CN103131373B - Composite adhesive for single-sided film reinforced little glue mica tape and preparation method thereof - Google Patents
Composite adhesive for single-sided film reinforced little glue mica tape and preparation method thereof Download PDFInfo
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- CN103131373B CN103131373B CN201310090395.4A CN201310090395A CN103131373B CN 103131373 B CN103131373 B CN 103131373B CN 201310090395 A CN201310090395 A CN 201310090395A CN 103131373 B CN103131373 B CN 103131373B
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Abstract
The invention relates to a composite adhesive for a single-sided film reinforced little glue mica tape and a preparation method thereof. The composite adhesive comprises the following raw materials: 1-20 parts of organic nano montmorillonite, 100-500 parts of bisphenol A type epoxy resin, 100-400 parts of acetone and 50-200 parts of toluene, wherein the organic nano montmorillonite is obtained by performing an aqueous solution ion exchange organic reaction on nano montmorillonite and alkyl methyl ammonium salt for 2 to 12 hours; and the mass ratio of the feeding amount of nano montmorillonite to the feeding amount of alkyl methyl ammonium salt is 1:0.2-1. The composite adhesive is high in compatibility with mica paper, and the adhesion force between the mica paper and the substrate film can be improved. In addition, the composite adhesive is simple in preparation process, low in cost and high in mechanical strength, the condensate formed by matching with epoxy-acid anhydride type VPI paint has high thermal deformation temperature, high impact strength, high tensile strength and low dielectric loss and can be expected to be widely applied to the fields of insulated mica products and the like.
Description
Technical field
The invention belongs to insulation mica products field, particularly relate to the composite gum of a kind of high-voltage motor single-sided film reinforcement low resin mica tape and the preparation method of this composite gum.
Background technology
Single-sided film reinforcement low resin mica tape is a kind of material for HV Electric Machine Coil lapped insulation, the insulation system that it is unique with one of epoxy-acid anhydrides type VPI insullac and other insulating material composition.The composite gum adopting in the manufacture of single-sided film reinforcement low resin mica tape is the main raw that affects product performance, traditional composite gum is all to adopt organic resin as matrix resin, because mica paper is inorganic mineral material, thereby poor with the consistency of organic resin, after formation mica tape, easily there is the phenomenon of mica paper and film layering, be unfavorable for the insulation processing of motor coil.
Therefore in prior art, the composite gum and the mica consistency that in the manufacture of single-sided film reinforcement low resin mica tape, adopt are poor.In order to meet the demand of practical application, be badly in need of exploitation with the single-sided film reinforcement low resin mica tape composite gum technology that mica consistency is good.
Summary of the invention
Technical problem to be solved by this invention is to overcome the deficiencies in the prior art, provide a kind of for single-sided film reinforcement low resin mica tape, and mica paper consistency is good, the composite gum that can improve adhesive power between mica paper and base material film.
The present invention also will provide a kind of preparation method of the composite gum for single-sided film reinforcement low resin mica tape simultaneously, the method technique is simple, cost is low, gained composite gum is with low cost, physical strength is high, coordinate the cured article of formation to there is higher heat-drawn wire, shock strength, tensile strength with epoxy-acid anhydrides type VPI paint and compared with low dielectric loss, and toughness increases, be expected to be used widely in fields such as insulation mica productss.
For solving the problems of the technologies described above, a kind of technical scheme that the present invention takes is:
For a composite gum for single-sided film reinforcement low resin mica tape, by weight, its composition of raw materials is as follows:
1～20 part of organic nano imvite;
100～500 parts of bisphenol A type epoxy resins;
100～400 parts, acetone;
50～200 parts of toluene;
Wherein, described organic nano imvite is that nano imvite carries out 2～12h at 40～80 DEG C aqueous solution ion-exchange with alkyl methyl ammonium salts organises and reacts gained, and wherein, the mass ratio that feeds intake of nano imvite and alkyl methyl ammonium salts is 1:0.2～1.
