CN1230477C - Freon-resistant resin composition and preparation process and use thereof - Google Patents
Freon-resistant resin composition and preparation process and use thereof Download PDFInfo
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- CN1230477C CN1230477C CN 03114357 CN03114357A CN1230477C CN 1230477 C CN1230477 C CN 1230477C CN 03114357 CN03114357 CN 03114357 CN 03114357 A CN03114357 A CN 03114357A CN 1230477 C CN1230477 C CN 1230477C
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Abstract
The present invention discloses a freon-resistant resin composition which comprises 5 to 30 wt% of epoxy resin with multiple functional groups, 5 to 35 wt% of linear epoxy resin, 5 to 50 wt% of multi-imide, 0 to 40 wt% of active diluting agent, 0 to 70 wt% of solvent, 5 to 50 wt% of liquid estolide and 0.1 to 2 wt% of peroxide initiator. The present invention also discloses a preparing method of the composition and uses of the composition in industry. The freon-resistant resin composition of the present invention maintains good freon-resistant performance of polyamide-imide resin and polyimide resin, and simultaneously has the advantages of good production, good technology of application and construction and environmental protection. The preparing method is simple, and the range of application of the composition is wide. The resin composition has the characteristic of low price.
Description
Technical field
The present invention relates to a kind of resin combination, particularly relate to a kind of freon resistant resin combination.The invention still further relates to the preparation method and its usage of above-mentioned resin combination.
Background technology
For a long time, the freon resistant insualtion resin composition adopts the polyamide-imide resin lacquer mostly; The polyimide resin lacquer.These resin paints have heat-resisting height, characteristics that the freon resistant performance is good.But these lacquers will use intensive polar solvent, as: NN-dimethyl formamide, NN-N,N-DIMETHYLACETAMIDE, dioxane etc.; The solidification value height, the time is long; Use complex manufacturing, harshness.In addition, the cost value costliness of lacquer.Owing to used intensive polar solvent, the most toxicity of these solvents wants high than usual vehicle, and therefore, the infringement that environment is caused is bigger.Owing to above-mentioned multiple reason makes the polyamide-imide resin lacquer; The use of polyimide resin lacquer has been subjected to certain limitation.
Summary of the invention
The purpose of this invention is to provide a kind of good freon resistant performance that had both kept polyamide-imide resin and polyimide resin lacquer, have good production and application and construction technology simultaneously and the freon resistant resin combination of environmental facies to the close friend.
Another object of the present invention provides the preparation method of above-mentioned freon resistant resin combination.
Another purpose of the present invention provides the purposes of above-mentioned freon resistant resin combination in industry.
Purpose of the present invention is achieved by the following technical programs.
Freon resistant resin combination of the present invention, contain following component by weight percentage:
A, polyfunctional epoxy resin 5%-30%;
B, linear epoxy resin 5%-35%;
C, multi-imide 5%-50%;
D, reactive thinner 0%-40%;
E, solvent 0%-70%;
F, liquid acid anhydrides 5%-50%;
G, peroxide initiator 0.1%-2%.
Polyfunctional epoxy resin wherein is the novolac epoxy of ester ring family's Resins, epoxy or functionality 〉=2.Linear epoxy resin wherein is the bisphenol A epoxide resin of oxirane value≤0.55.Multi-imide wherein is the polyimide oligomer of functionality 〉=2, preferred More Malay imide or bismaleimides or More Malay imide and bismaleimides.Reactive thinner wherein is ester ring family's epoxy active diluent or common epoxy active diluent.Solvent wherein is a low poison solvent, preferred F-20 solvent.Liquid acid anhydrides wherein is tetrahydrophthalic anhydride or Na Dike acid anhydrides or oleum lini acid anhydrides or tung oil acid anhydride.Peroxide initiator wherein can be middle temperature initiator, also can be high-temperature initiator.
Freon resistant resin combination of the present invention is faint yellow to the Vandyke brown transparent liquid.
Performance perameter was as follows after freon resistant resin combination Tetramune of the present invention solidified:
Color is yellowish, and to be clear to dark brown brown transparent;
Appearance of coat paint film light, smooth;
Cohesive force 〉=500N;
Volume specific resistance 〉=10
7M Ω .m;
Freon resistant performance 〉=25N (at 150 ℃, 168h, F
22. under the condition);
Electrical strength 〉=70MV/m;
Heat-resistance index 145-190 ℃.
The preparation method of freon resistant resin combination of the present invention may further comprise the steps:
Add the liquid acid anhydrides in the stainless steel oil bath reacting by heating still of a, belt stirrer, start and stir, heat;
B, when temperature of reaction kettle rises to 50 ℃, add the multi-imide resin measure, make temperature of reaction kettle in 0.5 hour, rise to 90 ℃-180 ℃ simultaneously;
C, isothermal reaction 0.5-5 hour, then, stop heating, continue to stir;
D, feeding cold oil are reduced to below 80 ℃ temperature of reaction kettle;
The solvent that e, adding measure continues to stir;
F, when reactant and solvent and or after reactive thinner mixes, add polyfunctional epoxy resin, linear epoxy resin and peroxide initiator successively;
Behind g, the thorough mixing, stop to stir;
H, filtration, packing.
