EP0066194B1 - Procédé de préparation et utilisation d'une laque aqueuse durcissable à la chaleur, electriquement isolante - Google Patents

Procédé de préparation et utilisation d'une laque aqueuse durcissable à la chaleur, electriquement isolante Download PDF

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Publication number
EP0066194B1
EP0066194B1 EP82104390A EP82104390A EP0066194B1 EP 0066194 B1 EP0066194 B1 EP 0066194B1 EP 82104390 A EP82104390 A EP 82104390A EP 82104390 A EP82104390 A EP 82104390A EP 0066194 B1 EP0066194 B1 EP 0066194B1
Authority
EP
European Patent Office
Prior art keywords
polyester
imide
weight
aqueous
ammonia
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Expired
Application number
EP82104390A
Other languages
German (de)
English (en)
Other versions
EP0066194A3 (en
EP0066194A2 (fr
Inventor
Udo Dr. Reiter
Hans-Uwe Dr. Schenck
Helmut Lehmann
Ferdinand Hansch
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Beck Dr and Co GmbH
Original Assignee
Beck Dr and Co GmbH
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by Beck Dr and Co GmbH filed Critical Beck Dr and Co GmbH
Priority to AT82104390T priority Critical patent/ATE21575T1/de
Publication of EP0066194A2 publication Critical patent/EP0066194A2/fr
Publication of EP0066194A3 publication Critical patent/EP0066194A3/de
Application granted granted Critical
Publication of EP0066194B1 publication Critical patent/EP0066194B1/fr
Expired legal-status Critical Current

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Classifications

    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01B—CABLES; CONDUCTORS; INSULATORS; SELECTION OF MATERIALS FOR THEIR CONDUCTIVE, INSULATING OR DIELECTRIC PROPERTIES
    • H01B3/00—Insulators or insulating bodies characterised by the insulating materials; Selection of materials for their insulating or dielectric properties
    • H01B3/18—Insulators or insulating bodies characterised by the insulating materials; Selection of materials for their insulating or dielectric properties mainly consisting of organic substances
    • H01B3/30—Insulators or insulating bodies characterised by the insulating materials; Selection of materials for their insulating or dielectric properties mainly consisting of organic substances plastics; resins; waxes
    • H01B3/308—Wires with resins
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y10—TECHNICAL SUBJECTS COVERED BY FORMER USPC
    • Y10T—TECHNICAL SUBJECTS COVERED BY FORMER US CLASSIFICATION
    • Y10T428/00—Stock material or miscellaneous articles
    • Y10T428/31504—Composite [nonstructural laminate]
    • Y10T428/31721—Of polyimide

