CN1523057A - Resin composition and rheostat - Google Patents
Resin composition and rheostat Download PDFInfo
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- CN1523057A CN1523057A CNA2004100041332A CN200410004133A CN1523057A CN 1523057 A CN1523057 A CN 1523057A CN A2004100041332 A CNA2004100041332 A CN A2004100041332A CN 200410004133 A CN200410004133 A CN 200410004133A CN 1523057 A CN1523057 A CN 1523057A
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Abstract
Provided is a resin composition having a high flame retardant property without using a halogen and red phosphorus-based flame retardant, further excellent in the balance of electric insulation, heat shock resistance, casting workability and sedimentation stability. This resin composition is provided by consisting of a bisphenol A type liquid state epoxy resin, a dimer acid-modified epoxy resin and a metal hydroxide of which surface is treated with a fatty acid as essential components, and having 40-300 phr blending amount of the metal hydroxide of which surface is treated with the fatty acid. Alternatively, the resin composition is provided by consisting of the bisphenol A type liquid state epoxy resin, the dimer acid-modified epoxy resin, the metal hydroxide of which surface is treated with the fatty acid and the metal hydroxide of which surface is not treated as essential components, and having 40-150 phr blending amount of the metal hydroxide of which surface is treated with the fatty acid and 175-300 phr total blending amount of the metal hydroxide of which surface is treated with the fatty acid and the metal hydroxide of which surface is not treated.
Description
Technical field
The present invention relates to not produce unnecessary gas and have good resin combination of balance between simultaneously electrical insulating property of high flame retardant, resistance to sudden heating, casting operation, the sedimentation stability and the variohm that uses this resin combination.
Background technology
Being used for for example insulated enclosure of the high pressure parts such as focus pack of the kickback transformer of TV developing device, is to be undertaken by injecting potting resin under the state that is placed into casing at circuit substrate.In this case, the cast resin that requires to be used for the insulated enclosure of high pressure part has high-caliber flame retardant resistance, electrical insulating property, resistance to sudden heating and casting operation.
Because electrical insulating property, casting operation, cost aspect are good, as the resin that is used for this purposes, usually use Resins, epoxy.In general, Resins, epoxy is combustible material, even adopt the structure of such Resins, epoxy, also needs to be processed into high flame retardant when using as the high pressure part.When giving ethoxyline resin antiflaming, for the decline with the original good characteristic of Resins, epoxy is suppressed to minimum, the method that has proposed at present is to cooperate halogen or the red phosphorus based flame retardant that is expected the high flame retardant effect with few consumption.
Yet the halogen fire retardant might produce the gas of halogen when burning, and the trend of its use of control is arranged.In addition, the red phosphorus based flame retardant at high temperature also might produce Phosphorus gas, so the trend of its use of control is also arranged.Therefore, need not use halogen and red phosphorus based flame retardant and have high flame retardant and electrical insulating property, resistance to sudden heating, casting operation between the resin combination used of the good high pressure part casting of balance.
At present, in order under the condition of not using halogen and red phosphorus based flame retardant, to give the Resins, epoxy high flame retardant, proposed to fill the method (with reference to patent documentation 1,2,3) of metal hydroxidess such as aluminium hydroxide, magnesium hydroxide at the resin camber.
[patent documentation 1] spy opens flat 9-241483 communique (full page)
[patent documentation 2] spy opens flat 5-25369 communique (full page)
[patent documentation 3] spy opens flat 11-116777 communique (full page)
Yet, in the method for present highly-filled metal hydroxides,, have the problem of casting operation decline because the viscosity of resin rises.In addition,, must carry out stir process during use with the material of dispersing and settling once more, thereby have the problem that needs numerous and diverse operation because the sedimentation of packing material and can form the settled layer of hard in when keeping.
Summary of the invention
Therefore, the object of the present invention is to provide at good resin combination and the variohm of balance that has under the condition of not using halogen and red phosphorus based flame retardant between high flame retardant and electrical insulating property, resistance to sudden heating, casting operation, the sedimentation stability.
The 1st resin combination of the present invention, be characterised in that the metal hydroxides that has carried out fatty acid treatment with bisphenol A-type liquid epoxy resin, dimer acid modified Resins, epoxy, surface is a neccessary composition, and the combined amount that the metal hydroxides of fatty acid treatment has been carried out on above-mentioned surface is 40phr～300phr.
According to the 1st resin combination of the present invention, constitute by the Resins, epoxy that contains bisphenol A-type liquid epoxy resin and dimer acid modified Resins, epoxy as neccessary composition, therefore can have high electrical insulating property and resistance to sudden heating concurrently.In addition, in this resin combination, be 40phr～300phr because the combined amount of the metal hydroxides of fatty acid treatment has been carried out on the surface, metal hydroxides becomes easy affinity and easy the dispersion in aqueous resin, therefore is difficult to sedimentation.By mixed metal hydroxides, can improve the flame retardant resistance of Resins, epoxy, also can avoid producing simultaneously unnecessary gas.
Here, phr (parts per hundred resin) is meant the addition (weight part) with respect to 100 weight part Resins, epoxy.In addition, carried out the combined amount of the metal hydroxides of fatty acid treatment for the surface, " 40phr～300phr " is meant more than the 40phr and below 300phr.
The 2nd resin combination of the present invention, be characterised in that with bisphenol A-type liquid epoxy resin, dimer acid modified Resins, epoxy, surperficial metal hydroxides and the surperficial untreated metal hydroxides that has carried out fatty acid treatment be neccessary composition, and the combined amount that the metal hydroxides of fatty acid treatment has been carried out on above-mentioned surface is 40phr～150phr, and total combined amount that the untreated metal hydroxides of metal hydroxides and above-mentioned surface of fatty acid treatment has been carried out on above-mentioned surface is 175phr～300phr.