The purposes characteristics of freon resistant resin combination of the present invention are, range of application is wider, can be used for freon resistant, water-fast, oil-resisting type electronic product, and application art can be taked wholely to soak, vacuum impregnation, drip and several different methods such as soak and construct.Be particularly suitable for making the good freon resistant lacquer of construction technology, be used for the refrigerator electric insulation coating layer.
Freon resistant resin combination of the present invention, polyimide oligomer wherein is in freon resistant that has guaranteed resin combination and outstanding electric property while, because its molecular weight is lower, active function groups is many, help with Resins, epoxy, reactive thinner and or solvent dissolve each other and form the stabilized resins system.
Freon resistant resin combination of the present invention, it is the adhesive property that utilizes Resins, epoxy outstanding that polyfunctional epoxy resin and linear epoxy resin are share; Outstanding electric, physical and mechanical properties with and outstanding processing performance, under the prerequisite of the least possible reduction resin combination thermotolerance of the present invention, assurance freon resistant performance, improve all round properties of product, especially improve the processing performance of resin combination, resin combination can be cured below 180 ℃.Simultaneously, also reduce the resin combination manufacturing cost to a certain extent.
Freon resistant resin combination of the present invention, use therein liquid acid anhydrides with Resins, epoxy and multi-imide resin oligopolymer reactive activity functional group, in resin combination, play solidifying agent, compatilizer and properties-correcting agent.The multi-imide oligopolymer can not produce precipitation in the presence of this acid anhydrides, has satisfactory stability.
The beneficial effect of freon resistant resin combination of the present invention is, both kept the good freon resistant performance of polyamide-imide resin and polyimide resin lacquer, have good production and application and construction technology simultaneously and to environmental facies to the close friend.Its preparation method is simple, and range of application is wider.This resin combination also has the characteristics of less expensive.
Embodiment
Below come by specific embodiment that the present invention is further illustrated.Following per-cent all is weight percents.
Embodiment 1: functionality is the More Malay imide 18% of 2.5-4.5; Bisphenol A epoxide resin 8%; Ester ring family Resins, epoxy 6%; Tung oil acid anhydride 20%; F-20 solvent 46%, peroxide initiator 2%.
Tung oil acid anhydride is added in the stainless steel oil bath reacting by heating still of belt stirrer, start heating, stir, when temperature of reaction kettle rises to 50 ℃, add the More Malay imide, make temperature of reaction kettle in 0.5 hour, rise to 160 ℃ simultaneously, continue to stir isothermal reaction 2 hours, stop heating then, continue to stir, and feed cold oil and make temperature of reaction kettle reduce to 60 ℃, add the F-20 solvent, continue to stir, after material mixes in the reactor, add ester ring family Resins, epoxy, bisphenol A epoxide resin adds peroxide initiator simultaneously, after thorough mixing is even, stop to stir, become the freon resistant resin combination of Vandyke brown transparent liquid after filtration, packing gets final product at last.
Embodiment 2: bismaleimides 10%, functionality 2.5-4 novolac epoxy 20%, bisphenol A epoxide resin 10%, oleum lini acid anhydrides 35%, F-20 solvent 24%, peroxide initiator 1%.
The oleum lini acid anhydrides is added in the stainless steel oil bath reacting by heating still of belt stirrer, start heating, stir, when temperature of reaction kettle rises to 50 ℃, add bismaleimides, make temperature of reaction kettle in 0.5 hour, rise to 90 ℃ simultaneously, continue to stir isothermal reaction 5 hours, stop heating then, continue to stir, and feed cold oil and make temperature of reaction kettle reduce to 60 ℃, add the F-20 solvent, continue to stir, after material mixes in the reactor, add novolac epoxy, bisphenol A epoxide resin adds peroxide initiator simultaneously, after thorough mixing is even, stop to stir, become the freon resistant resin combination of light yellow transparent liquid after filtration, packing gets final product at last.
Embodiment 3: the More Malay imide 30% of functionality 2.5-4.5; Linear epoxy resin 14%; Novolac epoxy 6%; Tung oil acid anhydride 30%; Epoxy active diluent 18.5%; Peroxide initiator 1.5%.
Tung oil acid anhydride is added in the stainless steel oil bath reacting by heating still of belt stirrer, start heating, stir, when temperature of reaction kettle rises to 50 ℃, add the More Malay imide, make temperature of reaction kettle in 0.5 hour, rise to 140 ℃ simultaneously, continue to stir isothermal reaction 4 hours, stop heating then, continue to stir, and feed cold oil and make temperature of reaction kettle reduce to 70 ℃, add the F-20 solvent, continue to stir, after material mixes in the reactor, add novolac epoxy, linear epoxy resin adds peroxide initiator simultaneously, after thorough mixing is even, stop to stir, become the freon resistant resin combination of light yellow transparent liquid after filtration, packing gets final product at last.