Definitions

  • the invention relates to a process for the preparation of aqueous thermosetting electrical insulating lacquers based on polyesterimides and their use as wire enamels or as impregnating lacquers, for. B. for the impregnation of enamelled wire windings.
  • polyesterimide solutions In order to process polyesterimide solutions well, relatively low solids contents have to be produced. Due to the specific solubility properties of PEI, phenols, cresols, xylenols, N-methylpyrrolidone, etc. must be used as solvents or as solvent mixtures. These solvents are mostly non-volatile, expensive and sometimes have a very unpleasant smell. In order to avoid unpleasant smells and environmental pollution from such solvents, very complex post-combustion systems are necessary.
  • aqueous systems have also been proposed as environmentally friendly and economical alternatives.
  • DE-A-23 51 077 and 23 51 078 describe aqueous PEI secondary dispersions.
  • these secondary dispersions have a solids content that is too low and also require special application devices.
  • FR-A-23 01 579 which corresponds to the content of DE-A-26 05 790, describes water-thinnable PEI electrical insulating lacquers which are tertiary with the aid of considerable amounts (5 to 30% by weight, preferably 20 to 30%) Amine and with the use of 5 to 20 wt.% Auxiliary solvent are converted into an aqueous form.
  • the paintwork thus obtained has softening points between 290 and 315 ° C.
  • DE-A-17 20 321 describes a process for the preparation of water-dilutable polyester imide resins with the aid of ammonia.
  • aromatic tricarboxylic anhydrides are first reacted with up to 80% of the stoichiometric amount of primary diamines which are necessary for imide formation and condensed with an excess of di- and / or trial alcohols.
  • the excess alcohol is then distilled off and the condensation product is heated to a temperature of above 80 ° C. with a small amount of aqueous ammonia, if appropriate with the addition of dialcohols, and the condensation product is then diluted with water.
  • FR-A-23 54 371 which corresponds to the content of DE-A-27 24 913, also shows water-soluble polyesterimide resins and processes for their preparation.
  • the products and manufacturing processes described herein result in products that have to be adjusted to a pH> 7 with amines, i. H. these products smell strongly of amines, which has an adverse effect on workplace hygiene.
  • larger amounts of auxiliary solvents are used (> 10%, as can be seen from the examples).
  • the object of the present invention is to provide a process for the production of aqueous thermosetting electrical insulating lacquers based on polyesterimides which makes it possible to easily obtain aqueous electrical insulating lacquers which do not have the disadvantages described above.
  • the present invention relates to a process for the preparation of aqueous thermosetting electrical insulating lacquers based on polyesterimides which have been obtained by condensation of aromatic tricarboxylic acid monoanhydrides, aromatic dicarboxylic acids or their esterifiable derivatives, diamines, diols and a triols containing an isocyanurate ring, which is characterized in that hydroxyl group-containing Polyesterimides with kinematic viscosities of 16 to 30 MM 2 - S - 1 (measured in a solution of 1 part of polyesterimide in 2 parts of N-methylpyrrolidone at 30 ° C) and acid numbers ⁇ 10 at temperatures between 80 and 130 ° C, optionally with use of up to 5% by weight, based on polyesterimide, of an organic solvent, with 5 to 15% by weight, based on polyesterimide, of ammonia in the form of an aqueous ammonia solution with aminolysis and hydrolysis, so that a solution with pH values between 6 and 6.9
  • the present invention also relates to the use of these aqueous electrical insulating lacquers as wire lacquers or impregnating lacquers.
  • water-thinnable lacquers are obtained by the process according to the invention, which show improved values in heat level compared to the water-thinnable lacquers obtained with tertiary amines.
  • the electrical insulating lacquers according to the invention are more economical and considerably more environmentally friendly due to the use of cheap ammonia instead of ethanolamines. They can be applied to the substrates to be coated using customary application systems and, after baking, show that the technical properties of the conventional polyesterimide lacquers dissolved in the above-mentioned organic solvents and thus problematic with regard to their environmental impact are at least equivalent.