According to the 2nd resin combination of the present invention, constitute by the Resins, epoxy that contains bisphenol A-type liquid epoxy resin and dimer acid modified Resins, epoxy as neccessary composition, therefore can have high electrical insulating property and resistance to sudden heating concurrently.In addition, in this resin combination, since according to the mixed of requirement the surface carried out the metal hydroxides and the surperficial untreated metal hydroxides of fatty acid treatment, become easy affinity and disperseing easily of metal hydroxides in aqueous resin, therefore free settling not.By mixed metal hydroxides, can improve the flame retardant resistance of Resins, epoxy, also can avoid producing simultaneously unnecessary gas.
Here, phr is meant the addition (weight part) with respect to 100 weight part Resins, epoxy.In addition, carried out the combined amount of the metal hydroxides of fatty acid treatment for the surface, " 40phr～150phr " is meant more than the 40phr and below 150phr.Equally, total combined amount of metal hydroxides is meant more than the 175phr and below 300phr for " 175phr～300phr ".
The 3rd resin combination of the present invention, be characterised in that with the bisphenol A-type liquid epoxy resin, dimer acid modified Resins, epoxy, the metal hydroxides of fatty acid treatment has been carried out on the surface, untreated metal hydroxides in surface and the organic compound that contains the tetrazolium skeleton are neccessary composition, and the combined amount that the metal hydroxides of fatty acid treatment has been carried out on above-mentioned surface is 40phr～150phr, the organic compound that contains the tetrazolium skeleton is 20phr～100phr, and the metal hydroxides of fatty acid treatment has been carried out on above-mentioned surface, untreated metal hydroxides in above-mentioned surface and the total combined amount that contains the organic compound of tetrazolium skeleton are 195phr～300phr.
According to the 3rd resin combination of the present invention, can keep the good casting operation and the electrical insulating property of Resins, epoxy itself on the one hand, can also obtain high flame retardant resistance simultaneously.
In any resin combination in the of the present invention the 1st to the 3rd, above-mentioned metal hydroxides is preferably aluminium hydroxide.Also have, as metal hydroxides, the oxyhydroxide that also can form by metals such as magnesium in addition.
In any resin combination in the of the present invention the 1st to the 3rd, preferably the ratio of above-mentioned bisphenol A-type liquid epoxy resin is 50 weight %～70 weight % in the Resins, epoxy, and the ratio of above-mentioned dimer acid modified Resins, epoxy is 30 weight %～50 weight % in the Resins, epoxy.
In any resin combination in the of the present invention the 1st to the 3rd, preferably contain acid anhydrides as solidifying agent.In this case, compare with other solidifying agent and can reduce mixture viscosity, so the casting operation is good.In addition, compare reactive low with host with other solidifying agent, mixture is difficult for taking place gelation (curing reaction) at normal temperatures, therefore can carry out the casting operation for a long time.
Any resin combination in the of the present invention the 1st to the 3rd, preferably the heat-drawn wire of cured article is 35 ℃～55 ℃.
Variohm of the present invention is, comprise insulation case and be loaded into the circuit substrate that is formed with resistive element on the surface in this casing, and described surface rushes at the casing inner bottom part, and the rear side of the foregoing circuit substrate that is surrounded by the side of above-mentioned insulation case be filled with the present invention 1 to 3 in any resin combination.
According to variohm of the present invention,,,, have good characteristics such as electrical insulating property, resistance to sudden heating simultaneously therefore to pyritous weather resistance height owing to used the high resin combination of flame retardant resistance even in the variohm of state that might reach a high temperature.
As mentioned above, resin combination of the present invention can be provided under the condition of not using the halogen of being pointed out to produce unnecessary gas and red phosphorus based flame retardant, sealing material that electrical insulating property when having high flame retardant, resistance to sudden heating, casting operation, sedimentation stability are good etc.Thereby the electronic component, particularly high pressure that uses resin combination of the present invention has good characteristics such as high flame retardant and electrical insulating property, resistance to sudden heating with electronic component, variohm etc.
Description of drawings
Fig. 1 is that expression is as filling the sectional view of high pressure part casting of the present invention with the focus pack of high pressure part one example of resin.
Among the figure, the insulated enclosure portion that 6-is made of resin.
Embodiment
Resin combination of the present invention, contain with bisphenol A-type liquid epoxy resin, dimer acid modified Resins, epoxy, anhydride curing agent, as the surface carried out the aluminium hydroxide of metal hydroxides one example of fatty acid treatment, as the aluminium hydroxide of surperficial untreated metal hydroxides one example host as neccessary composition, can mix packing material, reaction diluent as required, give general additives such as soft agent, fire retardant, coupler, defoamer, pigment.In addition, in the resin combination of the present invention as neccessary composition contain bisphenol A-type liquid epoxy resin, dimer acid modified Resins, epoxy, carried out as the surface fatty acid treatment metal hydroxides one example aluminium hydroxide and as the aluminium hydroxide of surperficial untreated metal hydroxides one example, can mix packing material, reaction diluent as required, give general additives such as soft agent, fire retardant, coupler, defoamer, pigment.In addition, in the resin combination of the present invention as neccessary composition contain bisphenol A-type liquid epoxy resin, dimer acid modified Resins, epoxy, carried out as the surface fatty acid treatment metal hydroxides one example aluminium hydroxide and as the aluminium hydroxide of untreated metal hydroxides one example in surface and as the bistetrazole piperazine that contains organic compound one example of tetrazolium skeleton, can mix packing material, reaction diluent as required, give general additives such as soft agent, fire retardant, coupler, defoamer, pigment.
Resin combination of the present invention is the cast resin of insulated enclosure that can be used for focus pack etc., particularly needs the electronic components such as variohm of excellent thermal shocking in the high pressure part, can carry out casting, curing by existing known method.
Expression one example is used the focus pack as variohm of resin combination of the present invention as sealing agent among Fig. 1.This focus pack is provided with circuit substrate 3 in casing 2, be provided with simultaneously to adjust the operating stick 4,5 that output voltage is used.For potted circuit substrate 3, fill the present invention the 1st to the 3rd cast resin composition described in each from the peristome of the rear side of casing 2, and by this resin formation insulated enclosure portion 6.
Resin combination of the present invention is characterised in that, do not use halogen and red phosphorus based flame retardant and have high flame retardant, and the balance between the electrical insulating property, resistance to sudden heating, casting operation, sedimentation stability is also good.