Preferably, the composition of raw materials of described composite gum is as follows:
2～15 parts of organic nano imvites;
150～250 parts of bisphenol A type epoxy resins;
100～200 parts, acetone;
50～70 parts of toluene.
According to further scheme of the present invention: described composite gum, by organic nano imvite and bisphenol A type epoxy resin, in toluene and acetone, is carried out intercalation gained in 60～100 DEG C of temperature and under stirring.
According to the present invention, described alkyl methyl ammonium salts can be for being selected from one or more the combination in two dodecyl dimethyl ammonium chloride, distearyl dimethyl ammonium chloride and hexadecyldimethyl benzyl ammonium ammonium chloride.
Described nano imvite (MTT) is that smectite clay (comprising that calcium base, sodium base, Sodium/Calcium base, magnesium base cover clay) forms through the dispersion of delaminating, the remodeling of purifying, super-fine classified, special organic composite, average wafer thickness is less than 25nm, smectite content is greater than 95%, commercially available acquisition.
Described bisphenol A type epoxy resin can be one or more the combination of commercial E44, E51 and CYD128, is not particularly limited.
The another technical scheme that the present invention takes is: a kind of preparation method of the composite gum for single-sided film reinforcement low resin mica tape, it comprises the steps:
(1), nano imvite being carried out at 40～80 DEG C to aqueous solution ion-exchange by proportioning with alkyl methyl ammonium salts organises and reacts 2～12h, after reaction finishes, successively after filtration, washing, vacuum-drying at 60～120 DEG C, pulverizes and sieves and obtain described organic nano imvite;
(2), the organic nano imvite of step (1) gained is mixed by proportioning with bisphenol A type epoxy resin, add the mixing solutions of acetone and toluene, in ultrasonic instrument, disperse 2～4h, then under 60～100 DEG C of stirrings, carry out intercalation 1～5h, finally filter and obtain described composite gum with 500 mesh sieves.
Preferably, in step (1), described washing adopts ethanol and water by volume for the mixture of 1:0.8～1.2 composition washs, and washs to the AgNO of washings 0.1M
3titration generates without white precipitate.
Preferably, in step (1), the mass ratio that feeds intake of nano imvite and alkyl methyl ammonium salts is 1:0.3～0.6.
Preferably, in step (1), described reaction is carried out at 55 DEG C～65 DEG C of temperature.
Preferably, in step (2), described reaction is carried out at 75 DEG C～100 DEG C of temperature.
Compared with prior art, tool of the present invention has the following advantages and significant beneficial effect:
Gained composite gum of the present invention has hot thixotropy, it is low temperature viscosity large (be conducive between film-mica bonding), high temperature viscosity rate of descent is high, be conducive to high-voltage motor single-sided film reinforcement low resin mica tape and manufacture composite gum fully wetting, infiltration in mica paper in moulding process, increase the gluing area of mica paper, thereby improved the adhesive power of mica paper and base material film.Owing to having adopted intercalation nano polynite technology, there is the capillary channel increasing in the glue-line-mica paper of the few adhesive tape of gained, be conducive to interpenetrating of vacuum pressure impregnation (VPI) insullac and composite gum, result is that the acid anhydrides in VPI insullac can be penetrated in glue-line, and high-temperature cross-linking curing reaction occurs glue-line under acid anhydrides effect; Equally, N+ in glue-line also can part reverse osmosis arrive VPI insullac inside, epoxy-acid anhydrides type VPI insullac is played to the promoter action of hot setting, after final film, composite gum, mica and VPI insullac solidify, form a fine and close entirety, realized without air-gap-insulated ideal effect.
Preparation method's technique of the present invention is simple, with low cost, gained composite gum physical strength is high, coordinate the cured article of formation to there is higher heat-drawn wire, shock strength, tensile strength with epoxy-acid anhydrides type VPI paint and compared with low dielectric loss, and toughness increases, be expected to be used widely in fields such as insulation mica productss.
Embodiment
Below in conjunction with specific embodiment, the present invention will be described in detail.
