CN102839566B - Low-dielectric loss phenolic aldehyde laminating paper board and manufacturing method thereof - Google Patents
Low-dielectric loss phenolic aldehyde laminating paper board and manufacturing method thereof Download PDFInfo
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Abstract
The invention relates to a low-dielectric loss phenolic aldehyde laminating paper board and a manufacturing method thereof. The method is simple and rapid in step, and due to the use of the phenolic aldehyde laminating paper board obtained by using the method, the dielectric loss factor is small, the electric strength is large and the breakdown voltage is high. The manufacturing method of the low-dielectric loss phenolic aldehyde laminating paper board comprises the following steps: directly dipping paper by using matrix resin dissolving liquid or mixed resin dissolving liquid, then baking the paper to obtain a prepreg, and conducting lamination and hot pressing molding on the preprg, wherein a preparation method of the matrix resin dissolving liquid comprises the steps of a. uniformly mixing phenol, dimethylbenzene formaldehyde and p-toluenesulfonic acid, and reacting to obtain a mixture 1; and b. adding triethanolamine in the mixture 1, then adding formaldehyde, triethylamine and ammonia water for reaction, then dewatering to obtain matrix resin, and adding a solvent to dissolve the matrix resin; and a preparation method of the mixed resin dissolving liquid comprises the steps of dissolving phenolic aldehyde epoxy resin by a solvent, and uniformly mixing phenolic aldehyde epoxy resin dissolving liquid and the matrix resin dissolving liquid to obtain the mixed resin dissolving liquid.
Description
Technical field
The present invention relates to a kind of laminated board and preparation method thereof, particularly relate to low dielectric loss laminated phenolic paper plate that a kind of dielectric dissipation factor is little, electrical strength is large and breakdown voltage is high and preparation method thereof.
Background technology
On high-voltage mutual inductor, high, that dielectric properties the are good insulating laminated sheet of mechanical strength is usually adopted to come supporting iron core and the packing ring as coil both sides.The insulating laminated sheet of high dielectric loss is used on high-voltage mutual inductor easily breakdown, thus causes the damage of equipment, and therefore for high-voltage mutual inductor insulating laminated sheet used, its dielectric dissipation factor is lower.The dielectric dissipation factor resin used with it of insulating laminated sheet is in close relations, and when base material is certain, resin medium loss is lower, and the dielectric loss of insulating laminated sheet is also lower.
Chinese patent (CN1511857A) discloses a kind of synthetic method of m-dimethyl benzene phenolic resin: first synthesize meta-xylene formaldehyde, between using, two benzaldehydes and phenol, formaldehyde react obtained m-dimethyl benzene phenolic resin under barium hydroxide catalysis again, then be prepared into epoxy xylenols urea formaldehyde with epoxy E-42, be used in conducting static anticorrosion paint.Chinese patent (CN1537913A) discloses a kind of for adhesive that is high temperature resistant, high-strength wearable brake material, with dimethylbenzene formaldehyde, phenol, catalyst and oxalic acid for raw material, first dimethylbenzene formaldehyde, phenol, catalyst are reacted 30min at 128 ~ 135 DEG C, then add formaldehyde, oxalic acid back flow reaction 90min, then obtain dimethylbenzene phenol-formaldehyde resin modified through normal pressure and decompression dehydration successively.
Japan Patent (JP5116067) is first reacted under Catalyzed by p-Toluenesulfonic Acid by xylene resin, metacresol, and reactant reacts obtained oily modification xylenols urea formaldehyde again under methenamine catalysis with tung oil, paraformaldehyde; Obtain water-based low molecule phenolic paint with mixture cresol and formaldehyde reaction simultaneously.Gluing adopts the mode of secondary gluing, and first use low molecule phenolic impregnated brown paper is also dried, the more oily modification xylenols urea formaldehyde of this brown paper is carried out second time dipping, and the laminated board normality dielectric dissipation factor finally obtained is 0.032 ~ 0.034.Japan Patent (JP5216508) is obtained oily modification xylenols urea formaldehyde first, then lacquer type organic coating is obtained with epoxy E-20 is composite with it, take the mode gluing of the gluing identical with patent (JP5116067), the dielectric dissipation factor of final obtained laminated board normality is: 0.029 ~ 0.0302.
The dimethylbenzene phenol-formaldehyde resin modified related in above-mentioned domestic patent, different from the xylenols urea formaldehyde Application Areas related to herein, the different properties of requirement, therefore synthesis material and mode different, thus make the structure of resin different.The xylenols urea formaldehyde related in Japan Patent, all have tung oil or linseed oil to participate in modification together, gluing mode all adopts secondary gluing, and technique is more complicated, and the dielectric dissipation factor of its laminated board is all about 0.03.