The Resins, epoxy that uses among the present invention uses in order to have excellent electric insulation and resistance to sudden heating concurrently as bisphenol A-type liquid epoxy resin and dimer acid modified Resins, epoxy.Typical example as the bisphenol A-type liquid epoxy resin, can enumerate EP-828 (manufacturing of japan epoxy resin Co., Ltd.), AER260 (manufacturing of epoxy Co., Ltd. of Asahi Chemical Industry), EP-4100 (Asahi Denka Kogyo K. K's manufacturing) etc., as the typical example of dimer acid modified Resins, epoxy, can enumerate EP-871 (Japanese epoxy Co., Ltd. make), YD-171 (Toto Kasei KK's manufacturing) etc.
Solidifying agent as using among the present invention is preferably anhydride curing agent.Specifiable is for example methyl tetrahydrochysene anhydride phthalic acid, methyl six hydrogen anhydride phthalic acids, anhydride phthalic acid, six hydrogen anhydride phthalic acids, end methylene radical tetrahydrochysene anhydride phthalic acid, dodecenyl succinic anhydride, octenyl succinic acid anhydride etc.These can be separately or in conjunction with using more than 2 kinds.
The aluminium hydroxide that uses among the present invention for having carried out the aluminium hydroxide and the surperficial untreated aluminium hydroxide of fatty acid treatment in the surface,, is not particularly limited so long as general commercially available pulverous aluminium hydroxide just can use as aluminium hydroxide.
Carried out the lipid acid of the aluminium hydroxide of fatty acid treatment as being used for the surface, can use stearic acid for example, Palmiticacid, tetradecanoic acid, month silicic acid, capric acid, sad, linolic acid, oleic acid, lipid acid that the coconut wet goods is general, can handle by existing known method.
This surface treatment is meant that becoming these lipid acid is adsorbed on the lip-deep state of aluminum hydroxide particles.
Owing to be adsorbed on this lip-deep lipid acid and improved the affinity of aluminum hydroxide particles for aqueous resin, so each particle of aluminium hydroxide uprising as the dispersiveness in the liquid of dispersion medium, each powder not free settling that becomes.
The combined amount that the aluminium hydroxide of fatty acid treatment has been carried out on the surface of using among the present invention is 40phr～300phr.Phr is with respect to the addition of 100 weight part Resins, epoxy (weight part).
In addition, be used for during with regard to the aluminium hydroxide that carried out fatty acid treatment at blending surface and surperficial untreated aluminium hydroxide with regard to the present invention's the combined amount of aluminium hydroxide, the combined amount that the aluminium hydroxide of fatty acid treatment has been carried out on the surface is 40phr～150phr, and the aluminium hydroxide of fatty acid treatment has been carried out on the surface and total combined amount of surperficial untreated aluminium hydroxide is 175phr～300phr.Phr is with respect to the addition of 100 weight part Resins, epoxy (weight part).
The aluminium hydroxide that has carried out fatty acid treatment on the surface is less than under the situation of 40phr, and the easy sedimentation (sedimentation stability reduction) that becomes of powder composition can form hard settled layer.
In addition, carried out the aluminium hydroxide of fatty acid treatment and total combined amount of surperficial untreated aluminium hydroxide on the surface and be less than under the situation of 175phr, flame retardant resistance can descend, and under the situation more than 300phr, because viscosity rises, the casting operation can descend.Total combined amount of aluminium hydroxide is in the scope of 200phr～290phr the time, and the balance of flame retardant resistance and casting operation is good especially, therefore more preferably.In addition, total combined amount of aluminium hydroxide is in the scope of 220phr～270phr the time, and the balance of flame retardant resistance and casting operation is good especially, and is therefore more preferred.
In addition, the present invention 3 in contain bisphenol A-type liquid epoxy resin, dimer acid modified Resins, epoxy as neccessary composition, carried out the aluminium hydroxide of metal hydroxides one example of fatty acid treatment as the surface, as the surface untreated metal hydroxides one example aluminium hydroxide and have in the resin combination of organic compound of tetrazolium skeleton, the organic compound with tetrazolium skeleton can use for example bistetrazole piperazine, bistetrazole two ammoniums, bistetrazole two guanidines, 5-phenyltetrazole, azo bistetrazole guanidine, azo bistetrazole Imidocarbonic acid dihydrazide etc.
The present invention 3 in the surface combined amount of having carried out the metal hydroxides of fatty acid treatment be 40phr～150phr, the organic compound that contains the tetrazolium skeleton is 20phr～100phr, and total combined amount that above-mentioned surface has been carried out the metal hydroxides of fatty acid treatment, the untreated metal hydroxides in above-mentioned surface and contained the organic compound of tetrazolium skeleton is 195phr～300phr.
Product of the present invention has high flame retardant, and the balance between the electrical insulating property, resistance to sudden heating, casting operation, sedimentation stability is also good, as preferred embodiments of the present invention, the heat-drawn wire of the cured article when the resin cured matter among the present invention take place is solidified is made as 35 ℃～55 ℃, promptly be made as belong to more than 35 ℃ and the scope below 55 ℃ in temperature, can obtain the special good quality production of balance between electrical insulating property and the shock-resistance.
Resin combination among the present invention does not limit to variohms such as being used for focus pack, so long as the parts of applying high voltage promptly can be used as its sealing material or insulating material and use.Resin combination described in the present invention can be used for for example high potential assembly, high-tension transformer etc.
In the present invention, as metal hydroxides, also can use magnesium hydroxide.
[embodiment 1]
Below, according to table 1 and table 2 illustrate the present invention 1 and 2 described in embodiment and comparative example, but the present invention is not limited to these.Represented in the table 1 the present invention 1 and the composition of a plurality of embodiment (embodiment 1～13) of 2 and the test-results of characteristic measurement, the composition of comparative example shown in the table 2 (comparative example 1～8) and the test-results of characteristic measurement.Also have, the numerical value unit of each composition of host and solidifying agent is phr (addition (weight part) when all Resins, epoxy is 100 weight parts) in table 1 and the table 2.