  • polyesterimides to be used for the process according to the invention and their structural components it should be stated that the basic structure of suitable polyesterimides can be found in DE-AS 14 45 263 and DE-AS 14 55 100.
  • the hydroxyl-containing polyester imide to be used according to the invention can preferably be prepared by the process described in DE-OS 14 55 182.
  • the PEI are condensation products from aromatic tricarboxylic acid monoanhydrides, aromatic dicarboxylic acids or their derivatives, diamines, diols and triols with an isocyanurate ring.
  • trimellitic anhydride As aromatic tricarboxylic acid monoanhydrides such. B. consider trimellitic anhydride, 3,4,3'-benzophenone tricarboxylic anhydride and hemimellitic anhydride, with trimellitic anhydride being preferred.
  • Suitable aromatic dicarboxylic acids and their esterifiable derivatives are e.g. B. terephthalic acid, isophthalic acid, benzophenone-4,4'-dicarboxylic acid; Esters of aromatic dicarboxylic acids, such as. B. the esters of terephthalic acid with lower alcohols containing 1 to 3 carbon atoms, e.g. B. dimethyl terephthalate, dimethyl isophthalate, diethyl terephthalate.
  • diamines are preferably those with primary amino groups, which are bound to aromatic groups, for. B. those of the general formula where X for a divalent residue, e.g. B. -CH2-, -0-. -CO-, ⁇ S ⁇ or ⁇ SO 2 - stands.
  • Examples of such diamines are diaminodiphenylmethane, diaminodiphenyloxide and benzophenonediamine.
  • Suitable diols are customary dihydric aliphatic alcohols, such as: 1,4-butanediol, trimethylene glycol, preferably ethylene glycol.
  • Tricarboxylic acid monoanhydride, dicarboxylic acid (derivative), diamine, diol and triol are generally in a molar ratio of 1.7-2.8 / 0.5-1.2 / 0.7-1.4 / 0.4-1.2 / 0.8-1.4, preferably 1.9-2.110.7-1.0 / 0.9-1.1 / 0.5-0.8 / 1.0-1.3.
  • the hydroxyl-containing polyesterimides can be prepared, for example, by the process described in DE-OS 14 55 182. The condensation is carried out here in ethylene glycol, polyesterimides being obtained which no longer contain carboxyl groups and thus have no acid number.
  • the hydroxyl group-containing polyesterimides to be used for the process according to the invention have acid numbers ⁇ 10, preferably ⁇ 5 and kinematic viscosities of 16 to 30, preferably 18 to 28 mm 2 .
  • S ⁇ 1 (measured in a solution of 1 part by weight of polyesterimide in 2 parts by weight of N-methylpyrrolidone at 30 ° C).
  • the hydroxyl-containing polyesterimides are at temperatures between 80 and 130 ° C, preferably 90 and 110 ° C, optionally with the use of up to 5% by weight, based on PEI, of an organic solvent, with 5 to 15, preferably 7.5 to 10% by weight, based on PEI, of ammonia in the form of an aqueous ammonia solution, which can contain, for example, 5 to 25% by weight of ammonia, treated with aminolysis and hydrolysis.
  • the result is a weakly acidic aqueous solution with pH values between 6 and 6.9, preferably 6.5 and 6.9.
  • Suitable organic solvents are water-miscible solvents, such as.
  • the PEI solution which is expediently cooled to 20 to 50 ° C., can also be mixed with 0.1 to 5, preferably 2 to 4,% by weight, based on PEI, of a water-soluble curing catalyst .
  • water-soluble curing catalysts are preferably water-soluble titanates, such as. B. Titanium tetralactate.
  • the dilution of the polyesterimide solutions to viscosities between 100 and 10000 mPa. s is done by adding deionized water.
  • polyesterimide solutions prepared according to the invention can be used directly for coating wires, e.g. B. of copper wires or as impregnating varnish for impregnating enamelled wire windings.
  • the application methods and devices which are customary for this purpose come into question.
  • the coatings are generally baked at temperatures of 200 to 550, preferably 400 to 520 ° C.
  • thermosetting polyesterimide lacquers produced according to the invention have good storage stability, are completely clear and have no ammonia smell.
  • the paintwork thus obtained also shows excellent properties with regard to the softening temperature, the thermal shock and the thermal aging behavior.
  • the aqueous wire enamel thus obtained has a solids content of 52.3% with a continuous viscosity in the Ford cup (4 mm) according to DIN 53 211 of 41 seconds.
  • the varnish is applied to a copper wire of 0.5 mm 0 in 8 passes using a conventional wire varnishing furnace 2.50 m long and baked at 460 ° C.
  • the take-off speed was 22 m / min.
  • the enamelled wire had the following properties when tested according to DIN 46453: Comparative example (according to DE-AS 17 20 321)
  • Example 1 of DE-AS 1720321 was reworked.
  • the solution thus obtained was coated (baking temperature 460 ° C., take-off speed 22 m / min).

