CN102190955A - Method for preparing polyamideimide wire enamel from mixed solvent - Google Patents
Method for preparing polyamideimide wire enamel from mixed solvent Download PDFInfo
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- CN102190955A CN102190955A CN 201110084757 CN201110084757A CN102190955A CN 102190955 A CN102190955 A CN 102190955A CN 201110084757 CN201110084757 CN 201110084757 CN 201110084757 A CN201110084757 A CN 201110084757A CN 102190955 A CN102190955 A CN 102190955A
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Abstract
The invention relates to a method for preparing polyamideimide wire enamel from a mixed solvent. The polyamideimide wire enamel is prepared by performing copolymerization on a resin comprising components such as aromatic polycarboxylic acid or anhydride thereof, isocyanate and the like in the mixed solvent at the temperature of between 50 and 140 DEG C. The polyamideimide wire enamel has high stability, excellent bonding property on copper leads and generally used basic coating of polyester or polyamideimide, lower viscosity compared with that of wire enamel singly using N-methylpyrrolidone as a main solvent and convenience in wire painting. In the polyamideimide wire enamel, various property indexes can meet or exceed requirements of international electrotechnical commission (IEC) standard; softening and breakdown temperature can reach more than 360 DEG C; and solid content can be up to 40 percent.
Description
Technical field
The present invention relates to prepare the novel method and the technology of polyamide-imide resin, be used to prepare highly filled, the high softening wire enamel that punctures temperature.
Background technology
In recent years, electrical equipment is towards high performance, miniaturization development, and therefore the wherein used miniaturization of important components and parts coil, lightweight will improve to some extent.Along with the miniaturization of coil, its working temperature also can raise certainly gradually, and wherein employed wire enamel also will use thermotolerance high, in the insullac of these good heat resistances, have the call no more than polyamide-imide enamelled wire varnishes.
Polyamide-imide enamelled wire varnishes is a kind of high comprehensive performance high temperature-resistant wire lacquer, is one of principal item of high temperature-resistant wire lacquer more than 200 grades in the world.It has not only kept the thermotolerance height, can be in the performance of 200 ℃ of following life-time service, and have good mechanical performance, resistance to chemical corrosion and cold-resistant matchmaker's property, and binding property, pliability with conductor have been improved significantly, wear resistance also increases simultaneously, and the mechanical property of paint film obtains balance preferably.
The polyamide-imide enamelled wire varnishes that provides on the market all is in the solution of N-Methyl pyrrolidone, fill by hydrocarbon in some cases, and N-Methyl pyrrolidone is expensive solvent, and corresponding relatively poor to the additive that uses.The preparation technology of present polyamide-imide resin, generally below 120 ℃, the reaction times is longer for its polymeric reaction temperature, causes its production cycle longer, and labour productivity is not high.
Summary of the invention
At above deficiency, the object of the present invention is to provide a kind of mixed solvent to prepare the method for polyamide-imide enamelled wire varnishes, guaranteeing that resinogen has under the prerequisite that performance do not descend, and shortens polymerization reaction time, to reduce corresponding energy consumption, labour wage, improve plant factor, unit output.Simultaneously, also study under the prerequisite that guarantees the wire enamel performance, use other solvents replacements or part to replace the N-Methyl pyrrolidone solvent, to reduce product cost.
The present invention solves the problems of the technologies described above the technical scheme that is adopted: a kind of mixed solvent prepares the method for polyamide-imide enamelled wire varnishes, prepare the polyamide-imide resin that wire enamel is used with mixed solvent, between 50 ~ 140 ℃, form, it is characterized in that through the reaction copolymerization:
Polyamide-imide enamelled wire varnishes comprises following component:
Aromatic multi-carboxy acid or its anhydrides 13 ~ 40 weight parts
Isocyanates 15 ~ 30 weight parts
Catalyzer 0.3 ~ 3 weight part
Mixed solvent 20 ~ 60 weight parts
Stopper 2.5 ~ 5 weight parts
Wherein: aromatic multi-carboxy acid or its anhydrides are one or more of benzenetricarboxylic acid or its acid anhydrides, pyromellitic acid or its acid anhydrides; Isocyanates is a tolylene diisocyanate, 2,4-diphenylmethanediisocyanate and 4, one or more of 4'-diphenylmethanediisocyanate, hexamethylene diisocyanate, polymeric polyisocyanate; Catalyzer is one or more of formic acid, acetate, zinc acetate, titanic acid ester, pyridine etc.; Mixed solvent is two or more a mixed solvent of N-Methyl pyrrolidone, ethylene glycol ether acetate, dimethyl formamide, dimethylbenzene, solvent oil, gamma-butyrolactone; Stopper is one or more of phenylcarbinol, methyl alcohol, ethanol, isopropylcarbinol, phosphoric acid.