Summary of the invention
The technical problem to be solved in the present invention is to provide a kind of low dielectric loss laminated phenolic paper plate and preparation method thereof, and the method step is simple, fast, the dielectric dissipation factor of use the method gained laminated phenolic paper plate is little, electrical strength is large and breakdown voltage is high.
A preparation method for low dielectric loss laminated phenolic paper plate, comprises the following steps: with matrix resin lysate or hybrid resin lysate direct impregnation paper, then obtain prepreg through baking and banking up with earth, then by superimposed for prepreg hot-forming and get final product;
The preparation method of wherein said matrix resin lysate is:
Dimethylbenzene formaldehyde 54 ~ 150 weight portion and p-methyl benzenesulfonic acid 0.4 ~ 1.0 weight portion of a, phenol 100 weight portion, number-average molecular weight 250-700 mix, and react 30 ~ 60min, obtain mixture 1 at the temperature of 105 ~ 112 DEG C;
B, in mixture 1, add triethanolamine 0.8 ~ 1.5 weight portion, cool to less than 90 DEG C and add formaldehyde 54 ~ 100 weight portion, triethylamine 0.49 ~ 1 weight portion and ammoniacal liquor 1.5 ~ 2.2 weight portion again, mix, be warmed up to 100 DEG C of reaction 1.5 ~ 3h, then defoamer is added, heated under vacuum dehydration obtains matrix resin, adds dissolution with solvents matrix resin, obtains matrix resin lysate;
The preparation method of wherein said hybrid resin lysate is: by novolac epoxy resin dissolution with solvents, obtain novolac epoxy resin lysate, novolac epoxy resin lysate is mixed with described matrix resin lysate, obtain hybrid resin lysate, the mass ratio of the matrix resin dissolved in the novolac epoxy resin dissolved in novolac epoxy resin lysate and matrix resin lysate is 1:9 ~ 3:7.
The preparation method of low dielectric loss laminated phenolic paper plate of the present invention, wherein said novolac epoxy resin is selected from one or more of following novolac epoxy resin: (1) molecular structure is such as formula shown in I and epoxide equivalent is 180 ~ 200g/eq; (2) molecular structure is such as formula shown in II and epoxide equivalent is 198 ~ 210g/eq; (3) molecular structure is as shown in formula III and epoxide equivalent is 230 ~ 250g/eq.The mensuration of epoxide equivalent is carried out according to the assay method in GBT 4612-2008 plastics-epoxide-epoxide equivalent.
The preparation method of low dielectric loss laminated phenolic paper plate of the present invention, the volatile content of wherein said prepreg is lower than 5%, and gel content is 45%.The test of volatile content performs according to standard A STM D3530/D3530M-97 (2008), and the test of gel content performs according to standard A STM D3529/D3529M-97 (2008).
The preparation method of low dielectric loss laminated phenolic paper plate of the present invention, in wherein said matrix resin lysate, the concentration of matrix resin is 45 ~ 50%(mass percent).
The preparation method of low dielectric loss laminated phenolic paper plate of the present invention, in wherein said novolac epoxy resin lysate, the concentration of novolac epoxy resin is 45 ~ 50%(mass percent).
The preparation method of low dielectric loss laminated phenolic paper plate of the present invention, adds one or more in solvent selected from methanol, toluene and acetone described in dissolution with solvents matrix resin.
The preparation method of low dielectric loss laminated phenolic paper plate of the present invention, by one or more in solvent selected from acetone described in novolac epoxy resin dissolution with solvents, toluene, glycol monoethyl ether and propylene glycol monomethyl ether.
The preparation method of low dielectric loss laminated phenolic paper plate of the present invention, wherein said paper is selected from one or more of bleached wood pulp paper, rag paper and bottom paper.
The preparation method of low dielectric loss laminated phenolic paper plate of the present invention, wherein the method for phenol, dimethylbenzene formaldehyde and p-methyl benzenesulfonic acid mixing is: by mixing after phenol and dimethylbenzene formaldehyde separately heating and melting and being cooled under 50 DEG C, then add the p-methyl benzenesulfonic acid dissolved with methyl alcohol wherein.
The preparation method of low dielectric loss laminated phenolic paper plate of the present invention, wherein said hot-forming method is: 125 DEG C of pre-temperature 30min, 160 DEG C, pressure 80kg/cm
2hot pressing 2h, cooling down.
The preparation method of low dielectric loss laminated phenolic paper plate of the present invention, wherein said defoamer is dimethicone.
Present invention also offers a kind of low dielectric loss laminated phenolic paper plate obtained by above-mentioned preparation method.
