CN104449345A - High heat-resistance grade polyamideimide enameled wire varnish and preparation method thereof - Google Patents

High heat-resistance grade polyamideimide enameled wire varnish and preparation method thereof Download PDF

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Publication number
CN104449345A
CN104449345A CN201310421826.0A CN201310421826A CN104449345A CN 104449345 A CN104449345 A CN 104449345A CN 201310421826 A CN201310421826 A CN 201310421826A CN 104449345 A CN104449345 A CN 104449345A
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China
Prior art keywords
polyamide
dimethylacetamide
mol ratio
preparation
high temperature
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Pending
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CN201310421826.0A
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Chinese (zh)
Inventor
张建清
张斌
张国生
李岩
杨胜杰
张杏荣
钱新华
姚扎西
张芬萍
张衡伟
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DANYANG STAR CHEMICAL Co Ltd
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DANYANG STAR CHEMICAL Co Ltd
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Priority to CN201310421826.0A priority Critical patent/CN104449345A/en
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    • CCHEMISTRY; METALLURGY
    • C09DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09DCOATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
    • C09D179/00Coating compositions based on macromolecular compounds obtained by reactions forming in the main chain of the macromolecule a linkage containing nitrogen, with or without oxygen, or carbon only, not provided for in groups C09D161/00 - C09D177/00
    • C09D179/04Polycondensates having nitrogen-containing heterocyclic rings in the main chain; Polyhydrazides; Polyamide acids or similar polyimide precursors
    • C09D179/08Polyimides; Polyester-imides; Polyamide-imides; Polyamide acids or similar polyimide precursors
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08GMACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
    • C08G73/00Macromolecular compounds obtained by reactions forming a linkage containing nitrogen with or without oxygen or carbon in the main chain of the macromolecule, not provided for in groups C08G12/00 - C08G71/00
    • C08G73/06Polycondensates having nitrogen-containing heterocyclic rings in the main chain of the macromolecule
    • C08G73/10Polyimides; Polyester-imides; Polyamide-imides; Polyamide acids or similar polyimide precursors
    • C08G73/14Polyamide-imides
    • CCHEMISTRY; METALLURGY
    • C09DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09DCOATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
    • C09D5/00Coating compositions, e.g. paints, varnishes or lacquers, characterised by their physical nature or the effects produced; Filling pastes
    • C09D5/18Fireproof paints including high temperature resistant paints
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08LCOMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L2201/00Properties
    • C08L2201/08Stabilised against heat, light or radiation or oxydation

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  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Materials Engineering (AREA)
  • Wood Science & Technology (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Health & Medical Sciences (AREA)
  • Medicinal Chemistry (AREA)
  • Polymers & Plastics (AREA)
  • Macromolecular Compounds Obtained By Forming Nitrogen-Containing Linkages In General (AREA)

Abstract

The present invention relates to a high heat-resistance grade polyamideimide enameled wire varnish preparation method, which comprises: (1) preparing a high heat-resistance grade polyamideimide resin, wherein dimethylacetamide, 4,4'-diamino diphenyl ether, pyromellitic dianhydride, and 3,3',4,4'-benzophenonetetracarboxylic dianhydride or 4,4'-oxydiphthalic anhydride or 1,4-bis(3,4-dicarboxyphenoxy)benzene dianhydride are adopted to synthesize the resin, the dimethylacetamide and the 4,4'-diamino diphenyl ether are added to a reactor, stirring dissolving is performed, the mixed solution of pyromellitic dianhydride, 4,4'-diamino diphenyl ether, and 3,3',4,4'-benzophenonetetracarboxylic dianhydride or 4,4'-oxydiphthalic anhydride or the 1,4-bis(3,4-dicarboxyphenoxy)benzene dianhydride is added in an equal amount adding manner in eight batches, and a stirring reaction is performed until achieving a transparent state; and (2) taking the polyamideimide resin, dimethylacetamide and xylene, and uniformly stirring to obtain the high heat-resistance grade polyamideimide enameled wire varnish. The high heat-resistance grade polyamideimide enameled wire varnish of the present invention has good heat resistance, wherein the cut-through temperature is more than or equal to 400 DEG C, and the thermal shock temperature is more than or equal to 230 DEG C.