Landscapes

  • Physics & Mathematics (AREA)
  • Spectroscopy & Molecular Physics (AREA)
  • Paints Or Removers (AREA)
  • Organic Insulating Materials (AREA)
  • Macromolecular Compounds Obtained By Forming Nitrogen-Containing Linkages In General (AREA)
  • Macromonomer-Based Addition Polymer (AREA)
  • Compositions Of Macromolecular Compounds (AREA)
  • Polymers With Sulfur, Phosphorus Or Metals In The Main Chain (AREA)
  • Application Of Or Painting With Fluid Materials (AREA)

Claims (4)

1. Procédé de préparation de peintures ou vernis aqueuses, électroisolantes, durcissables à chaud, à base de polyesterimides, qui ont été obtenus par condensation d'anhydrides tricarboxyliques, d'acides aromatiques dicarboxyliques ou leurs dérivés, diamines, diols et triols contenant un noyau isocyanurate, caractérisé par le fait que des polyesterimides à groupes hydroxyde, d'une viscosité cinématique de 16 à 30 mm2. S-1 (mesurée dans une solution de 1 partie de polyestérimide dans 2 parties de N-méthyl- pyrrolidone, à 30 °C) et d'indice d'acide <10, à des températures comprises entre 80 et 130 °C, éventuellement avec utilisation de jusqu'à 5 % en poids, rapporté au polyestérimide, d'un solvant organique, sont traités, sous aminolyse et hydrolyse, avec 5 à 15 % en poids, rapporté au polyesterimide, d'ammoniaque sous forme de solution ammoniacale aqueuse, de manière qu'il en résulte une solution d'un pH compris entre 6 et 6, 9, et, par addition d'eau totalement dessalée, sont dilués à une viscosité comprise entre 100 et 10000 mPa. s, encore 0,1 à 5 % en poids, rapporté au polyestérimide, d'un catalyseur de durcissement, soluble dans l'eau, étant encore ajoutés après le traitement à l'ammoniaque.
2. Procédé selon la revendication 1, caractérisé par le fait que l'on utilise, comme triol contenant un noyau isocyanurate, du trishydroxyéthylisocyanurate.
3. Procédé selon la revendication 1 ou 2, caractérisé par le fait que l'on utilise, comme dérivé estérifiable d'un acide dicarboxylique aromatique, du téréphtalate de diméthyle.
4. Utilisation des peintures aqueuses, fabriquées par un procédé selon l'une des revendications précédentes, comme laques d'émaillage ou vernis au trempé.
EP82104390A 1981-05-29 1982-05-19 Procédé de préparation et utilisation d'une laque aqueuse durcissable à la chaleur, electriquement isolante Expired EP0066194B1 (fr)

Priority Applications (1)

Application Number Priority Date Filing Date Title
AT82104390T ATE21575T1 (de) 1981-05-29 1982-05-19 Verfahren zur herstellung waessriger hitzehaertbarer elektroisolierlacke und deren verwendung.

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
DE3121306A DE3121306C2 (de) 1981-05-29 1981-05-29 Verfahren zur Herstellung wäßriger hitzehärtbarer Elektroisolierlacke und deren Verwendung
DE3121306 1981-05-29

Publications (3)

Publication Number Publication Date
EP0066194A2 EP0066194A2 (fr) 1982-12-08
EP0066194A3 EP0066194A3 (en) 1983-04-20
EP0066194B1 true EP0066194B1 (fr) 1986-08-20

Family

ID=6133448

Family Applications (1)

Application Number Title Priority Date Filing Date
EP82104390A Expired EP0066194B1 (fr) 1981-05-29 1982-05-19 Procédé de préparation et utilisation d'une laque aqueuse durcissable à la chaleur, electriquement isolante

Country Status (8)

Country Link
US (1) US4439579A (fr)
EP (1) EP0066194B1 (fr)
JP (1) JPS57200465A (fr)
AT (1) ATE21575T1 (fr)
BR (1) BR8203143A (fr)
DE (2) DE3121306C2 (fr)
ES (1) ES8304190A1 (fr)
SU (1) SU1429936A3 (fr)

Families Citing this family (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPS60235047A (ja) * 1984-05-07 1985-11-21 Toyota Motor Corp 内燃機関用ヒ−タ付酸素センサの温度制御方法
US4562100A (en) * 1984-09-14 1985-12-31 E. I. Du Pont De Nemours And Company Polyimide coating compositions from diesterified anhydride and aromatic diamine
US4576990A (en) * 1984-11-15 1986-03-18 Nitto Electric Industrial Co., Ltd. Water-soluble insulating varnish
US4954543A (en) * 1988-10-17 1990-09-04 Gaf Chemicals Corporation Coating for increasing sensitivity of a radiation imageable polyacetylenic film
FR2664899B1 (fr) * 1990-07-18 1994-09-30 Chevalets Aubert Sa Composition et methode d'obtention des vernis electro-isolants contenant de l'eau a base de resines esterimides au trihydroxyethylisocyanurate destines a l'emaillage des fils electriques.
CN109468048B (zh) * 2018-10-29 2020-01-14 苏州太湖电工新材料股份有限公司 一种电子变压器用的水性绝缘漆及其制备方法和应用

