CN100564473C - A kind of preparation method of modified epoxide resin embedding material - Google Patents
A kind of preparation method of modified epoxide resin embedding material Download PDFInfo
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- CN100564473C CN100564473C CN 200710056080 CN200710056080A CN100564473C CN 100564473 C CN100564473 C CN 100564473C CN 200710056080 CN200710056080 CN 200710056080 CN 200710056080 A CN200710056080 A CN 200710056080A CN 100564473 C CN100564473 C CN 100564473C
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Abstract
The present invention is a kind of high performance modified epoxide resin embedding material and preparation method thereof.This material is made of A liquid and B liquid, and A liquid comprises Resins, epoxy, organo montmorillonite, filler, and other auxiliary agent of base polyurethane prepolymer for use as modification, and B liquid comprises solidifying agent and promotor.This potting compound has low toxicity, wetting property is good, loading level is high, and its cured article has low linear expansivity, good weathering resistance and toughness; Preparation technology is simple for this potting compound, and excellent performance is applicable to the embedding of the electric elements of operating temperature range broad.
Description
Technical field
The invention belongs to the novel high polymer material field, particularly relate to a kind of preparation method of modified epoxide resin embedding material.
Background technology
Resins, epoxy is used widely in electric elements embedding field owing to have advantages such as the low and linear expansivity of excellent dielectric properties, mechanical property, adhesive property, corrosion resistance nature and cured article shrinking percentage is little.At present external Resins, epoxy A wide selection of colours and designs, some specific epoxy resins as: biphenyl type epoxy resin, dicyclopentadiene type Resins, epoxy, naphthalene nucleus type Resins, epoxy etc. since its good performance more and more obtain in the embedding field paying attention to, great majority these specific epoxy resin mechanical properties and thermal property excellences, viscosity is low, loading level is big, add these specific epoxy resins of part in PGL after filling mass filler, the anti-cracking of its cured article, weathering resistance is good, internal stress is low.And China's Resins, epoxy industrial structure is extremely unreasonable at present: common bisphenol A type epoxy resin proportion of production is near 95%, high-performance special Resins, epoxy only accounts for 5%, and in the global Resins, epoxy consumption ratio, common bisphenol A type epoxy resin accounts for 80%, all the other 20% are the specific epoxy resin, this causes on the one hand low-end market, and drug on the market, and high-end market supply falls short of demand.Some high performance electricians pour into a mould special epoxy resin, electronic devices and components embedding with a large amount of dependence on import of products such as Resins, epoxy.The epoxide resin encapsulation material of more present lower performances, it is base-material that domestic production producer great majority adopt bisphenol A type epoxy resin, end carboxyl liquid butyronitrile rubber (CTBN) is done or " strange scholar " toughner of domestic exploitation in recent years is epoxy resin toughened through adding, and adds filler, solidifying agent and other auxiliary agent again and mixes.Under the conditions such as, working conditions gentleness narrower at room temperature static environment, operating temperature range, this type of epoxide resin encapsulation material can satisfy customer requirements substantially, and for the embedding element of a few thing wider range (wide-40～120 ℃ as working temperature), deficiency such as cured article ubiquity poor toughness, easy to crack, weathering resistance difference.
Develop rapidly along with electronic apparatus industry, a kind of bisphenol A type epoxy resin with low side of active demand is a base-material, it is carried out obtaining high performance epoxide resin encapsulation material after the modification, satisfy the consumers demand of the contour performance epoxide resin encapsulation material of electronic apparatus, this development for electronic industry has important and practical meanings.
Summary of the invention
For the poor toughness of the Resins, epoxy Embedding Material cured article that solves present use, technical problem easy to crack, the invention provides a kind of modified epoxide resin embedding material and preparation method thereof.