Description

A kind of high temperature classification polyamide-imide enamelled wire varnishes and preparation method thereof
Technical field
The present invention relates to the preparation of wire enamel, be specially a kind of high temperature classification polyamide-imide enamelled wire varnishes and preparation method thereof.
Background technology
Wire enamel is the indispensable electrical insulating coating being applied to electrical equipment, is one of critical materials controlling electric installation economic and technical norms and operation life.Along with epoch and expanding economy, all requirements at the higher level are proposed to the temperature resistant grade of enameled wire in military and people's livelihood field.
Polyamidoimide paint is the main raw material of universal high-performance composite coating enamel-cover circle, lenticular wire, is a kind of C level high temperature-resistant wire lacquer of high comprehensive performance, is widely used in the manufacture of traction electric machine, sealed electric-motor, the particularly coil of resistance to refrigerant condenser.There is in its backbone structure heat-resisting imide ring and flexible amide group simultaneously, thermotolerance is high, can life-time service at 210 DEG C, there is good mechanical property, dielectric properties, resistance to refrigerant and resistance to chemical corrosion, and have with the binding property of conductor, reelability and wear resistance and significantly promote.The cut through temperature of common polyamide imide enamelled wire varnishes, at about 350 DEG C, in order to adapt to the occasion of higher temperature classification, needs to provide a kind of polyamide-imide enamelled wire varnishes with higher temperature classification.
Summary of the invention
Technical problem to be solved by this invention is high temperature classification polyamide-imide enamelled wire varnishes providing a kind of cut through temperature more than 400 DEG C and preparation method thereof.
For solving the problems of the technologies described above, the invention provides a kind of preparation method of high temperature classification polyamide-imide enamelled wire varnishes, comprising the steps:
(1) preparation of high temperature classification polyamide-imide resin: adopt N,N-DIMETHYLACETAMIDE, 4, 4'-diaminodiphenyl oxide, pyromellitic acid anhydride, 3, 3', 4, 4'-benzophenone tetracarboxylic dianhydride carrys out synthetic resins, wherein 4, the mol ratio of 4'-diaminodiphenyl oxide and pyromellitic acid anhydride is 10:9 ~ 2:1, 4, 4'-diaminodiphenyl oxide and 3, 3', 4, the mol ratio of 4'-benzophenone tetracarboxylic dianhydride is 2:1 ~ 10:1, 3, 3', 4, 4'-benzophenone tetracarboxylic dianhydride+pyromellitic acid anhydride and 4, the mol ratio of 4'-diaminodiphenyl oxide is 4:5 ~ 5:4, N,N-DIMETHYLACETAMIDE and 4, the mol ratio of 4'-diaminodiphenyl oxide is 5:1 ~ 5:2,
Add N,N-DIMETHYLACETAMIDE, 4,4'-diaminodiphenyl oxides in reaction vessel, stirring and dissolving, divide 8 batches of equivalent to add the mixing solutions of pyromellitic acid anhydride and 4,4'-diaminodiphenyl oxide and 3,3', 4,4'-benzophenone tetracarboxylic dianhydride, stirring reaction is to transparent;
(2) get above-mentioned polyamide-imide resin, N,N-DIMETHYLACETAMIDE, dimethylbenzene, stir and obtain high temperature classification polyamide-imide enamelled wire varnishes, wherein the mol ratio of polyamide-imide resin, N,N-DIMETHYLACETAMIDE, dimethylbenzene is 20:3:3.