In each embodiment, nano imvite (MMT) is all selected the NANN0LIN DK-4 of Zhe-jiang Jiang Feng rainbow novel material limited-liability company below.Epoxy-acid anhydrides type high-voltage motor solvent-free paint is all selected the TH1149-6 of Chinese Suzhou Taihu Electric New Material Co. Ltd..
Embodiment 1
The present embodiment provides a kind of preparation method of the composite gum for single-sided film reinforcement low resin mica tape, and it comprises the steps:
(1), by two dodecyl dimethyl ammonium chloride 10g, nano imvite (MMT) 25g, distilled water 65g mixes, at 60 ± 5 DEG C, carry out the aqueous solution ion-exchange reaction that organises, reaction times 5～6h, reaction finishes, and filters, after filtering with ethanol: water=1:1(volume ratio) solution washing filter cake to the AgNO of washings 0.1M
3titration generates without white precipitate; Then vacuum-drying at 110～120 DEG C, pulverize, sieving makes organic nano imvite;
(2), by step (1) gained organic nano imvite 2g, CYD128 bisphenol A type epoxy resin 200g mixes, add the mixing solutions 200g(acetone of acetone and toluene: toluene=2:1 mass ratio), in ultrasonic instrument, disperse after 2h, under 80 ± 5 DEG C of stirrings, carry out intercalation 5h, finally filter with 500 mesh sieves, obtain described composite gum.
The thickness of preparing by this composite gum is the naked copper row that the few wrapped long 600mm of adhesive tape of 0.1mm, cross section are 5 × 20mm2, the number of plies is 10 layers, then carry out VPI insulation processing with TH1149-6, taking-up is put into press after drying and is carried out plastic squeeze, and the glue of extruding is carrying out before various performance tests solidifying 4h at 155 DEG C.
Embodiment 2
The present embodiment provides a kind of preparation method of the composite gum for single-sided film reinforcement low resin mica tape, and it comprises the steps:
(1), by distearyl dimethyl ammonium chloride 10g, nano imvite (MMT) 25g, distilled water 65g mixes, at 60 ± 5 DEG C, carry out the aqueous solution ion-exchange reaction that organises, reaction times 5～6h, reaction finishes, and filters, after filtering with ethanol: water=1:1(volume ratio) solution washing washings extremely generate without white precipitate with the AgNO3 titration of 0.1M; Then vacuum-drying at 100～110 DEG C, pulverize, sieving makes organic nano imvite.
(2), by step (1) gained organic nano imvite 6g, E44 bisphenol A type epoxy resin 200g mixes, add the mixing solutions 200g(acetone of acetone and toluene: toluene=2:1 mass ratio), in ultrasonic instrument, disperse after 2h, under 80 ± 5 DEG C of stirrings, carry out intercalation 6h, finally filter and obtain described composite gum with 500 mesh sieves.
The thickness of preparing by this composite gum is the naked copper row that the few wrapped long 600mm of adhesive tape of 0.1mm, cross section are 5 × 20mm2, the number of plies is 10 layers, then carry out VPI insulation processing with TH1149-6, taking-up is put into press after drying and is carried out plastic squeeze, and the glue of extruding is carrying out before various performance tests solidifying 4h at 155 DEG C.
Embodiment 3
The present embodiment provides a kind of preparation method of the composite gum for single-sided film reinforcement low resin mica tape, and it comprises the steps:
(1), by distearyl dimethyl ammonium chloride 10g, nano imvite (MMT) 25g, distilled water 65g mixes, at 60 ± 5 DEG C, carry out the aqueous solution ion-exchange reaction that organises, reaction times 5～6h, reaction finishes, and filters, after filtering with ethanol: water=1:1(volume ratio) solution washing washings to the AgNO with 0.1M
3titration generates without white precipitate; Then vacuum-drying at 110～120 DEG C, pulverize, sieving makes organic nano imvite.