The composition formation and the proportioning of a kind of modified epoxide resin embedding material provided by the invention are as follows:
This modified epoxide resin embedding material is made of A liquid and B liquid; The quality proportioning of described A liquid and B liquid is: (70～90): 100; Described A liquid and B liquid will be packed respectively and place;
The Resins, epoxy that described A liquid is the base polyurethane prepolymer for use as modification, organo montmorillonite, filler, thinner, coupling agent and pigment are formed, and B liquid is solidifying agent and promotor compositions;
The base polyurethane prepolymer for use as of described A liquid is to be made of isocyanic ester and polyvalent alcohol or hydroxy-terminated polybutadienes, and its mole proportioning is :-NCO :-OH=1.5～3;
Described isocyanic ester is '-diphenylmethane diisocyanate (MDI), tolylene diisocyanate (TDI) or polymethylene multi-phenenyl isocyanate (PAPI);
Polyvalent alcohol is PEG2000, PPG1000, PPG2000 or PTMEG2000;
The Resins, epoxy of described A liquid is bisphenol A type epoxy resin E-51 or E-44;
The quality proportioning of the base polyurethane prepolymer for use as of described A liquid and Resins, epoxy is: (5～40): 100;
The organo montmorillonite of described A liquid is made of tensio-active agent and sodium-based montmorillonite, and tensio-active agent and sodium-based montmorillonite quality proportioning are: (10～40): 100; Described tensio-active agent is: dodecyl primary amine, hexadecyl primary amine, hexadecyl quaternary ammonium salt, octadecyl primary amine or octadecyl quaternary ammonium salt;
The quality proportioning of the organo montmorillonite of described A liquid and Resins, epoxy is: (1～10): 100;
The filler of described A liquid is: fusion silica powder, crystal type silica powder, active micro silicon powder, lime carbonate, aluminum oxide or their mixture; The filler fineness is 200～1000 orders; The quality proportioning of filler and Resins, epoxy is: (100～450): 100;
The thinner of described A liquid is: polypropylene glycol diglycidyl ether, 1,4 butanediol diglycidyl ether, neopentylglycol diglycidyl ether, epoxy propane butyl ether, propylene oxide phenyl ether, benzyl glycidyl ether or their mixture; The quality proportioning of thinner and Resins, epoxy is: (5～40): 100;
The coupling agent of described A liquid is: γ-An Bingjisanyiyangjiguiwan (KH-550), γ-(2,3-epoxy third oxygen) propyl trimethoxy silicane (KH560), γ-(methacryloxypropyl) propyl trimethoxy silicane (KH570) or their mixture; The quality proportioning of coupling agent and filler is: (0.05～1.00): 100;
The pigment of described A liquid is high-carbon black pigment; The quality proportioning of pigment and filler is: (0.3～0.5): 100;
The solidifying agent of described B liquid and promotor quality proportioning are: (0.2～1): 100;
The solidifying agent of described B liquid is liquid methyl tetrahydrophthalic anhydride;
The promotor of described B liquid is: Benzyl base dimethylamine, cyano group imidazoles, glyoxal ethyline, 2-methyl-4-ethyl imidazol(e) or their mixture.
The preparation method of a kind of modified epoxide resin embedding material provided by the present invention, its step and condition are as follows:
By proportional quantity the isocyanic ester adding is furnished with agitator, thermometer, in the four-hole reactor of nitrogen protection pipe, be warming up to 70～140 ℃, under the logical nitrogen protection, under agitation condition, splash into polyvalent alcohol or hydroxy-terminated polybutadienes, dropwise through 0.5h, stir 0.5～3h down for 70～140 ℃, in reactor, add bisphenol A type epoxy resin subsequently in temperature, stir 0.5～3h down for 70～140 ℃ in temperature again, stop nitrogen protection then, be cooled to 50～90 ℃, add organo montmorillonite, stir 0.5～3h down for 50～90 ℃ in temperature, be cooled to 40 ℃ subsequently, press proportional quantity again and add filler, coupling agent, thinner and pigment mix, discharging makes A liquid;
Press proportional quantity solidifying agent and promotor are added in the reactor, stir, make B liquid.
Constitute modified epoxide resin embedding material by A liquid and B liquid; Described A liquid with the quality of B liquid than proportioning is: (70～90): 100.
Described A liquid and B liquid will be packed respectively and place.