[table 1]
| Embodiment | ||||||||||||||
| ???1 | ???2 | ????3 | ????4 | ????5 | ????6 | ????7 | ????8 | ????9 | ????10 | ????11 | ????12 | ????13 | ||
| Host | Bisphenol A-type liquid epoxy resin (EP-828) | ???70 | ???60 | ????53 | ????40 | ????30 | ????53 | ????53 | ????53 | ????53 | ????53 | ????53 | ????53 | ????53 |
| Dimer acid modified Resins, epoxy (YD-171) | ???30 | ???40 | ????47 | ????60 | ????70 | ????47 | ????47 | ????47 | ????47 | ????47 | ????47 | ????47 | ????47 | |
| Aluminium hydroxide (H-34HL) (the Oleum Cocois item for disposal of H-34) | ???100 | ???100 | ????100 | ????100 | ????100 | ????75 | ????88 | ????113 | ????125 | ????40 | ????300 | ????150 | ||
| The stearic acid item for disposal of H-34 | ????100 | |||||||||||||
| The epoxy silane item for disposal of H-34 | ||||||||||||||
| The propenyl silane treatment product of H-34 | ||||||||||||||
| Aluminium hydroxide (H-31) | ???132 | ???132 | ????132 | ????132 | ????132 | ????132 | ????100 | ????115 | ????148 | ????165 | ????192 | ????150 | ||
| The total of coupler/defoamer/pigment | ???2.51 | ???2.51 | ????2.51 | ????2.51 | ????2.51 | ????2.51 | ????2.51 | ????2.51 | ????2.51 | ????2.51 | ????2.51 | ????2.51 | ????2.51 | |
| Solidifying agent | Acid anhydrides (MT-500) | ???35 | ???33 | ????31 | ????28 | ????24 | ????31 | ????31 | ????31 | ????31 | ????31 | ????31 | ????31 | ????31 |
| Acid anhydrides (DSA) | ???35 | ???33 | ????31 | ????28 | ????24 | ????31 | ????31 | ????31 | ????31 | ????31 | ????31 | ????31 | ????31 | |
| Curing catalyst (HD-ACC-43) | ???1.0 | ???1.0 | ????0.9 | ????0.8 | ????0.7 | ????0.9 | ????0.9 | ????0.9 | ????0.9 | ????0.9 | ????0.9 | ????0.9 | ????0.9 | |
| The total of surface treated aluminium hydroxide and undressed aluminium hydroxide [phr] | ???232 | ???232 | ????232 | ????232 | ????232 | ????232 | ????175 | ????203 | ????261 | ????290 | ????232 | ????300 | ????300 | |
| Flame retardant resistance | ???V-0 | ???V-0 | ????V-0 | ????V-0 | ????V-0 | ????V-0 | ????V-0 | ????V-0 | ????V-0 | ????V-0 | ????V-0 | ????V-0 | ????V-0 | |
| Electrical insulating property | ???◎ | ???◎ | ????◎ | ????◎ | ????○ | ????◎ | ????◎ | ????◎ | ????◎ | ????◎ | ????◎ | ????◎ | ????◎ | |
| Resistance to sudden heating | ???○ | ???◎ | ????◎ | ????◎ | ????◎ | ????◎ | ????◎ | ????◎ | ????◎ | ????◎ | ????◎ | ????◎ | ????◎ | |
| It in the casting operability () mixture viscosity [Pas] | ???◎ ?????(9) | ???◎ ?????(10) | ????◎ ???????(10) | ????◎ ???????(11) | ????◎ ???????(11) | ????◎ ???????(10) | ????◎ ???????(5) | ????◎ ???????(6) | ????◎ ???????(12) | ????○ ???????(16) | ????○ ???????(16) | ????○ ???????(18) | ????○ ???????(16) | |
| Sedimentation stability | ???◎ | ???◎ | ????◎ | ????◎ | ????◎ | ????◎ | ????◎ | ????◎ | ????◎ | ????◎ | ????◎ | ????◎ | ????◎ | |
| Heat-drawn wire [℃] | ???59 | ????55 | ????46 | ????35 | ????＜30 | ????47 | ????46 | ????45 | ????46 | ????47 | ????46 | ????47 | ????47 | |
[table 2]
| Comparative example | |||||||||
| ????1 | ????2 | ????3 | ????4 | ????5 | ????6 | ????7 | ????8 | ||
| Host | Bisphenol A-type liquid epoxy resin (EP-828) | ????100 | ????53 | ????53 | ????53 | ???53 | ????53 | ????53 | |
| Dimer acid modified Resins, epoxy (YD-171) | ???100 | ????47 | ????47 | ????47 | ???47 | ????47 | ????47 | ||
| Aluminium hydroxide (H-34HL) (the Oleum Cocois item for disposal of H-34) | ????100 | ???100 | ???50 | ????150 | ????30 | ||||
| The stearic acid item for disposal of H-34 | |||||||||
| The epoxy silane item for disposal of H-34 | ????100 | ||||||||
| The propenyl silane treatment product of H-34 | ????100 | ||||||||
| Aluminium hydroxide (H-31) | ????132 | ???132 | ????232 | ????132 | ????132 | ???66 | ????180 | ????202 | |
| The total of coupler/defoamer/face material | ????2.51 | ???2.51 | ????2.51 | ????2.51 | ????2.51 | ???2.51 | ????2.51 | ????2.51 | |
| Solidifying agent | Acid anhydrides (MT-500) | ????42 | ???17 | ????31 | ????31 | ????31 | ???31 | ????31 | ????31 |
| Acid anhydrides (DSA) | ????42 | ???17 | ????31 | ????31 | ????31 | ???31 | ????31 | ????31 | |
| Curing catalyst (HD-ACC-43) | ????1.2 | ???0.5 | ????0.9 | ????0.9 | ????0.9 | ???0.9 | ????0.9 | ????0.9 | |
| The total of surface treated aluminium hydroxide and undressed aluminium hydroxide [phr] | ????232 | ???232 | ????232 | ????232 | ????232 | ???116 | ????330 | ????232 | |
| Flame retardant resistance | ????- | ???- | ????V-0 | ????V-0 | ????V-0 | Can not classify | ????V-0 | ????V-0 | |
| Electrical insulating property | ????◎ | ??× | ????◎ | ????◎ | ????- | ???◎ | ????- | ????◎ | |
| Resistance to sudden heating | ????× | ??◎ | ????◎ | ????◎ | ????◎ | ???◎ | ????◎ | ????◎ | |
| It in the casting operability () mixture viscosity [Pas] | ????- | ??- | ????× ???????(＞20) | ????- | ????- | ???◎ ?????(3) | ????× ???????(＞20) | ????○ ???????(17) | |
| Sedimentation stability | ????◎ | ??◎ | ????× | ????× | ????× | ???◎ | ????◎ | ????× | |
| Heat-drawn wire [℃] | ????＞80 | ??＜30 | ????45 | ????46 | ????46 | ???45 | ????47 | ????46 | |
Also have,, 100 ℃ of following thermofixations 3 hours, can obtain cured article then by mixing host and solidifying agent.