(2), by step (1) gained organic nano imvite 10g, E44 bisphenol A type epoxy resin 200g mixes, add the mixing solutions 200g(acetone of acetone and toluene: toluene=2:1 mass ratio), in ultrasonic instrument, disperse after 2h, under 80 ± 5 DEG C of stirrings, carry out intercalation 6h, finally filter and obtain described composite gum with 500 mesh sieves.
The thickness of preparing by this composite gum is that the few wrapped long 600mm of adhesive tape of 0.1mm, cross section are 5 × 20mm
2naked copper row, the number of plies is 10 layers, then carries out VPI insulation processing with TH1149-6, takes out to put into press after drying and carry out plastic squeeze, the glue of extruding is carrying out solidifying 4h before various performance tests at 155 DEG C.
Embodiment 4
The present embodiment provides a kind of preparation method of the composite gum for single-sided film reinforcement low resin mica tape, and it comprises the steps:
(1), by two dodecyl dimethyl ammonium chloride 10g, nano imvite (MMT) 25g, distilled water 65g mixes, at 60 ± 5 DEG C, carry out the aqueous solution ion-exchange reaction that organises, reaction times 5～6h, reaction finishes, and filters, after filtering with ethanol: water=1:1(volume ratio) solution washing washings to the AgNO with 0.1M
3titration generates without white precipitate; Then vacuum-drying at 110～120 DEG C, pulverize, sieving makes organic nano imvite.
(2), by step (1) gained organic nano imvite 14g, E44 bisphenol A type epoxy resin 200g mixes, add the mixing solutions 200g(acetone of acetone and toluene: toluene=2:1 mass ratio), in ultrasonic instrument, disperse after 2h, under 90 ± 5 DEG C of stirrings, carry out intercalation 6h, finally filter and obtain described composite gum with 500 mesh sieves.
The thickness of preparing by this composite gum is the naked copper row that the few wrapped long 600mm of adhesive tape of 0.1mm, cross section are 5 × 20mm2, the number of plies is 10 layers, then carry out VPI insulation processing with TH1149-6, taking-up is put into press after drying and is carried out plastic squeeze, and the glue of extruding is carrying out before various performance tests solidifying 4h at 155 DEG C.
Embodiment 5
The present embodiment provides a kind of preparation method of the composite gum for single-sided film reinforcement low resin mica tape, and it comprises the steps:
(1), by hexadecyldimethyl benzyl ammonium ammonium chloride 15g, nano imvite (MMT) 25g, distilled water 65g mixes, at 60 ± 5 DEG C, carry out the aqueous solution ion-exchange reaction that organises, reaction times 5～6h, reaction finishes, and filters, after filtering with ethanol: water=1:1(volume ratio) solution washing washings to the AgNO with 0.1M
3titration generates without white precipitate; Then vacuum-drying at 110～120 DEG C, pulverize, sieving makes organic nano imvite.
(2), by step (1) gained organic nano imvite 6g, E51 bisphenol A type epoxy resin 200g mixes, add the mixing solutions 200g(acetone of acetone and toluene: toluene=2:1 mass ratio), in ultrasonic instrument, disperse after 2h, under 90 ± 5 DEG C of stirrings, carry out intercalation 4h, finally filter and obtain described composite gum with 500 mesh sieves.
The thickness of preparing by this composite gum is that the few wrapped long 600mm of adhesive tape of 0.1mm, cross section are 5 × 20mm
2naked copper row, the number of plies is 10 layers, then carries out VPI insulation processing with TH1149-6, takes out to put into press after drying and carry out plastic squeeze, the glue of extruding is carrying out solidifying 4h before various performance tests at 155 DEG C.
Embodiment 6
The present embodiment provides a kind of preparation method of the composite gum for single-sided film reinforcement low resin mica tape, and it comprises the steps:
(1), by hexadecyldimethyl benzyl ammonium ammonium chloride 8g, nano imvite (MMT) 25g, distilled water 65g mixes, at 60 ± 5 DEG C, carry out the aqueous solution ion-exchange reaction that organises, reaction times 5～6h, reaction finishes, and filters, after filtering with ethanol: water=1:1(volume ratio) solution washing washings to the AgNO with 0.1M
3titration generates without white precipitate; Then vacuum-drying at 110～120 DEG C, pulverize, sieving makes organic nano imvite.