The using method of a kind of modified epoxide resin embedding material provided by the present invention, its step and condition are as follows:
A. electric elements taken off rust, clean, dry;
B. A liquid is heated to 40～60 ℃ of temperature, vacuum defoamation 20～30min;
C. be (70～90) with A liquid and B liquid by the quality proportioning: 100 mixed are even,
Vacuum defoamation;
D. at preheating electric elements more than 80 ℃, then potting compound is injected in the electric elements vacuum defoamation;
E. electric elements are entered program curing, under 85～100 ℃ of temperature, solidify 1～3h, under 110～130 ℃ of temperature, solidify 1～3h, under 130～150 ℃ of temperature, solidify 1～3h;
F. after curing finished, electric elements naturally cooled to room temperature in baking oven.
About being described as follows of the Monitoring techniques index of the product performance of a kind of modified epoxide resin embedding material provided by the present invention:
The detection method that provides according to SJ/T 11125-1997 standard, to a kind of modified epoxide resin embedding material provided by the present invention cured article and the relevant performance of contrast product carried out check and analysis, the results are shown in the following table.
The performance of table 1 epoxide resin encapsulation material cured article
Beneficial effect: the performance of a kind of modified epoxide resin embedding material that the present invention is prepared is better than the performance of present like product, this potting compound has low toxicity, wetting property is good, loading level is high, and its cured article has low linear expansivity, good weathering resistance and toughness; Preparation technology is simple for this potting compound, and excellent performance is applicable to the embedding of the electric elements of operating temperature range broad.Economic balance shows: a kind of comprehensive cost of modified epoxide resin embedding material can satisfy the standard-required of Embedding Material fully far below the like product of being sold in the market.
Embodiment
Embodiment 1～4th, about the preparation method's of a kind of modified epoxide resin embedding material provided by the present invention embodiment.
Embodiment 1
3.00g MDI joined be furnished with agitator, in the 500mL four-hole boiling flask of thermometer, nitrogen protection pipe, be warming up to 85 ℃, logical nitrogen protection splashes into PPG200012.99g under stirring condition, dropwise behind 0.5h, stirs 2h under this temperature.In flask, add 74.95g bisphenol A type epoxy resin E-44 then, after 85 ℃ of temperature stir 2h down, stop nitrogen protection.Be cooled to 65 ℃ then, add the organo montmorillonite 3.75g that had handled by octadecyl trimethyl ammonium chloride, stir 1.5h down for 65 ℃ in temperature.Be cooled to 40 ℃ subsequently, add 600 order active micro silicon powder 224.85g, 14.99g epoxy propane butyl ether, 0.75g carbon black, mix, discharging makes A liquid.In the 100mL beaker, add the liquid methyl tetrahydrophthalic anhydride of 63.71g, 0.64g cyano group imidazoles, stir, make B liquid.
Constitute modified epoxide resin embedding material by A liquid and B liquid; Described A liquid with the quality of B liquid than proportioning is: 70: 100.Described A liquid and B liquid will be packed respectively and place.
Embodiment 2
4.43g MDI joined be furnished with agitator, in the 500mL four-hole boiling flask of thermometer, nitrogen protection pipe; be warming up to 120 ℃, logical nitrogen protection splashes into PTMG200017.68g under stirring condition; behind 0.5h, dropwise, stir 1.5h down for 120 ℃ in temperature.In flask, add 147.37g bisphenol A type epoxy resin E-51 then, keep stopping nitrogen protection behind 120 ℃ of stirring 1.5h.Be cooled to 55 ℃ then, add the organo montmorillonite 2.95g that had handled with the dodecyl primary amine, stir 2h down for 55 ℃ in temperature.Be cooled to 40 ℃ subsequently, add 400 order active micro silicon powder 147.37g, 14.74g polypropylene glycol diglycidyl ether, 0.74g carbon black, mix, discharging makes A liquid.In the 250mL beaker, add the liquid methyl tetrahydrophthalic anhydride of 125.26g, 0.63g glyoxal ethyline, stir, make B liquid.Constitute modified epoxide resin embedding material by A liquid and B liquid; Described A liquid with the quality of B liquid than proportioning is: 90: 100.Described A liquid and B liquid will be packed respectively and place.