Described 3,3', 4,4'-benzophenone tetracarboxylic dianhydrides can be replaced with the two Tetra hydro Phthalic anhydride of 4,4'-oxygen or 3,3', 4,4'-triphen bis ether tetracarboxylic acid dianhydride, and consumption is consistent.
A kind of high temperature classification polyamide-imide enamelled wire varnishes, it adopts above-mentioned preparation method to obtain.
Technique effect of the present invention: the enameled wire good heat resistance that high temperature classification polyamide-imide enamelled wire varnishes prepared by (1) the present invention coats, 3,3' of introducing, 4, the two Tetra hydro Phthalic anhydride of 4'-benzophenone tetracarboxylic dianhydride, 4,4'-oxygen or 3,3', 4,4'-triphen bis ether tetracarboxylic acid dianhydride is all containing two or more phenyl ring, and rigid radical is more, thus enhances the thermotolerance of paint film, cut through temperature is more than 400 DEG C, and caloric impact temperature is more than 230 DEG C; (2) the enameled wire dielectric loss flex point coated is high, more than 190/250 DEG C; (3) this preparation method enormously simplify complete processing, improves production efficiency.
Embodiment
Embodiment 1
The preparation method of the high temperature classification polyamide-imide enamelled wire varnishes of the present embodiment, comprises the steps:
(1) preparation of high temperature classification polyamide-imide resin: get N,N-DIMETHYLACETAMIDE 10 parts, 4,4'-diaminodiphenyl oxide 2 parts, pyromellitic acid anhydride 1.5 parts, 3,3', 4,4'-benzophenone tetracarboxylic dianhydride 0.5 part, adds N,N-DIMETHYLACETAMIDE, 4,4'-diaminodiphenyl oxides in reaction vessel, stirring and dissolving, 8 batches of equivalent are divided to add pyromellitic acid anhydride, 3,3', 4, the mixing solutions of 4'-benzophenone tetracarboxylic dianhydride, stirring reaction is to transparent;
(2) get described polyamide-imide resin 20 parts, N,N-DIMETHYLACETAMIDE 3 parts, dimethylbenzene 3 parts, stir and obtain high temperature classification polyamide-imide enamelled wire varnishes.
Embodiment 2
The material of preparing of polyamide-imide resin in embodiment 1 is replaced with: N,N-DIMETHYLACETAMIDE 10 parts, 4,4'-diaminodiphenyl oxide 2 parts, pyromellitic acid anhydride 1 part, 3,3', 4,4'-benzophenone tetracarboxylic dianhydride 1 part, all the other steps are constant.
Embodiment 3
The material of preparing of polyamide-imide resin in embodiment 1 is replaced with: N,N-DIMETHYLACETAMIDE 10 parts, 4,4'-diaminodiphenyl oxide 2 parts, pyromellitic acid anhydride 1.5 parts, 3,3', 4,4'-triphen bis ether tetracarboxylic acid dianhydride 0.5 part; 3,3', 4,4'-benzophenone tetracarboxylic dianhydride replaces with 3,3', and 4,4'-triphen bis ether tetracarboxylic acid dianhydride, all the other steps are constant.
Embodiment 4
The material of preparing of polyamide-imide resin in embodiment 1 is replaced with: N,N-DIMETHYLACETAMIDE 10 parts, 4,4'-diaminodiphenyl oxide 2 parts, pyromellitic acid anhydride 1 part, 3,3', 4,4'-triphen bis ether tetracarboxylic acid dianhydride 1 part; 3,3', 4,4'-benzophenone tetracarboxylic dianhydride replaces with 3,3', and 4,4'-triphen bis ether tetracarboxylic acid dianhydride, all the other steps are constant.
Comparative example: with common polyamide imide enamelled wire varnishes (as four STAI68 reaching Chemical Co., Ltd.).
Comparative example and embodiment performance test as shown in the table.