In addition, each characteristic can be measured by measuring method shown below.
(1) flame retardant resistance: with cured article be processed into 127mm * 12.7mm, thickness is the rectangular plate shape of 3.2mm, measure according to the test method of UL94V.According to the judgment standard of UL94V, judge with V-0, V-1, V-2,4 grades such as can not classify.The flame retardant resistance of V-0 is the highest, and descends gradually according to V-1, V-2, the order that can not classify.
(2) electrical insulating property: with cured article be processed into 100mm * 100mm, thickness is the rectangular plate shape of 2mm, according to the test method of JIS specification K6911, the volume specific resistance under measuring 100 ℃.Judge according to following benchmark.
◎: 1 * 10
12More than the Ω cm
Zero: 1 * 10
11Above and the less than 1 * 10 of Ω cm
12Ω cm
*: less than 1 * 10
11Ω cm
(3) resistance to sudden heating: mix host and solidifying agent, in the uncovered resin casing of casting 35g to 60mm * 70mm, high 5mm, make sample then by thermofixation.This sample is placed in the cold cycling of-40 ℃/2 hours and 110 ℃/2 hours, fissured cycle number takes place in range estimation in cast resin cured article or resin casing.Judgement is carried out according to following benchmark.
◎: circulate and the crack does not take place after 100 times yet
The crack takes place in the time of zero: 51～100 times
*: circulate the crack takes place 0～50 time the time
(4) casting operation: mix host and solidifying agent, the viscometer RVDV-2+ (using small amount of sample adapter (adapter) SSA14/6R) that adopts Brookfield company to make, the viscosity (mixture viscosity) under measuring 25 ℃.Judge according to following benchmark.
◎: not enough 15Pas
Zero: the above and not enough 20Pas of 15Pas
*: more than the 20Pas
(5) sedimentation stability: 100g host is put into the Glass Containers that capacity is 100ml, clog, after placing 7 under 60 ℃, return to room temperature, confirm to have or not hard settled layer by glass stick with stopper.Judge according to following benchmark.
◎: do not have hard settled layer
*: hard settled layer is arranged
(6) heat-drawn wire: cured article is processed into the shape of 13mm * 13mm * 127mm,, under load 66psi, measures according to the test method of ASTMD648.
Embodiment 1～12: use EP-828 (Japanese epoxy Co., Ltd. make) as the bisphenol A-type liquid epoxy resin, use YD-171 (Toto Kasei KK's manufacturing) as dimer acid modified Resins, epoxy, use to mix the material of MT-500 (New Japan Chem Co., Ltd's manufacturing) and DSA (Sanyo Chemical Industries, Ltd.'s manufacturing) at 1: 1 as anhydride curing agent.The aluminium hydroxide that has carried out fatty acid treatment as the surface uses H-34HL (Showa Denko K. K's manufacturing, handle the material that obtains behind the H-34 of same company manufacturing with Oleum Cocois, median size is 4 μ m), use H-31 (Showa Denko K. K makes, and median size is 20 μ m not) as the untreated aluminium hydroxide in surface.In embodiment 6, carried out other examples of the aluminium hydroxide of fatty acid treatment as the surface, used the aluminium hydroxide of handling H-34 (Showa Denko K. K's manufacturing) with stearic acid.
By under reduced pressure stir above-mentioned bisphenol A-type liquid epoxy resin, dimer acid modified Resins, epoxy, the surface has been carried out the aluminium hydroxide of fatty acid treatment, surperficial untreated aluminium hydroxide and silane coupling agent SH6040 (eastern beautiful ダ ウ コ-ニ Application グ silicon Co., Ltd. makes) 1.5phr, defoamer SH5500 (eastern beautiful ダ ウ コ-ニ Application グ silicon Co., Ltd. makes) 0.01phr, pigment 1.0phr and has been made host, and by stirring and dissolving curing catalyst HD-ACC-43 in above-mentioned anhydride curing agent (mostly Industry Co., Ltd makes) making solidifying agent.
By embodiment 1～13 as can be seen, with the bisphenol A-type liquid epoxy resin, dimer acid modified Resins, epoxy, anhydride curing agent, the aluminium hydroxide of fatty acid treatment has been carried out on the surface, the untreated aluminium hydroxide in surface is as neccessary composition, and the combined amount that the aluminium hydroxide of fatty acid treatment has been carried out on the surface is 40phr～150phr, the aluminium hydroxide of fatty acid treatment has been carried out on the surface and total combined amount of surperficial untreated aluminium hydroxide is in the resin combination of 175phr～300phr, flame retardant resistance, electrical insulating property, resistance to sudden heating, the casting operation, balance between the sedimentation stability is good.
In addition, as can be seen because have electrical insulating property decline when heat-drawn wire descends, when heat-drawn wire rises the resistance to sudden heating downward trend, so heat-drawn wire is preferably 35 ℃～55 ℃ scope especially.
Comparative example 1 and 2: only using the bisphenol A-type liquid epoxy resin as Resins, epoxy or only using under the situation of dimer acid modified Resins, epoxy, the balance between electrical insulating property and the resistance to sudden heating can be destroyed.Promptly under the situation of only using the bisphenol A-type liquid epoxy resin, resistance to sudden heating reduces, and under the situation of only using dimer acid modified Resins, epoxy, electrical insulating property reduces.