(2), by step (1) gained organic nano imvite 6g, CYD128 bisphenol A type epoxy resin 200g mixes, add the mixing solutions 200g(acetone of acetone and toluene: toluene=2:1 mass ratio), in ultrasonic instrument, disperse after 2h, under 85 ± 5 DEG C of stirrings, carry out intercalation 6h, finally filter and obtain described composite gum with 500 mesh sieves.
The thickness of preparing by this composite gum is that the few wrapped long 600mm of adhesive tape of 0.1mm, cross section are 5 × 20mm
2naked copper row, the number of plies is 10 layers, then carries out VPI insulation processing with TH1149-6, takes out to put into press after drying and carry out plastic squeeze, the glue of extruding is carrying out solidifying 4h before various performance tests at 155 DEG C.
Composite gum to embodiment 1～6 and the insulated coil of making thereof are extruded the performance of glue and are tested according to corresponding national standard, and result is respectively referring to table 1 and table 2.
Comparative example 1
This example provides a kind of preparation method of composite gum of prior art, and it is appropriate by 100 parts of 6101#/601#/604# epoxy resin (commercially available), 50 parts of bi-maleimide modified tung oil acid anhydride resins (commercially available), organic carboxyl acid salt catalyst (zinc) 1-5 part, acetone, toluene mixes in right amount.
The thickness of preparing by this composite gum is the naked copper row that the long 600mm of 0.1mm single-sided film reinforcement low resin mica tape wrapped (half Die bag), cross section are 5 × 20mm2, the number of plies is 10 layers, then carry out VPI insulation processing with TH1149-6, taking-up is put into press after drying and is carried out plastic squeeze, and the glue of extruding is carrying out before various performance tests solidifying 4h at 155 DEG C.
The performance of the composite gum of table 1 embodiment 1～6
Table 2 embodiment 1～6 and comparative example 1 are extruded the performance of glue
As shown in Table 2, mechanical property and the resistance toheat of extruding glue according to the single-sided film reinforcement low resin mica tape lapped insulation coil of preparation of the present invention are higher than the composite gum of comparative example, and dielectric properties increase.
Above-described embodiment is only explanation technical conceive of the present invention and feature; its object is to allow person skilled in the art can understand content of the present invention and implement according to this; can not limit the scope of the invention with this; all equivalences that spirit is done according to the present invention change or modify, within all should being encompassed in protection scope of the present invention.
Claims (10)
1. for a composite gum for single-sided film reinforcement low resin mica tape, it is characterized in that: by weight, its composition of raw materials is as follows:
1～20 part of organic nano imvite;
100～500 parts of bisphenol A type epoxy resins;
100～400 parts, acetone;
50～200 parts of toluene;
Wherein, described organic nano imvite is that nano imvite carries out 2～12h at 40～80 DEG C aqueous solution ion-exchange with alkyl methyl ammonium salts organises and reacts gained, and wherein, the mass ratio that feeds intake of nano imvite and alkyl methyl ammonium salts is 1:0.2～1.
2. the composite gum for single-sided film reinforcement low resin mica tape according to claim 1, is characterized in that: the composition of raw materials of described composite gum is as follows:
2～15 parts of organic nano imvites;
150～250 parts of bisphenol A type epoxy resins;
100～200 parts, acetone;
50～70 parts of toluene.
3. the composite gum for single-sided film reinforcement low resin mica tape according to claim 1, it is characterized in that: described composite gum is by described organic nano imvite and described bisphenol A type epoxy resin, in described toluene and acetone, carry out intercalation gained in 60～100 DEG C of temperature and under stirring.