Embodiment 4: bismaleimides 5%, the More Malay imide 5% of functionality 2.5-4.5, linear epoxy resin 10%, ester ring family Resins, epoxy 10%, oleum lini acid anhydrides 20%, F-20 solvent 49.5%, peroxide initiator 0.5%.
The oleum lini acid anhydrides is added in the stainless steel oil bath reacting by heating still of belt stirrer, start heating, stir, when temperature of reaction kettle rises to 50 ℃, add bismaleimides and More Malay imide, make temperature of reaction kettle in 0.5 hour, rise to 180 ℃ simultaneously, continue to stir isothermal reaction 0.5 hour, stop heating then, continue to stir, and feed cold oil and make temperature of reaction kettle reduce to 60 ℃, add the F-20 solvent, continue to stir, after material mixes in the reactor, add novolac epoxy, linear epoxy resin adds peroxide initiator simultaneously, after thorough mixing is even, stop to stir, become the freon resistant resin combination of Vandyke brown look transparent liquid after filtration, packing gets final product at last.
Embodiment 5: bismaleimides 20%, the More Malay imide 20% of functionality 2.5-4.5, linear epoxy resin 5%, novolac epoxy 10%, tung oil acid anhydride 30%, F-20 solvent 10%, epoxy type reactive thinner 5%, peroxide initiator 0.1%.
Tung oil acid anhydride is added in the stainless steel oil bath reacting by heating still of belt stirrer, start heating, stir, when temperature of reaction kettle rises to 50 ℃, add bismaleimides and More Malay imide, make temperature of reaction kettle in 0.5 hour, rise to 140 ℃ simultaneously, continue to stir isothermal reaction 4 hours, stop heating then, continue to stir, and feed cold oil and make temperature of reaction kettle reduce to 60 ℃, add the F-20 solvent, continue to stir, after material mixes in the reactor, add novolac epoxy, linear epoxy resin adds peroxide initiator simultaneously, after thorough mixing is even, stop to stir, become the freon resistant resin combination of light yellow transparent liquid after filtration, packing gets final product at last.
Claims (5)
1, freon resistant resin combination is characterized in that: contain following component by weight percentage:
A, polyfunctional epoxy resin 5%~30%,
B, linear epoxy resin 5%-35%,
C, multi-imide 5%-50%,
D, reactive thinner 0%~40%,
E, solvent 0%~70%,
F, liquid acid anhydrides 5%~50%
G, peroxide initiator 0.1%~2%
Wherein, polyfunctional epoxy resin is the novolac epoxy of ester ring family's Resins, epoxy or functionality 〉=2; Linear epoxy resin is the bisphenol A type epoxy resin of oxirane value≤0.55; Multi-imide is the polyimide oligomer of functionality 〉=2; Reactive thinner is ester ring family's epoxy active diluent or common epoxy active diluent; Solvent is a low poison solvent; Peroxide initiator is middle temperature initiator or high-temperature initiator; Multi-imide is More Malay imide or bismaleimides or More Malay imide and bismaleimides; Solvent is the F-20 solvent; The liquid acid anhydrides is tetrahydrophthalic anhydride, Na Dike acid anhydrides, oleum lini acid anhydrides or tung oil acid anhydride.
2, the preparation method of freon resistant resin combination according to claim 1 is characterized in that: may further comprise the steps:
A, in the oil bath reactor, add the liquid acid anhydrides, stir, heating;
B, when temperature of reactor rises to 50 ℃, add the multi-imide resin measure, make temperature of reactor in 0.5 hour, rise to 90 ℃~180 ℃ simultaneously
C, isothermal reaction 0.5~5 hour. then, stop heating, continue to stir;
D, feeding cold oil cool to below 80 ℃ reactor;
The solvent that e, adding measure continues to stir;
F, when reactant and solvent and (or) after reactive thinner mixes, be sequentially added into polyfunctional epoxy resin, linear epoxy resin and additive;
G, behind thorough mixing, stop to stir;
H, filtration, packing.
3, the preparation method of freon resistant resin combination according to claim 2 is characterized in that: the reactor described in the step a is the stainless steel oil bath reacting by heating still of belt stirrer.
4, freon resistant resin combination according to claim 1, be applied to freon resistant, water-fast or oil-resisting type electronic product wholely soak, vacuum impregnation or drip soaking technology.
5, freon resistant resin combination according to claim 1 is applied to the refrigerator electric insulation coating layer.
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CN 03114357 CN1230477C (en) | 2003-04-30 | 2003-04-30 | Freon-resistant resin composition and preparation process and use thereof |
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CN 03114357 CN1230477C (en) | 2003-04-30 | 2003-04-30 | Freon-resistant resin composition and preparation process and use thereof |
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CN1450132A CN1450132A (en) | 2003-10-22 |
CN1230477C true CN1230477C (en) | 2005-12-07 |
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CN102533059A (en) * | 2011-12-21 | 2012-07-04 | 株洲时代新材料科技股份有限公司 | Solvent-free impregnating varnish and preparation and use methods thereof |
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