Preparation method's step of low dielectric loss laminated phenolic paper plate of the present invention is simple, quick, the laminated paper board dielectric dissipation factor under 1MHz standby by xylenols aldehyde radical body resin-made can reach 0.020, perpendicular layers in 90 DEG C of oil can reach 15kV/mm to electrical strength, and in 90 DEG C of oil, parallel layers can reach 48kV to breakdown voltage; The dielectric dissipation factor of the laminated paper board obtained with hybrid resin under 1MHz can reach 0.012, perpendicular layers in 90 DEG C of oil can reach 20kV/mm to electrical strength, in 90 DEG C of oil, parallel layers can reach 67kV to breakdown voltage, may be used in high-voltage mutual inductor, effectively reduce the thermal losses caused of dielectric loss, enhance the security of high-voltage mutual inductor.
Detailed description of the invention
Embodiment 1
(1) preparation of matrix resin lysate
A, be a weight portion with 2.25g, phenol 225g(is equivalent to 100 weight portions) and number-average molecular weight be that the dimethylbenzene formaldehyde 123g(of 250-700 is equivalent to 54.67 weight portions) mix after heating and melting separately and be cooled under 50 DEG C, then add the p-methyl benzenesulfonic acid 0.9g(dissolved with a small amount of methyl alcohol wherein and be equivalent to 0.40 weight portion), mix, at the temperature of 105 DEG C, react 30min, obtain mixture 1;
B, in mixture 1, add triethanolamine 1.8g(be equivalent to 0.80 weight portion), cool to less than 90 DEG C and add 123g formaldehyde (being equivalent to 54.67 weight portions), 1.1g triethylamine (being equivalent to 0.49 weight portion), 3.5g ammoniacal liquor (being equivalent to 1.56 weight portions) again, mix, after being warmed up to 100 DEG C of reaction 3h, drip proper quantity of defoaming agent dimethicone, thermal dehydration under vacuumized conditions, vacuum is-0.085MPa, stop dehydration obtaining matrix resin when temperature recovery to 90 DEG C, add methyl alcohol, make the matrix resin lysate that concentration is 45%;
(2) preparation of hybrid resin lysate
By molecular structure such as formula I and epoxide equivalent is the bisphenol A-type novolac epoxy resin acetone solution of 180 ~ 200g/eq, make the novolac epoxy resin lysate that concentration is 45%, novolac epoxy resin lysate is mixed with described matrix resin lysate, obtain hybrid resin lysate, the mass ratio of the matrix resin dissolved in the novolac epoxy resin dissolved in novolac epoxy resin lysate and matrix resin lysate is followed successively by 1:9,2:8,3:7;
(3) preparation of laminated board
Volatile content is cured to bleached wood pulp paper lower than 5% at 135 DEG C respectively with after matrix resin lysate or hybrid resin lysate dipping bleached wood pulp paper, gel content is 45%, obtain semi-solidization sheet, 125 DEG C of pre-temperature 30min again after being superposed by semisolid sheet, 160 DEG C, pressure 80kg/cm
2hot pressing 2h, cooling down and get final product.Matrix resin laminated paper board is designated as 1#, and mixing resin laminated cardboard is designated as 1a, 1b, 1c successively, and performance is as shown in table 1,
Table 1
The test condition of relative dielectric constant: frequency 1MHz, temperature 20 DEG C.
The test condition of dielectric dissipation factor is: voltage 1KV, frequency 1MHz, and sample is tested at 20 DEG C without any heat treatment.
Embodiment 2
(1) preparation of matrix resin lysate
A, be a weight portion with 2.25g, phenol 225g(is equivalent to 100 weight portions) and number-average molecular weight be that the dimethylbenzene formaldehyde 225g(of 250-700 is equivalent to 100 weight portions) mix after heating and melting separately and be cooled under 50 DEG C, then add the p-methyl benzenesulfonic acid 1.2g(dissolved with a small amount of methyl alcohol wherein and be equivalent to 0.53 weight portion), mix, at the temperature of 112 DEG C, react 45min, obtain mixture 1;
B, in mixture 1, add triethanolamine 2.3g(be equivalent to 1.02 weight portions), cool under 90 DEG C and add 164g formaldehyde (being equivalent to 72.89 weight portions), 1.7g triethylamine (being equivalent to 0.76 weight portion), 5.0g ammoniacal liquor (being equivalent to 2.22 weight portions) again, mix, after being warmed up to 100 DEG C of reaction 2h, drip proper quantity of defoaming agent dimethicone, thermal dehydration under vacuumized conditions, vacuum is-0.085MPa, stop dehydration obtaining matrix resin when temperature recovery to 90 DEG C, add toluene, make the matrix resin lysate that concentration is 50%;
(2) preparation of hybrid resin lysate
By molecular structural formula such as formula II and the orthoresol type novolac epoxy resin methyl alcohol of epoxide equivalent 198 ~ 210g/eq dissolve, make the novolac epoxy resin lysate that concentration is 50%, novolac epoxy resin lysate is mixed with described matrix resin lysate, obtain hybrid resin lysate, the mass ratio of the matrix resin dissolved in the novolac epoxy resin dissolved in novolac epoxy resin lysate and matrix resin lysate is followed successively by 1:9,2:8,3:7;
(3) preparation method of laminated board
The preparation method of laminated board is identical with embodiment 1, replaces bleached wood pulp paper with rag paper.Matrix resin laminated paper board is designated as 2#, and mixing resin laminated cardboard is designated as 2a, 2b, 2c successively, and performance is as shown in table 2,
Table 2
The test condition of relative dielectric constant: frequency 1MHz, temperature 20 DEG C.