Embodiment 3
10.67g PAPI joined be furnished with agitator, in the 500mL four-hole boiling flask of thermometer, nitrogen protection pipe; be warming up to 100 ℃, logical nitrogen protection dropwise adds hydroxy-terminated polybutadienes 8.01g under agitation condition; dropwise through 0.5h, stir 1.5h down for 100 ℃ in temperature.In flask, add 62.26g bisphenol A type epoxy resin E-51 then, stop nitrogen protection behind the stirring 2h down at 100 ℃.Be cooled to 75 ℃ then, add the organo montmorillonite 0.62g that had handled by cetyl trimethylammonium bromide, stir 1h down at 75 ℃.Be cooled to 40 ℃ subsequently, add 249.04g fusion silicon powder, 18.68g fat glycidyl ether, 0.75g carbon black, 1.25gKH560, mix, discharging makes A liquid.In the 100mL beaker, add the liquid methyl tetrahydrophthalic anhydride of 49.81g, 1.00g 2-methyl-4-ethyl imidazol(e), get B liquid after stirring.Constitute modified epoxide resin embedding material by A liquid and B liquid; Described A liquid with the quality of B liquid than proportioning is: 80: 100.Described A liquid and B liquid will be packed respectively and place.
Embodiment 4
3.60g TDI joined be furnished with agitator, in the 500mL four-hole boiling flask of thermometer, nitrogen protection pipe, be warming up to 75 ℃, logical nitrogen protection splashes into PPG100020.70g under stirring condition, dropwise behind 0.5h, stirs 2.5h down at 75 ℃.In flask, add 97.56g bisphenol A type epoxy resin E-51 then, stop nitrogen protection behind the stirring 2.5h down, be cooled to 50 ℃, add the organo montmorillonite 7.80g that had handled by the octadecyl primary amine, stir 2h down at 50 ℃ at 75 ℃.Be cooled to 40 ℃ subsequently, add 195.12g quartz type silicon powder, 24.39g propylene oxide phenyl ether, 0.73g carbon black, 0.98g KH550, mix, discharging makes A liquid.In the 150mL beaker, add the liquid methyl tetrahydrophthalic anhydride of 87.80g, 1.32g Benzyl base dimethylamine, stir, make B liquid.Constitute modified epoxide resin embedding material by A liquid and B liquid; Described A liquid with the quality of B liquid than proportioning is: 75: 100.Described A liquid and B liquid will be packed respectively and place.
The embodiment of using method
This example is the explanation about the using method of a kind of modified epoxide resin embedding material provided by the present invention.
A liquid is put into baking oven,, add B liquid then, mix the final vacuum deaeration in 50 ℃ of following vacuum defoamations of temperature.Electric elements are put into the inherent 80 ℃ of dry 0.5h of baking oven, then potting compound is injected in the electric elements vacuum defoamation.Condition of cure is 95 ℃ of 2h, 120 ℃ of 3h, 145 ℃ of 2h.Close baking oven after curing finishes, naturally cooling embedding part is to room temperature.Described A liquid with the quality of B liquid than proportioning is: (70～90): 100;
The performance index of the cured article of embodiment 1～4 one kind of modified epoxide resin embedding material are listed in the table 1.
Comparative Examples embodiment
This example is a Comparative Examples, is the contrast with potting compound TCG1695 commonly used in the market.
The TCG1695A liquid that money chemistry (Wuxi) company limited in capital is produced adds TCG1695B liquid after 50 ℃ of following vacuum defoamations, mix vacuum defoamation.Electric elements are put into the inherent 80 ℃ of dry 0.5h of baking oven, then potting compound is injected in the electric elements vacuum defoamation.Condition of cure is 80 ℃ of 2h, 100 ℃ of 2h, 130 ℃ of 3h.Close baking oven after curing finishes, naturally cooling embedding part is to room temperature, and the condensate performance that obtains sees Table 1.
By the performance index of embodiment and Comparative Examples cured article more as can be seen: the performance of a kind of modified epoxide resin embedding material that the present invention is prepared is better than the performance of present like product, economic balance shows: a kind of comprehensive cost of modified epoxide resin embedding material can satisfy the standard-required of Embedding Material fully far below the like product of being sold in the market.