4. according to the composite gum for single-sided film reinforcement low resin mica tape described in any one claim in claims 1 to 3, it is characterized in that: described alkyl methyl ammonium salts is one or more the combination being selected from two dodecyl dimethyl ammonium chloride, distearyl dimethyl ammonium chloride and hexadecyldimethyl benzyl ammonium ammonium chloride.
5. according to the composite gum for single-sided film reinforcement low resin mica tape described in any one claim in claims 1 to 3, it is characterized in that: described nano imvite average wafer thickness is less than 25nm, and smectite content is greater than 95%.
6. according to the composite gum for single-sided film reinforcement low resin mica tape described in any one claim in claims 1 to 3, it is characterized in that: described bisphenol A type epoxy resin is one or more the combination of commercial E44, E51 and CYD128.
7. a preparation method for the composite gum for single-sided film reinforcement low resin mica tape described in any one claim in claim 1 to 6, is characterized in that: comprise the steps:
(1), nano imvite being carried out at 40～80 DEG C to aqueous solution ion-exchange by proportioning with alkyl methyl ammonium salts organises and reacts 2～12h, after reaction finishes, successively after filtration, washing, vacuum-drying at 60～120 DEG C, pulverizes and sieves and obtain described organic nano imvite;
(2), the organic nano imvite of step (1) gained is mixed by proportioning with bisphenol A type epoxy resin, add the mixing solutions of acetone and toluene, in ultrasonic instrument, disperse 2～4h, then under 60～100 DEG C of stirrings, carry out intercalation 1～5h, finally filter and obtain described composite gum with 500 mesh sieves.
8. preparation method according to claim 7, is characterized in that: in step (1), described washing adopts ethanol and water by volume for the mixture of 1:0.8～1.2 composition washs, and washs to the AgNO of washings 0.1M
3titration generates without white precipitate.
9. preparation method according to claim 8, is characterized in that: in step (1), described reaction is carried out at 55 DEG C～65 DEG C of temperature.
10. preparation method according to claim 8, is characterized in that: in step (2), described reaction is carried out at 75 DEG C～100 DEG C of temperature.
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| CN201310090395.4A CN103131373B (en) | 2013-03-20 | 2013-03-20 | Composite adhesive for single-sided film reinforced little glue mica tape and preparation method thereof |
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| CN107134328B (en) * | 2017-04-21 | 2019-01-25 | 南通中菱电力科技股份有限公司 | A kind of preparation method of few ageing-resistant mica tape of glue-type |
| CN108384479B (en) * | 2018-02-01 | 2019-12-03 | 苏州太湖电工新材料股份有限公司 | Adhesive of high thermal conductivity low resin mica tape and preparation method thereof and low resin mica tape |
| CN109467678A (en) * | 2018-11-07 | 2019-03-15 | 哈尔滨电机厂有限责任公司 | A kind of high-voltage motor stator coil paulownia horse epoxy glass mica paper tape manufacturing method |
| CN111534260B (en) * | 2020-04-24 | 2021-12-14 | 北京康美特科技股份有限公司 | Epoxy resin packaging adhesive and preparation method and application thereof |
| CN115691859A (en) * | 2022-10-19 | 2023-02-03 | 湖北平安电工实业有限公司 | Calcined three-in-one mica tape and manufacturing process thereof |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1250790A (en) * | 1998-10-13 | 2000-04-19 | 中国科学院化学研究所 | Antiflowing epoxy resin/mentmorillonite compound and its preparing process |
| CN101659844A (en) * | 2008-08-26 | 2010-03-03 | 上海同立电工材料有限公司 | Radiation-resistant mica tape adhesive, preparation method thereof and application thereof |
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2013
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Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1250790A (en) * | 1998-10-13 | 2000-04-19 | 中国科学院化学研究所 | Antiflowing epoxy resin/mentmorillonite compound and its preparing process |
| CN101659844A (en) * | 2008-08-26 | 2010-03-03 | 上海同立电工材料有限公司 | Radiation-resistant mica tape adhesive, preparation method thereof and application thereof |
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