The test condition of dielectric dissipation factor is: voltage 1KV, frequency 1MHz, and sample is tested at 20 DEG C without any heat treatment.
Embodiment 3
(1) preparation of matrix resin lysate
A, be a weight portion with 1.50g, phenol 150g(is equivalent to 100 weight portions) and number-average molecular weight be that the dimethylbenzene formaldehyde 225g(of 250-700 is equivalent to 150 weight portions) mix after heating and melting separately and be cooled under 50 DEG C, then add the p-methyl benzenesulfonic acid 1.5g(dissolved with a small amount of methyl alcohol wherein and be equivalent to 1 weight portion), mix, react 60min at 108 DEG C after, obtain mixture 1;
B, in mixture 1, add triethanolamine 2.2g(be equivalent to 1.47 weight portions), cool under 90 DEG C and add 150g formaldehyde (being equivalent to 100 weight portions), 1.5g triethylamine (being equivalent to 1 weight portion), 3.7g ammoniacal liquor (being equivalent to 2.47 weight portions) again, mix, after being warmed up to 100 DEG C of reaction 1.5h, drip proper quantity of defoaming agent dimethicone, thermal dehydration under vacuumized conditions, vacuum is-0.085MPa, stop dehydration obtaining matrix resin when temperature recovery to 90 DEG C, add acetone, make the matrix resin lysate that concentration is 47%;
(2) preparation of hybrid resin lysate
By molecular structural formula as formula III and the aralkylphenol type novolac epoxy resin spent glycol monomethyl ether of epoxide equivalent 230 ~ 250g/eq dissolve, make the novolac epoxy resin lysate that concentration is 47%, novolac epoxy resin lysate is mixed with described matrix resin lysate, obtain hybrid resin lysate, the mass ratio of the matrix resin dissolved in the novolac epoxy resin dissolved in novolac epoxy resin lysate and matrix resin lysate is followed successively by 1:9,2:8,3:7;
(3) preparation method of laminated board
The preparation method of laminated board is identical with embodiment 1, replaces bleached wood pulp paper with bottom paper.Matrix resin laminated paper board is designated as 3#, and mixing resin laminated cardboard is designated as 3a, 3b, 3c successively, and performance is as shown in table 3,
Table 3
The test condition of relative dielectric constant: frequency 1MHz, temperature 20 DEG C.
The test condition of dielectric dissipation factor is: voltage 1KV, frequency 1MHz, and sample is tested at 20 DEG C without any heat treatment.
Above-described embodiment is only be described the preferred embodiment of the present invention; not scope of the present invention is limited; under not departing from the present invention and designing the prerequisite of spirit; the various distortion that those of ordinary skill in the art make technical scheme of the present invention and improvement, all should fall in protection domain that claims of the present invention determines.