Comparative example 3: do not having blending surface to carry out under the situation of aluminium hydroxide of fatty acid treatment, sedimentation stability significantly reduces.
Comparative example 4 and 5: the surface treatment of aluminium hydroxide is changed to epoxy silane processing, propenyl silane treatment with under the surface-treated situation that replaces employing lipid acid, and sedimentation stability significantly reduces.
Comparative example 6 and 7: carried out on the surface under the situation of the not enough 175phr of total combined amount of the aluminium hydroxide of fatty acid treatment and surperficial untreated aluminium hydroxide, flame retardant resistance reduces, and can not get UL94V-0.In addition, if surpass 300phr, then mixture viscosity rises, casting operation decline.
Comparative example 8: the aluminium hydroxide that has carried out fatty acid treatment on the surface is that the total amount of 30phr and aluminium hydroxide is all under the situation of 232phr mutually with embodiment 11, and sedimentation stability significantly reduces.
Embodiment 2]
Following according to table 3 and table 4 explanation the present invention 3 described in embodiment and comparative example, but the present invention is not limited to these.The composition of a plurality of embodiment (embodiment 21～29) of expression the present invention's 3 and the test-results of characteristic measurement are represented the composition of comparative example (comparative example 21～25) and the test-results of characteristic measurement in the table 3 in the table 4.Also have, the numerical value unit of each composition of host and solidifying agent is phr (addition (weight part) when all Resins, epoxy is 100 weight parts) in table 3 and the table 4.
[table 3]
| Embodiment | ||||||||||
| ????21 | ????22 | ????23 | ????24 | ????25 | ????26 | ????27 | ????28 | ????29 | ||
| Host | Bisphenol A-type liquid epoxy resin (EP-828) | ????53 | ????53 | ????53 | ????53 | ????60 | ????53 | ????53 | ????60 | ????60 |
| Dimer acid modified Resins, epoxy (YD-171) | ????47 | ????47 | ????47 | ????47 | ????40 | ????47 | ????47 | ????40 | ????40 | |
| Aluminium hydroxide (H-34HL) (the Oleum Cocois item for disposal of H-34) | ????40 | ????150 | ????75 | ????100 | ????70 | ????100 | ????100 | ????70 | ????70 | |
| Aluminium hydroxide (H-31) | ????172 | ????130 | ????100 | ????100 | ????130 | ????100 | ????100 | ????210 | ????130 | |
| The organic compound (BHTPIPE) that contains the tetrazolium skeleton | ????20 | ????20 | ????20 | ????20 | ????20 | ????50 | ????100 | ????20 | ????100 | |
| The total of coupler/defoamer/pigment | ????2.51 | ????2.51 | ????2.51 | ????2.51 | ????2.5 | ????2.51 | ????2.51 | ????2.5 | ????2.5 | |
| Solidifying agent | Acid anhydrides (MT-500) | ????31 | ????31 | ????31 | ????31 | ????61 | ????31 | ????31 | ????40 | ????40 |
| Acid anhydrides (DSA) | ????31 | ????31 | ????31 | ????31 | ????0 | ????31 | ????31 | ????40 | ????40 | |
| Curing catalyst (HD-ACC-43) | ????0.9 | ????0.9 | ????0.9 | ????0.9 | ????0.9 | ????0.9 | ????0.9 | ????1.2 | ????1.2 | |
| Surface treated aluminium hydroxide and undressed aluminium hydroxide and the total [phr] that contains the organic compound of tetrazolium skeleton | ????232 | ????300 | ????195 | ????220 | ????220 | ????250 | ????300 | ????300 | ????300 | |
| Flame retardant resistance (classification) | ????V-0 | ????V-0 | ????V-0 | ????V-0 | ????V-0 | ????V-0 | ????V-0 | ????V-0 | ????V-0 | |
| (combustion time) | ????◎ | ????◎ | ????◎ | ????◎ | ????◎ | ????◎ | ????◎ | ????◎ | ????◎ | |
| Electrical insulating property | ????◎ | ????◎ | ????◎ | ????◎ | ????◎ | ????◎ | ????◎ | ????◎ | ????◎ | |
| Resistance to sudden heating | ????◎ | ????◎ | ????◎ | ????◎ | ????○ | ????◎ | ????◎ | ????○ | ????○ | |
| It in the casting operability () mixture viscosity [Pas] | ????○ ???????(15) | ????○ ???????(17) | ????◎ ???????(7) | ????◎ ???????(11) | ????◎ ???????(11) | ????○ ???????(15) | ????○ ???????(19) | ????○ ???????(16) | ????○ ???????(17) | |
| Sedimentation stability | ????◎ | ????◎ | ????◎ | ????◎ | ????◎ | ????◎ | ????◎ | ????◎ | ????◎ | |
| Heat-drawn wire [℃] | ????46 | ????47 | ????46 | ????46 | ????63 | ????47 | ????47 | ????62 | ????62 | |
[table 4]
| Comparative example | |||||||
| ????21 | ????22 | ????23 | ????24 | ????25 | ????26 | ||
| Host | Bisphenol A-type liquid epoxy resin (EP-828) | ????53 | ????53 | ????53 | ????53 | ????53 | ????53 |
| Dimer acid modified Resins, epoxy (YD-171) | ????47 | ????47 | ????47 | ????47 | ????47 | ????47 | |
| Aluminium hydroxide (H-34HL) (the Oleum Cocois item for disposal of H-34) | ????30 | ????100 | ????100 | ????75 | ????75 | ????100 | |
| Aluminium hydroxide (H-31) | ????182 | ????100 | ????100 | ????100 | ????75 | ????132 | |
| The organic compound (BHTPIPE) that contains the tetrazolium skeleton | ????20 | ????0 | ????10 | ????120 | ????20 | ????100 | |
| The total of coupler/defoamer/pigment | ????2.51 | ????2.51 | ????2.51 | ????2.51 | ????2.51 | ????2.51 | |
| Solidifying agent | Acid anhydrides (MT-500) | ????31 | ????31 | ????31 | ????31 | ????31 | ????31 |
| Acid anhydrides (DSA) | ????31 | ????31 | ????31 | ????31 | ????31 | ????31 | |
| Curing catalyst (HD-ACC-43) | ????0.9 | ????0.9 | ????0.9 | ????0.9 | ????0.9 | ????0.9 | |
| Surface treated aluminium hydroxide and undressed aluminium hydroxide and the total [phr] that contains the organic compound of tetrazolium skeleton | ????232 | ????200 | ????210 | ????295 | ????170 | ????332 | |
| Flame retardant resistance (classification) | ????V-0 | ????V-0 | ????V-0 | ????V-0 | ????V-1 | ????V-0 | |
| (combustion time) | ????◎ | ????× | ????× | ????◎ | ????× | ????◎ | |
| Electrical insulating property | ????◎ | ????◎ | ????◎ | ????◎ | ????◎ | ????◎ | |
| Resistance to sudden heating | ????◎ | ????◎ | ????◎ | ????◎ | ????◎ | ????◎ | |
| It in the casting operability () mixture viscosity [Pas] | ????○ ???????(16) | ????◎ ????????(8) | ????◎ ???????(10) | ????× ???????(＞20) | ????◎ ???????(6) | ????× ???????(＞20) | |
| Sedimentation stability | ????× | ????◎ | ????◎ | ????◎ | ????◎ | ????◎ | |
| Heat-drawn wire [℃] | ????46 | ????46 | ????46 | ????47 | ????45 | ????47 | |
The cured article of the resin shown in these embodiment 2 row is by mixing host and solidifying agent, obtaining in 3 hours 100 ℃ of curing through vacuum defoamation then.In addition, each characteristic can be measured by measuring method shown below.