Its preparation method: get aromatic multi-carboxy acid or its anhydrides 13 ~ 40 weight parts, isocyanates 15 ~ 30 weight parts, catalyzer 0.3 ~ 3 weight part, mixed solvent 20 ~ 60 weight parts add polyreaction in the reactor, a little heat or be warming up to 50 ℃ naturally, be incubated and slowly be warming up to 60 ~ 80 ℃ after 2 ~ 4 hours, heat up again after being incubated 2 ~ 5 hours again, after temperature rises to 130 ~ 140 ℃, every sampling and testing resin viscosity half an hour, cone-plate viscosity in the time of 30 ℃ reaches 280 ~ 650mPa.s(resin: behind the N-Methyl pyrrolidone=1:1), promptly stop heating, add stopper 2.5 ~ 5 weight parts, termination reaction, after adding mixed solvent 10 ~ 30 weight parts again, filter discharging.
The polyamide-imide enamelled wire varnishes that the present invention makes, good stability, subcoat to copper conductor and normally used polyester or polyester-imide base has good binding property, and viscosity ratio to do the wire enamel viscosity of main solvent with N-Methyl pyrrolidone separately low, be convenient to be coated with line.Every performance index all satisfy or are higher than the requirement of International Power IEC standard, wherein softeningly puncture temperature and can reach more than 360 ℃, and can be made into solids content up to 40% wire enamel.
Embodiment
Embodiment 1:
Mixed solvent prepares the method for polyamide-imide enamelled wire varnishes: get benzenetricarboxylic acid or its acid anhydrides 15 weight parts, tolylene diisocyanate 20 weight parts, formic acid 1 weight part, N-Methyl pyrrolidone 10 ~ 20 weight parts, ethylene glycol ether acetate 10 ~ 20 weight parts, add polyreaction in the reactor, a little heat or be warming up to 50 ℃ naturally, be incubated and slowly be warming up to 60 ~ 80 ℃ after 2 ~ 4 hours, heat up again after being incubated 2 ~ 5 hours again, after temperature rises to 130 ~ 140 ℃, every sampling and testing resin viscosity half an hour, cone-plate viscosity when reaching 30 ℃ of viscosity reaches 280 ~ 650mPa.s(resin: behind the N-Methyl pyrrolidone=1:1), promptly stop heating, add stopper phenylcarbinol 5 weight parts, termination reaction, add mixed solvent N-Methyl pyrrolidone and ethylene glycol ether acetate and solvent oil again behind totally 10 ~ 30 weight parts, filter discharging.
Embodiment 2:
Mixed solvent prepares the method for polyamide-imide enamelled wire varnishes: get benzenetricarboxylic acid or its acid anhydrides, pyromellitic acid or its acid anhydrides be totally 30 weight parts, 2,4-diphenylmethanediisocyanate and 4, each 15 weight part of 4'-diphenylmethanediisocyanate, acetate 2 weight parts, N-Methyl pyrrolidone 10 ~ 20 weight parts, dimethyl formamide 10 ~ 20 weight parts, add polyreaction in the reactor, a little heat or be warming up to 50 ℃ naturally, be incubated and slowly be warming up to 60 ~ 80 ℃ after 2 ~ 4 hours, heat up again after being incubated 2 ~ 5 hours again, after temperature rises to 130 ~ 140 ℃, every sampling and testing resin viscosity half an hour, cone-plate viscosity in the time of 30 ℃ reaches 280 ~ 650mPa.s(resin: behind the N-Methyl pyrrolidone=1:1), promptly stop heating, add stopper phenylcarbinol 5 weight parts, termination reaction, add the mixed solvent N-Methyl pyrrolidone again, dimethyl formamide and dimethylbenzene behind totally 10 ~ 30 weight parts, filter discharging.
The present invention controls speed of reaction by control reaction temperature in the control of technology, to prevent that polymerization is too fast and cause that molecular weight distribution is inhomogeneous, or reacted slowly and prolong the production time.