Claims (6)

1. a preparation method for high temperature classification polyamide-imide enamelled wire varnishes, is characterized in that comprising the steps:
(1) preparation of high temperature classification polyamide-imide resin: adopt N,N-DIMETHYLACETAMIDE, 4,4'-diaminodiphenyl oxides, pyromellitic acid anhydride, 3,3', 4,4'-benzophenone tetracarboxylic dianhydride carrys out synthetic resins, adds N,N-DIMETHYLACETAMIDE, 4 in reaction vessel, 4'-diaminodiphenyl oxide, stirring and dissolving, point 8 batches of equivalent add pyromellitic acid anhydride and 4,4'-diaminodiphenyl oxide and 3,3', the mixing solutions of 4,4'-benzophenone tetracarboxylic dianhydride, stirring reaction is to transparent;
(2) get above-mentioned polyamide-imide resin, N,N-DIMETHYLACETAMIDE, dimethylbenzene, stir and obtain high temperature classification polyamide-imide enamelled wire varnishes.
2. the preparation method of high temperature classification polyamide-imide enamelled wire varnishes as claimed in claim 1, it is characterized in that: in step (1) 4, the mol ratio of 4'-diaminodiphenyl oxide and pyromellitic acid anhydride is 10:9 ~ 2:1,4,4'-diaminodiphenyl oxide and 3,3', the mol ratio of 4,4'-benzophenone tetracarboxylic dianhydride is 2:1 ~ 10:1,3,3', the mol ratio of 4,4'-benzophenone tetracarboxylic dianhydride+pyromellitic acid anhydride and 4,4'-diaminodiphenyl oxide is 4:5 ~ 5:4, the mol ratio of N,N-DIMETHYLACETAMIDE and 4,4'-diaminodiphenyl oxide is 5:1 ~ 5:2.
3. the preparation method of high temperature classification polyamide-imide enamelled wire varnishes as claimed in claim 2, is characterized in that: in step (2), the mol ratio of polyamide-imide resin, N,N-DIMETHYLACETAMIDE, dimethylbenzene is 20:3:3.
4. the preparation method of high temperature classification polyamide-imide enamelled wire varnishes as claimed in claim 3, is characterized in that: described 3,3', 4,4'-benzophenone tetracarboxylic dianhydride can with the two Tetra hydro Phthalic anhydride of 4,4'-oxygen or 3,3', 4,4'-triphen bis ether tetracarboxylic acid dianhydride is replaced, and consumption is consistent.
5. the high temperature classification polyamide-imide enamelled wire varnishes prepared of a preparation method as claimed in claim 1, it is characterized in that: in step (1) 4, the mol ratio of 4'-diaminodiphenyl oxide and pyromellitic acid anhydride is 10:9 ~ 2:1,4,4'-diaminodiphenyl oxide and 3,3', the mol ratio of 4,4'-benzophenone tetracarboxylic dianhydride is 2:1 ~ 10:1,3,3', the mol ratio of 4,4'-benzophenone tetracarboxylic dianhydride+pyromellitic acid anhydride and 4,4'-diaminodiphenyl oxide is 4:5 ~ 5:4, the mol ratio of N,N-DIMETHYLACETAMIDE and 4,4'-diaminodiphenyl oxide is 5:1 ~ 5:2;
In step (2), the mol ratio of polyamide-imide resin, N,N-DIMETHYLACETAMIDE, dimethylbenzene is 20:3:3.
6. high temperature classification polyamide-imide enamelled wire varnishes as claimed in claim 5, is characterized in that: described 3,3', 4,4'-benzophenone tetracarboxylic dianhydride can with the two Tetra hydro Phthalic anhydride of 4,4'-oxygen or 3,3', 4,4'-triphen bis ether tetracarboxylic acid dianhydride is replaced, and consumption is consistent.
CN201310421826.0A 2013-09-16 2013-09-16 High heat-resistance grade polyamideimide enameled wire varnish and preparation method thereof Pending CN104449345A (en)

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Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPH10199337A (en) * 1997-01-13 1998-07-31 Sumitomo Electric Ind Ltd Insulation wire
CN101139501A (en) * 2007-10-11 2008-03-12 同济大学 Polyimide thermostable aqueous dispersion coating material and preparation method and use thereof
CN102358808A (en) * 2011-09-02 2012-02-22 无锡百川化工股份有限公司 Polyamide-imide enameled wire varnish modifier and preparation method thereof
CN102838928A (en) * 2011-06-20 2012-12-26 日立电线株式会社 Polyamide-imide resin insulating coating material, insulated wire and coil

Patent Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPH10199337A (en) * 1997-01-13 1998-07-31 Sumitomo Electric Ind Ltd Insulation wire
CN101139501A (en) * 2007-10-11 2008-03-12 同济大学 Polyimide thermostable aqueous dispersion coating material and preparation method and use thereof
CN102838928A (en) * 2011-06-20 2012-12-26 日立电线株式会社 Polyamide-imide resin insulating coating material, insulated wire and coil
CN102358808A (en) * 2011-09-02 2012-02-22 无锡百川化工股份有限公司 Polyamide-imide enameled wire varnish modifier and preparation method thereof

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Application publication date: 20150325