(1) flame retardant resistance (classification): with cured article be processed into 127mm * 12.7mm, thickness is the rectangular plate shape of 3.2mm, according to the determination of test method of UL94V.According to the judgment standard of UL94V, judge with V-0, V-1, V-2,4 grades such as can not classify.The flame retardant resistance of V-0 is the highest, and reduces gradually according to V-1, V-2, the order that can not classify.
Flame retardant resistance (combustion time): with cured article be processed into 127mm * 12.7mm, thickness is the rectangular plate shape of 1.6mm, being determined at has the flame time (sample has the time of flame) when carrying out the contact of 20 seconds flame under the flame contact conditions identical with the combustion test method of UL94V.Judge according to following benchmark.
◎: less than 5 seconds
*: more than 5 seconds
(2) electrical insulating property: with cured article be processed into 100mm * 100mm, thickness is the plate shape of 2mm, according to the test method of JIS specification K6911, the volume specific resistance under measuring 100 ℃.Judge according to following benchmark.
◎: 1 * 10
12More than the Ω cm
Zero: 1 * 10
11Above and the less than 1 * 10 of Ω cm
12Ω cm
*: less than 1 * 10
11Ω cm
(3) resistance to sudden heating: mix host and solidifying agent, in the uncovered resin casing of casting 35g to 60mm * 70mm, high 5mm, make sample then by thermofixation.This sample is placed in the cold cycling of-40 ℃/2 hours and 110 ℃/2 hours, fissured cycle number takes place in range estimation cast resin cured article or the resin casing.Judge according to following benchmark.
◎: circulate and the crack does not take place after 100 times yet
The crack takes place in the time of zero: 51～100 times
*: circulate the crack takes place 0～50 time the time
(4) casting operation: mix host and solidifying agent, the viscometer RVDV-2+ (using small amount of sample adapter SSA14/6R) that adopts Brooker Er De company to make, the viscosity (mixture viscosity) under measuring 25 ℃.Judge according to following benchmark.
◎: not enough 15Pas
Zero: the above and not enough 20Pas of 15Pas
*: more than the 20Pas
(5) sedimentation stability: 100g host is put into the Glass Containers that capacity is 100ml, clog, after placing 7 under 60 ℃, return to room temperature, confirm to have or not hard settled layer with glass stick with stopper.Judge according to following benchmark.
◎: do not have hard settled layer
*: hard settled layer is arranged
(6) heat-drawn wire: cured article is processed into the shape of 13mm * 13mm * 127mm,, under load 66psi, measures according to the test method of ASTMD648.
Embodiment 21～29: use bisphenol A-type liquid epoxy resin EP-828 (japan epoxy resin manufacturing) and dimer acid modified Resins, epoxy YD-171 (Dongdu changes into manufacturing) as Resins, epoxy (A), use H-34HL (clear and electrician makes) and H-31 (clear and electrician makes) as aluminium hydroxide (B), use bistetrazole piperazine (セ Le テ ト ラ BHT-PIPE as the organic compound that contains the tetrazolium skeleton (C), Yonghe County changes into industry manufacturing), use MT-500 (new Japanese physics and chemistry manufacturing) and DSA (Sanyo Chemical Industries, Ltd.'s manufacturing) as acid anhydrides (D), use HD-ACC-43 (mostly industry manufacturing) as curing catalyst (E).
By under reduced pressure stirring above-mentioned (A), (B), (C) and silane coupling agent SH6040 (eastern beautiful ダ ウ コ-ニ Application グ make), defoamer SH5500 (eastern beautiful ダ ウ コ-ニ Application グ makes), pigment prepared host, and prepare solidifying agent by stirring and dissolving above-mentioned (D), (E).
By embodiment 21～27 as can be seen, with the bisphenol A-type liquid epoxy resin, dimer acid modified Resins, epoxy, the metal hydroxides of fatty acid treatment has been carried out on the surface, untreated metal hydroxides in surface and the organic compound that contains the tetrazolium skeleton are neccessary composition, and the combined amount that the metal hydroxides of fatty acid treatment has been carried out on the surface is 40phr～150phr, the organic compound that contains the tetrazolium skeleton is 20phr～100phr, the metal hydroxides of fatty acid treatment has been carried out on above-mentioned surface, untreated metal hydroxides in above-mentioned surface and the total combined amount that contains the organic compound of tetrazolium skeleton are the resin combination of 195phr～300phr, combustion time, less than was 5 seconds, and flame retardant resistance is good.