The japanning condition:
| Type, baker are long | MD5/2-2/24 high-speed wire-drawing enamelling machine, 8m |
| The japanning mode | Mould 6 roads |
| Oven drying temperature (℃) | 440/470/470 |
| Wire gauge | 0.50mm |
| Speed | 31m/min |
Technical performance index is as follows:
Can be found out by above-mentioned performance index, prepare polyamide-imide enamelled wire varnishes with the inventive method, solids content can reach 40%, and has higher dielectric loss and the softening temperature that punctures, and other performance index are unaffected simultaneously.And the polyamide-imide enamelled wire varnishes solids content of general method preparation does not reach 40%, and dielectric loss and softening puncture temperature are lower.Temperature of reaction is between 50 ~ 140 ℃, and wherein, the reaction times that is higher than 120 ℃ decides according to required viscosity.
Claims (7)
1. a mixed solvent prepares polyamide-imide enamelled wire varnishes, prepares the polyamide-imide resin that wire enamel is used with mixed solvent, forms through the reaction copolymerization between 50 ~ 140 ℃, it is characterized in that:
Described polyamide-imide enamelled wire varnishes comprises following component:
Aromatic multi-carboxy acid or its anhydrides 13 ~ 40 weight parts
Isocyanates 15 ~ 30 weight parts
Catalyzer 0.3 ~ 3 weight part
Mixed solvent 20 ~ 60 weight parts
Stopper 2.5 ~ 5 weight parts.
2. a kind of mixed solvent according to claim 1 prepares polyamide-imide enamelled wire varnishes, it is characterized in that: aromatic multi-carboxy acid or its anhydrides are one or more of benzenetricarboxylic acid or its acid anhydrides, pyromellitic acid or its acid anhydrides.
3. a kind of mixed solvent according to claim 1 prepares polyamide-imide enamelled wire varnishes, it is characterized in that: described isocyanates is a tolylene diisocyanate, 2,4-diphenylmethanediisocyanate and 4, one or more of 4'-diphenylmethanediisocyanate, hexamethylene diisocyanate, polymeric polyisocyanate.
4. a kind of mixed solvent according to claim 1 prepares polyamide-imide enamelled wire varnishes, it is characterized in that: described catalyzer is one or more of formic acid, acetate, zinc acetate, titanic acid ester, pyridine etc.
5. a kind of mixed solvent according to claim 1 prepares polyamide-imide enamelled wire varnishes, it is characterized in that: described mixed solvent is two or more a mixed solvent of N-Methyl pyrrolidone, ethylene glycol ether acetate, dimethyl formamide, dimethylbenzene, solvent oil, gamma-butyrolactone.
6. a kind of mixed solvent according to claim 1 prepares polyamide-imide enamelled wire varnishes, it is characterized in that: described stopper is one or more of phenylcarbinol, methyl alcohol, ethanol, isopropylcarbinol, phosphoric acid.
7. one kind prepares the method that claim 1 mixed solvent prepares polyamide-imide enamelled wire varnishes: it is characterized in that: get aromatic multi-carboxy acid or its anhydrides 13 ~ 40 weight parts, isocyanates 15 ~ 30 weight parts, catalyzer 0.3 ~ 3 weight part, mixed solvent 20 ~ 60 weight parts add polyreaction in the reactor, a little heat or be warming up to 50 ℃ naturally, be incubated and slowly be warming up to 60 ~ 80 ℃ after 2 ~ 4 hours, heat up again after being incubated 2 ~ 5 hours again, after temperature rises to 130 ~ 140 ℃, every sampling and testing resin viscosity half an hour, cone-plate viscosity in the time of 30 ℃ reaches 280 ~ 650mPa.s(resin: behind the N-Methyl pyrrolidone=1:1), promptly stop heating, add stopper 2.5 ~ 5 weight parts, termination reaction, after adding mixed solvent 10 ~ 30 weight parts again, filter discharging.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 201110084757 CN102190955A (en) | 2011-04-06 | 2011-04-06 | Method for preparing polyamideimide wire enamel from mixed solvent |
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| Application Number | Priority Date | Filing Date | Title |
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| CN 201110084757 CN102190955A (en) | 2011-04-06 | 2011-04-06 | Method for preparing polyamideimide wire enamel from mixed solvent |