Claims (2)
1. modified epoxide resin embedding material is characterized in that: the composition of a kind of modified epoxide resin embedding material provided by the invention constitute and proportioning as follows:
This modified epoxide resin embedding material is made of A liquid and B liquid; The quality proportioning of described A liquid and B liquid is: (70～90): 100; Described A liquid and B liquid will be packed respectively;
The Resins, epoxy that described A liquid is the base polyurethane prepolymer for use as modification, organo montmorillonite, filler, thinner, coupling agent and pigment are formed, and B liquid is solidifying agent and promotor compositions;
The base polyurethane prepolymer for use as of described A liquid is to be made of isocyanic ester and polyvalent alcohol or hydroxy-terminated polybutadienes, and its mole proportioning is :-NCO :-OH=1.5～3;
Described isocyanic ester is '-diphenylmethane diisocyanate, tolylene diisocyanate or polymethylene multi-phenenyl isocyanate;
Polyvalent alcohol is PEG2000, PPG1000, PPG2000 or PTMEG2000;
The Resins, epoxy of described A liquid is bisphenol A type epoxy resin E-51 or E-44;
The quality proportioning of the base polyurethane prepolymer for use as of described A liquid and Resins, epoxy is: (5～4O): 100;
The organo montmorillonite of described A liquid is made of tensio-active agent and sodium-based montmorillonite, and tensio-active agent and sodium-based montmorillonite quality proportioning are: (10～40): 100; Described tensio-active agent is: dodecyl primary amine, hexadecyl primary amine, hexadecyl quaternary ammonium salt, octadecyl primary amine or octadecyl quaternary ammonium salt;
The quality proportioning of the organo montmorillonite of described A liquid and Resins, epoxy is: (1～10): 100;
The filler of described A liquid is: fusion silica powder, crystal type silica powder, active micro silicon powder, lime carbonate, aluminum oxide or their mixture; The filler fineness is 200～1000 orders; The quality proportioning of filler and Resins, epoxy is: (100～450): 100;
The thinner of described A liquid is: polypropylene glycol diglycidyl ether, 1,4 butanediol diglycidyl ether, neopentylglycol diglycidyl ether, epoxy propane butyl ether, propylene oxide phenyl ether, benzyl glycidyl ether or their mixture; The quality proportioning of thinner and Resins, epoxy is: (5～40): 100;
The coupling agent of described A liquid is: γ-An Bingjisanyiyangjiguiwan, γ-(2,3-epoxy third oxygen) propyl trimethoxy silicane, γ-(methacryloxypropyl) propyl trimethoxy silicane or their mixture; The quality proportioning of coupling agent and filler is: (0.05～1.00): 100;
The pigment of described A liquid is high-carbon black pigment; The quality proportioning of pigment and filler is: (0.3～0.5): 100;
The solidifying agent of described B liquid and promotor quality proportioning are: (0.2～1): 100;
The solidifying agent of described B liquid is liquid methyl tetrahydrophthalic anhydride;
The promotor of described B liquid is: benzyldimethylamine, cyano group imidazoles, glyoxal ethyline, 2-methyl-4-ethyl imidazol(e) or their mixture.
2. the preparation method of a kind of modified epoxide resin embedding material as claimed in claim 1 is characterized in that, step and condition are as follows:
By proportional quantity the isocyanic ester adding is furnished with agitator, thermometer, in the four-hole reactor of nitrogen protection pipe, be warming up to 70～140 ℃, under the logical nitrogen protection, under agitation condition, splash into polyvalent alcohol or hydroxy-terminated polybutadienes, dropwise through 0.5h, stir 0.5～3h down for 70～140 ℃, in reactor, add bisphenol A type epoxy resin subsequently in temperature, stir 0.5～3h down for 70～140 ℃ in temperature again, stop nitrogen protection then, be cooled to 50～90 ℃, add organo montmorillonite, stir 0.5～3h down for 50～90 ℃ in temperature, be cooled to 40 ℃ subsequently, press proportional quantity again and add filler, coupling agent, thinner and pigment mix, discharging makes A liquid;
Press proportional quantity solidifying agent and promotor are added in the reactor, stir, make B liquid;
Constitute modified epoxide resin embedding material by A liquid and B liquid; Described A liquid with the quality of B liquid than proportioning is: (70～90): 100; Described A liquid and B liquid will be packed respectively.
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