Comparative example 21: because the not enough 40phr of the metal hydroxides of fatty acid treatment has been carried out on the surface, so sedimentation stability descends.
Comparative example 22: owing to do not contain the organic compound with tetrazolium skeleton, reach combustion time more than 5 seconds, flame retardant resistance descends.
Comparative example 23: owing to contain the not enough 20phr of the organic compound of tetrazolium skeleton, reach combustion time more than 5 seconds, flame retardant resistance descends.
Comparative example 24: surpass 100phr owing to contain the organic compound of tetrazolium skeleton, mixture viscosity rises, casting operation decline.
Comparative example 25: because the not enough 195phr of total combined amount that the surface has been carried out metal hydroxides, the surperficial untreated metal hydroxides of fatty acid treatment and contained the organic compound of tetrazolium skeleton, so the classification of flame retardant resistance becomes V-1.
Comparative example 26: because total combined amount that the surface has been carried out metal hydroxides, the surperficial untreated metal hydroxides of fatty acid treatment and contained the organic compound of tetrazolium skeleton surpasses 300phr, mixture viscosity rises, casting operation reduction.
[embodiment 3]
Below, the focus pack at as variohm one example describes according to Fig. 1.
Focus pack 1 shown in Fig. 1 has the insulation case 2 of an opening.Be formed in the section portion 7 on insulation case 2 inner peripheral surfaces to engage and be fixed with the insulativity substrate 3 that is made of aluminum oxide etc., its surface rushes at the inner bottom part of casing.The rear side molding of substrate 3 by by the present invention 1 to 3 in the redix 6 formed of any resin combination, substrate 3 is insulated really in the outside thus.Front face at casing is provided with a plurality of dead eyes 8,9, and turning axle 4,5 can rotate in these dead eyes 8,9 respectively.
On the surface of substrate 3, dispose output terminal electrode, the screen voltage of not shown focus pack voltage the output terminal electrode, comprise the resistive element adjusting the variable resistor part that focus voltage uses and adjust the variable resistor part that screen voltage uses, connect in the input terminal electrode of this resistive element and ground terminal electrode etc.Each slide block 10,11 that has 2 terminals in the time of with each turning axle 4,5 one rotation is configured to square end and contacts with the central electrode (not shown) of connecting the output terminal electrode, and the opposing party's terminal slides on circular-arc variable resistance part.Above-mentioned input terminal electrode and ground terminal electrode are connected with high voltage input terminal and ground terminal (all not shown) respectively.
Turning axle 4,5 is integrally formed by insulative resin, has the axle 12,13 that can be inserted on the dead eye 8,9 respectively with rotating freely.On the front end face of axle 12,13, be formed with the combinable crosswise combined holes 14,15 of instrument such as screwdriver.
Claims (8)
1. resin combination, the metal hydroxides that it is characterized in that having carried out with bisphenol A-type liquid epoxy resin, dimer acid modified Resins, epoxy, surface fatty acid treatment is a neccessary composition, and the combined amount that the metal hydroxides of fatty acid treatment has been carried out on described surface is 40phr～300phr.
2. resin combination, it is characterized in that with bisphenol A-type liquid epoxy resin, dimer acid modified Resins, epoxy, surperficial metal hydroxides and the surperficial untreated metal hydroxides that has carried out fatty acid treatment be neccessary composition, and the combined amount that the metal hydroxides of fatty acid treatment has been carried out on described surface is 40phr～150phr, and total combined amount that the untreated metal hydroxides of metal hydroxides and described surface of fatty acid treatment has been carried out on described surface is 175phr～300phr.
3. resin combination, it is characterized in that with the bisphenol A-type liquid epoxy resin, dimer acid modified Resins, epoxy, the metal hydroxides of fatty acid treatment has been carried out on the surface, untreated metal hydroxides in surface and the organic compound that contains the tetrazolium skeleton are neccessary composition, and the combined amount that the metal hydroxides of fatty acid treatment has been carried out on described surface is 40phr～150phr, the organic compound that contains the tetrazolium skeleton is 20phr～100phr, and the metal hydroxides of fatty acid treatment has been carried out on described surface, untreated metal hydroxides in described surface and the total combined amount that contains the organic compound of tetrazolium skeleton are 195phr～300phr.
4. according to each described resin combination among the claim 1-3, it is characterized in that described metal hydroxides is an aluminium hydroxide.
5. according to each described resin combination among the claim 1-4, the ratio that it is characterized in that the liquid epoxy resin of bisphenol A-type described in the Resins, epoxy is 50 weight %～70 weight %, and the ratio of dimer acid modified Resins, epoxy described in the Resins, epoxy is 30 weight %～50 weight %.
6. according to each described resin combination among the claim 1-5, it is characterized in that containing acid anhydrides as solidifying agent.
7. according to each described resin combination among the claim 1-6, the heat-drawn wire that it is characterized in that cured article is 35 ℃～55 ℃.
8. variohm, comprise insulation case and be loaded into the circuit substrate that is formed with resistive element on the surface in this casing, and described surface rushes at the casing inner bottom part, the rear side of the described circuit substrate that is surrounded by the side of described insulation case be filled with in the claim 1 to 7 each resin combination.
Applications Claiming Priority (4)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP2003038035 | 2003-02-17 | ||
| JP2003038035 | 2003-02-17 | ||
| JP2003408835A JP4013894B2 (en) | 2003-02-17 | 2003-12-08 | Resin composition and variable resistor |
| JP2003408835 | 2003-12-08 |
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| CN1523057A true CN1523057A (en) | 2004-08-25 |
| CN1309784C CN1309784C (en) | 2007-04-11 |
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| GB9227155D0 (en) * | 1992-12-31 | 1993-02-24 | Rhone Poulenc Chemicals | Inhibiting calcium carbonate crystal growth |
| CN1121942C (en) * | 1999-04-29 | 2003-09-24 | 北京化工大学 | Composite base laminated board covered with copper foil and its production method |
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