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105295696A (en) * | 2015-11-19 | 2016-02-03 | 山东莱河电磁线有限公司 | Wear-resistant enamelled wire paint |
| CN106543431B (en) * | 2016-11-01 | 2018-12-07 | 万华化学集团股份有限公司 | A kind of imido method of synthesizing polyether |
| CN109096903A (en) * | 2018-07-27 | 2018-12-28 | 江苏恒兴制漆有限公司 | A kind of high-fire resistance wire enamel and preparation method thereof |
| CN111621225A (en) * | 2020-05-27 | 2020-09-04 | 苏州东特绝缘科技有限公司 | Preparation method of black polyamideimide coating, coating and enameled wire |
| CN114133564A (en) * | 2022-01-14 | 2022-03-04 | 兰州大学 | Polyamide-imide prepared by microchannel reactor and preparation method thereof |
| CN114566306A (en) * | 2022-03-16 | 2022-05-31 | 兰州大学 | Conductive silver paste and preparation method and application thereof |
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| CN1449424A (en) * | 2000-08-25 | 2003-10-15 | 施奈克泰迪国际公司 | Polyamide-imide resin solution and the use thereof for producing wire enamels |
| US20060025543A1 (en) * | 2003-01-30 | 2006-02-02 | Guenter Stevens | Process for the preparation of storage-stable polyamidoimide resins and coating materials which contain them |
| CN101124270A (en) * | 2005-02-21 | 2008-02-13 | Ls电线有限公司 | Enamel vanish composition for enamel wire and enamel wire using the same |
| CN101128543A (en) * | 2005-03-17 | 2008-02-20 | 日立化成工业株式会社 | Resin composition and coating film forming material containing the same |
| CN101397477A (en) * | 2007-09-29 | 2009-04-01 | 宝山钢铁股份有限公司 | Method for preparing polyamide-imide enamelled wire varnishes |
| CN101735716A (en) * | 2009-11-24 | 2010-06-16 | 丹阳四达化工有限公司 | Method for preparing corona-resistant wire enamel |
| CN101831240A (en) * | 2009-03-13 | 2010-09-15 | 日立卷线株式会社 | Insulating coating composition and insulated wire, and coil formed using the same |
-
2011
- 2011-04-06 CN CN 201110084757 patent/CN102190955A/en active Pending
Patent Citations (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1449424A (en) * | 2000-08-25 | 2003-10-15 | 施奈克泰迪国际公司 | Polyamide-imide resin solution and the use thereof for producing wire enamels |
| US20060025543A1 (en) * | 2003-01-30 | 2006-02-02 | Guenter Stevens | Process for the preparation of storage-stable polyamidoimide resins and coating materials which contain them |
| CN101124270A (en) * | 2005-02-21 | 2008-02-13 | Ls电线有限公司 | Enamel vanish composition for enamel wire and enamel wire using the same |
| CN101128543A (en) * | 2005-03-17 | 2008-02-20 | 日立化成工业株式会社 | Resin composition and coating film forming material containing the same |
| CN101397477A (en) * | 2007-09-29 | 2009-04-01 | 宝山钢铁股份有限公司 | Method for preparing polyamide-imide enamelled wire varnishes |
| CN101831240A (en) * | 2009-03-13 | 2010-09-15 | 日立卷线株式会社 | Insulating coating composition and insulated wire, and coil formed using the same |
| CN101735716A (en) * | 2009-11-24 | 2010-06-16 | 丹阳四达化工有限公司 | Method for preparing corona-resistant wire enamel |
Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105295696A (en) * | 2015-11-19 | 2016-02-03 | 山东莱河电磁线有限公司 | Wear-resistant enamelled wire paint |
| CN106543431B (en) * | 2016-11-01 | 2018-12-07 | 万华化学集团股份有限公司 | A kind of imido method of synthesizing polyether |
| CN109096903A (en) * | 2018-07-27 | 2018-12-28 | 江苏恒兴制漆有限公司 | A kind of high-fire resistance wire enamel and preparation method thereof |
| CN111621225A (en) * | 2020-05-27 | 2020-09-04 | 苏州东特绝缘科技有限公司 | Preparation method of black polyamideimide coating, coating and enameled wire |
| CN114133564A (en) * | 2022-01-14 | 2022-03-04 | 兰州大学 | Polyamide-imide prepared by microchannel reactor and preparation method thereof |
| CN114566306A (en) * | 2022-03-16 | 2022-05-31 | 兰州大学 | Conductive silver paste and preparation method and application thereof |
| CN114566306B (en) * | 2022-03-16 | 2023-10-03 | 兰州大学 | Conductive silver paste and preparation method and application thereof |
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Application publication date: 20110921 |