85 |
| Embodiment 2 | 12 | 4 | 4 | 23 | 73 |
| Embodiment 3 | 20 | - | - | 18 | 90 |
See also Fig. 1 for shown in the viscosity change curve of different ingredients solidifying agent of the present invention, compare with simple fatty amine curing agent, mixed curing agent of the present invention changes comparatively smooth in time in initial stage viscosity.The twice required time that the viscosity of three curing systems increases to initial viscosity was respectively 30 minutes, 23 minutes and 18 minutes, and this explanation used mixed curing agent operating time of the present invention is longer, and set time is short than comparative example.
Claims (6)
1. double-component epoxy resin embedding adhesive, comprise Resins, epoxy A component and solidifying agent B component, it is characterized in that: solidifying agent B component is for comprising the mixed curing agent of cashew nut oil modified amine hardener and fatty amine curing agent at least, described solidifying agent B component is counted 10～15 parts of fatty amine curing agents by weight, the mixed curing agent of 2～6 parts of cashew nut oil modified amine and 2～6 parts of polyetheramines; Or be the mixed curing agent of 12～15 parts of fatty amines and 12～15 parts of cashew nut oil modified amine, wherein,
Described double-component epoxy resin embedding adhesive comprises:
Resins, epoxy A component is 100 parts of bisphenol A epoxide resins, 120～180 parts of fillers, 1～5 part of thixotropic agent, 15～30 parts of reactive thinners, 0.8～3 part of defoamer, 1～3 part of mineral black; And solidifying agent B component;
The blending ratio of described Resins, epoxy A component and solidifying agent B component is 4～5: 1; Described filler is 90～130 parts of precipitator method barium sulfate and 30～50 parts of lime carbonate,
Described thixotropic agent is a thermal silica, and reactive thinner is a benzyl glycidyl ether, and defoamer is a polysiloxane defoamers.
2. at the preparation method of the double-component epoxy resin embedding adhesive of claim 1:
The preparation of Resins, epoxy A component comprises: add reactive thinner, defoamer and mineral black, add filler and thixotropic agent then, normal pressure stirred after 2～5 minutes in stirrer, vacuumized, and improved stirring velocity, vacuum stirring 20～40 minutes;
The preparation of solidifying agent B component comprises: each component was stirred in the high-speed stirring still 5～20 minutes;
Wherein, Resins, epoxy A component is 1～5 part of 100 parts of bisphenol A epoxide resin, 120～180 parts of fillers, thixotropic agent, 15～30 parts of reactive thinners, 0.8～3 part of defoamer, 1～3 part of mineral black;
Solidifying agent B component is 10～15 parts of fatty amine curing agents, the mixed curing agent of 2～6 parts of cashew nut oil modified amine and 2～6 parts of polyetheramines, or be the mixed curing agent of 12～15 parts of fatty amines and 12～15 parts of cashew nut oil modified amine;
The blending ratio of described Resins, epoxy A component and solidifying agent B component is 4～5: 1.
3. the preparation method of double-component epoxy resin embedding adhesive according to claim 2, it is characterized in that: it is 5～30rpm that described Resins, epoxy A component normal pressure stirs the revolution rotating speed, the rotation rotating speed is 100～400rpm, vacuum stirring revolution rotating speed is 10～40rpm, the rotation rotating speed is 200～800rpm, and vacuum tightness is 0.05～0.10Mpa; Described solidifying agent B component mixing speed is 200～800rpm.
4. at the can sealing technique of the described double-component epoxy resin embedding adhesive of claim 1, the two-pack joint sealant comprises Resins, epoxy A component and solidifying agent B component, it is characterized in that: described solidifying agent B component comprises the mixed curing agent of cashew nut oil modified amine hardener and fatty amine curing agent at least, with Resins, epoxy A component and solidifying agent B component mixing and stirring, carry out potting, spray one deck raw spirit on the joint sealant surface after 10～15 minutes.
5. the can sealing technique of double-component epoxy resin embedding adhesive according to claim 4, it is characterized in that: the embedding time of described Resins, epoxy A component and solidifying agent B component is 20～30 minutes, be 1～3 hour the set time after the embedding, solidifies back shore hardness D and be not less than 80.
6. at the purposes of the described double-component epoxy resin embedding adhesive of claim 1, the embedding of the big-and-middle-sized metal detection equipment that is used to produce in batches.
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