Claims (10)
1. a preparation method for low dielectric loss laminated phenolic paper plate, is characterized in that comprising the following steps: with matrix resin lysate or hybrid resin lysate direct impregnation paper, then obtain prepreg through baking and banking up with earth, then by superimposed for prepreg hot-forming and get final product;
The preparation method of wherein said matrix resin lysate is:
Dimethylbenzene formaldehyde 54 ~ 150 weight portion and p-methyl benzenesulfonic acid 0.4 ~ 1.0 weight portion of a, phenol 100 weight portion, number-average molecular weight 250 ~ 700 mix, and react 30 ~ 60min, obtain mixture 1 at the temperature of 105 ~ 112 DEG C;
B, in mixture 1, add triethanolamine 0.8 ~ 1.5 weight portion, cool to less than 90 DEG C and add formaldehyde 54 ~ 100 weight portion, triethylamine 0.49 ~ 1 weight portion and ammoniacal liquor 1.5 ~ 2.5 weight portion again, mix, be warmed up to 100 DEG C of reaction 1.5 ~ 3h, then defoamer is added, heated under vacuum dehydration obtains matrix resin, adds dissolution with solvents matrix resin, obtains matrix resin lysate;
The preparation method of wherein said hybrid resin lysate is: by novolac epoxy resin dissolution with solvents, obtain novolac epoxy resin lysate, novolac epoxy resin lysate is mixed with described matrix resin lysate, obtain hybrid resin lysate, the mass ratio of the matrix resin dissolved in the novolac epoxy resin dissolved in novolac epoxy resin lysate and matrix resin lysate is 1:9 ~ 3:7.
2. the preparation method of low dielectric loss laminated phenolic paper plate according to claim 1, is characterized in that: described novolac epoxy resin is selected from one or more of following novolac epoxy resin: (1) molecular structure is such as formula shown in I and epoxide equivalent is 180 ~ 200g/eq; (2) molecular structure is such as formula shown in II and epoxide equivalent is 198 ~ 210g/eq; (3) molecular structure is as shown in formula III and epoxide equivalent is 230 ~ 250g/eq.
3. the preparation method of low dielectric loss laminated phenolic paper plate according to claim 2, is characterized in that: the volatile content of described prepreg is lower than 5%, and gel content is 45%.
4. according to the preparation method of the low dielectric loss laminated phenolic paper plate one of claim 1-3 Suo Shu, it is characterized in that: described paper is selected from one or more of bleached wood pulp paper, rag paper and bottom paper.
5. the preparation method of low dielectric loss laminated phenolic paper plate according to claim 4, it is characterized in that: in described matrix resin lysate, the concentration of matrix resin is 45 ~ 50%, in described novolac epoxy resin lysate, the concentration of novolac epoxy resin is 45 ~ 50%.
6. the preparation method of low dielectric loss laminated phenolic paper plate according to claim 5, is characterized in that: add one or more in solvent selected from methanol, toluene and acetone described in dissolution with solvents matrix resin.
7. the preparation method of low dielectric loss laminated phenolic paper plate according to claim 5, is characterized in that: by one or more in solvent selected from acetone described in novolac epoxy resin dissolution with solvents, methyl alcohol, glycol monoethyl ether and propylene glycol monomethyl ether.
8. the preparation method of low dielectric loss laminated phenolic paper plate according to claim 5, it is characterized in that: the method for phenol, dimethylbenzene formaldehyde and p-methyl benzenesulfonic acid mixing is: by mixing after phenol and dimethylbenzene formaldehyde separately heating and melting and being cooled under 50 DEG C, then add the p-methyl benzenesulfonic acid dissolved with methyl alcohol wherein.
9. the preparation method of low dielectric loss laminated phenolic paper plate according to claim 5, is characterized in that: described hot-forming method is: 125 DEG C of pre-temperature 30min, 160 DEG C, pressure 80kg/cm
2hot pressing 2h, cooling down.
10. one kind according to the claim 1-9 low dielectric loss laminated phenolic paper plate that prepared by the preparation method of low dielectric loss laminated phenolic paper plate described in any one.
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| CN101458983A (en) * | 2009-01-05 | 2009-06-17 | 中电电气集团有限公司 | Insulation laminated paper board and preparation thereof |
| CN101691449A (en) * | 2009-09-04 | 2010-04-07 | 广东生益科技股份有限公司 | Method for improving flame retardant efficiency of phenoxy phosphazene compound and prepreg, laminated board and laminated board for printed circuit prepared by method |
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| JPS62190261A (en) * | 1986-02-17 | 1987-08-20 | Toagosei Chem Ind Co Ltd | Insulating paste |
| JP3371916B2 (en) * | 1993-08-05 | 2003-01-27 | 三菱瓦斯化学株式会社 | Epoxy resin composition |
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| CN101458983A (en) * | 2009-01-05 | 2009-06-17 | 中电电气集团有限公司 | Insulation laminated paper board and preparation thereof |
| CN101691449A (en) * | 2009-09-04 | 2010-04-07 | 广东生益科技股份有限公司 | Method for improving flame retardant efficiency of phenoxy phosphazene compound and prepreg, laminated board and laminated board for printed circuit prepared by method |
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| Title |
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| 改性二甲苯甲醛树脂的研制及其在层压板中的应用;李庆华等;《绝缘材料通讯》;20001231;第4页右栏第2段至第5页左栏第2段，第6页表2 * |
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