Family Cites Families (25)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CA907236A (en) * 1972-08-08 General Electric Company Polyesterimide base coating compositions
DE1445263C3 (de) * 1961-12-12 1979-12-13 Dr. Beck & Co Ag, 2000 Hamburg Verwendung von Polyesterimiden für die Einbrennisolierung auf elektrischen Leitern
AT287304B (de) * 1961-11-02 1971-01-25 Beck & Co Gmbh Dr Verfahren zur Herstellung von neuen Esterimidharzen
DE1495100B2 (de) * 1961-11-02 1972-05-10 Dr. Beck & Co Ag, 2000 Hamburg Verfahren zur herstellung von polyesterimiden
DE1495152B2 (de) * 1963-11-15 1973-07-12 Dr. Beck & Co Ag, 2000 Hamburg Verfahren zur herstellung von hitzehaertbaren kunstharzen
US3852246A (en) * 1964-06-09 1974-12-03 Beck & Co Gmbh Polyesterimide resins
DE1495182C3 (de) * 1964-06-09 1978-03-09 Dr. Beck & Co Ag, 2000 Hamburg Verwendung von hitzehärtbaren PoIyesterimidharzen zur lösungsmittelfreien Weiterverarbeitung
US3426098A (en) * 1965-05-20 1969-02-04 Schenectady Chemical Polyester-polyimide wire enamel
DE1645435C1 (de) * 1965-05-20 1983-04-21 Schenectady Chemicals, Inc., Schenectady, N.Y. Verfahren zur Herstellung von Polyesterimiden
AT285943B (de) * 1967-11-11 1970-11-25 Beck & Co Ag Dr Verfahren zur Herstellung von wässerigen Esterimidharzlösungen
DE1720321C3 (de) * 1967-11-11 1979-10-11 Dr. Beck & Co Ag, 2000 Hamburg Wasserlösliche Esterimidharze
JPS569559B1 (fr) * 1970-03-12 1981-03-02
IT1021282B (it) * 1973-10-11 1978-01-30 Basf Ag Processo per la preparazione di dispersioni di poliesterimidi
DE2351078B2 (de) * 1973-10-11 1975-08-07 Basf Ag, 6700 Ludwigshafen Überzugsmittel für die Drahtlackierung
JPS51125197A (en) * 1974-11-07 1976-11-01 Furukawa Electric Co Ltd:The A method for preparing a water-soluble polyester solution
GB1528221A (en) * 1975-01-15 1978-10-11 Cean Spa Process for manufacturing enamels of polyester-polyimide resins particularly for coating electrical conductors
AT336748B (de) * 1975-02-19 1977-05-25 Beck & Co Ag Dr Verfahren zur herstellung wasserverdunnbarer elektroisolierlacke
DE2630758A1 (de) * 1975-08-08 1977-02-10 Stolllack Ag Verfahren zur herstellung von lack
US4127553A (en) * 1976-04-20 1978-11-28 Hitachi Chemical Company, Ltd. Electrical insulating resin composition comprising a polyester resin or ester-imide resin
US4179423A (en) * 1976-06-09 1979-12-18 Schenectady Chemicals, Inc. Water-soluble polyester imide resins
GB1557850A (en) * 1976-06-09 1979-12-12 Schenectady Midland Water soluble polyester imide resins
US4104221A (en) * 1976-08-24 1978-08-01 Dr. Beck & Co., Ag Process for making water diluted electroinsulation enamels
JPS6014783B2 (ja) * 1977-06-28 1985-04-16 三菱電機株式会社 水溶性塗料の製造法
JPS5950187B2 (ja) * 1977-09-13 1984-12-06 協和油化株式会社 水溶性塗料
US4290929A (en) * 1979-07-13 1981-09-22 Essex Group, Inc. Aqueous solutions of polyesterimides and methods of making the same

Also Published As

Publication number Publication date
ES512633A0 (es) 1983-02-16
EP0066194A3 (en) 1983-04-20
BR8203143A (pt) 1983-05-17
SU1429936A3 (ru) 1988-10-07
ES8304190A1 (es) 1983-02-16
DE3272692D1 (en) 1986-09-25
DE3121306A1 (de) 1982-12-23
JPS57200465A (en) 1982-12-08
US4439579A (en) 1984-03-27
DE3121306C2 (de) 1987-01-02
EP0066194A2 (fr) 1982-12-08
ATE21575T1 (de) 1986-09-15

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