CN102942815A - Preparation method for environmental protection type polyamide-imide wire enamel - Google Patents
Preparation method for environmental protection type polyamide-imide wire enamel Download PDFInfo
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- CN102942815A CN102942815A CN2012104185084A CN201210418508A CN102942815A CN 102942815 A CN102942815 A CN 102942815A CN 2012104185084 A CN2012104185084 A CN 2012104185084A CN 201210418508 A CN201210418508 A CN 201210418508A CN 102942815 A CN102942815 A CN 102942815A
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Abstract
The present invention discloses a preparation method for an environment protection type polyamide-imide wire enamel. The preparation method comprises: adopting an ester solvent with a boiling point of more than 150 DEG C as a main solvent; adding the main solvent to a reactor, and stirring; heating to a temperature of 50-60 DEG C, and dissolving; pouring isocyanate and anhydride, controlling a reaction temperature to a range of 80-85 DEG C, and maintain for 1-3 h; heating to a temperature of 120-125 DEG C within 1 h, and maintain for 1-3 h; heating to a temperature of 155-160 DEG C within 1 h, and performing the reaction until a transparent state is achieved; cooling to a temperature of 130-135 DEG C, adding the main solvent, and concurrently and rapidly adding a mixture of a blocking agent and a catalyst, and carrying out thermal insulation for 1-1.5 h at a temperature of 100-115 DEG C; and finally adding a diluent to carry out wire enamel adjustment, wherein a solid content of the wire enamel is adjusted to 36-20%.
Description
Technical field
The present invention relates to a kind of wire enamel technology, relate in particular to a kind of preparation method of environment-friendly type polyamide-imide enamelled wire varnishes.
Background technology
Polyamidoimide has advantages of that high heat resistance, anti-refrigerant performance are good etc. outstanding, is widely used in producing the high heat-resisting high performance enameled wire that requires, such as the composite enameled wire with anti-refrigerant performance etc.
But there is again following shortcoming simultaneously in the polyamide-imide enamelled wire varnishes of producing at present, 1) cost is high, because its main solvent N-Methyl pyrrolidone price in the used solvent species of wire enamel is the highest, it is equally also converted to heat by catalyticcombustion in the Production of Enamel Wires process as solvent, and after N-Methyl pyrrolidone (NMP) burning heat of gained not as good as cresols (combustion heat: NMP=3010kJ/mol, cresols=3706kJ/mol).2) toxicity is large, and the main solvent N-Methyl pyrrolidone of using in the polyamide-imide enamelled wire varnishes at present has toxicity, is that restriction is used in chemical pact.The 5th batch of announcing in February, 2011 of Europe chemical management administration (ECHA) shown great attention to and just comprised N-Methyl pyrrolidone (1-methyl-2-pyrrolidone, CAS 872-50-4) in the material (REACH).3) deficiency in the enamelling technique process, because the polyamidoimide lacquer is as primary solvent take N-Methyl pyrrolidone, N-Methyl pyrrolidone is intensive polar solvent, the easy moisture absorption, wire enamel is exposed in the cylinder in the air and the moisture absorption at lacquer, particularly under the processing condition of felt japanning, cause resin in felt, to be separated out after the moisture absorption, block flowing of coating with lacquer in the felt, affect the japanning of enameled wire, the felt that will in time more renew so often takes two or three days in the time of moist day and changes once, both affect working efficiency, also increased the pollution to environment.4) immiscible with other kind enameled wire, present polyamide-imide enamelled wire varnishes all can not mix mutually with wire enamels take cresols as primary solvent such as polyester-imides, if after careless the mixing, can muddiness separate out immediately, bring very inconvenient to the enamel-cover process, such as, the cleaning during enamelling machine conversion production kind is clean especially, can produce a large amount of cleaning solvents like this; Also want SC when producing composite enameled wire, pay special attention to finish paint and can not mix with priming paint.
Present polyamide-imide enamelled wire varnishes had both had its irreplaceable outstanding advantages; be restricted again and awkward shortcoming; especially need for what constantly advance in conjunction with modern society; particularly to the environment protection aspect; just must change the main solvent of polyamide-imide enamelled wire varnishes, replace N-Methyl pyrrolidone with other main solvent.
Summary of the invention
The invention provides a kind of preparation method who does not prepare polyamide-imide enamelled wire varnishes take N-Methyl pyrrolidone as main solvent.
For achieving the above object, the present invention adopts following technical scheme:
The preparation method of environment-friendly type polyamide-imide enamelled wire varnishes, be higher than 150 ℃ of esters solvents as main solvent take boiling point, its preparation method comprises the steps: to add main solvent in reactor, stir, be warmed up to 50～60 ℃ of dissolvings, drop into isocyanic ester and acid anhydrides, the control temperature of reaction kept 1 hour to 3 hours in 80～85 ℃ of scopes again; In 1 hour, temperature is elevated in 120～125 ℃ of scopes, kept 1 hour to 3 hours; In 1 hour, again temperature is elevated in 155～160 ℃ of scopes, reaction is to transparent; At this moment, reduce the temperature in 130～135 ℃ of scopes, again add main solvent, and the while adds the mixture of encapsulant and catalyzer fast, 100～115 ℃ of insulations 1～1.5 hour, add at last thinner and carry out paint, adjust the solids content 36% to 20% of lacquer;
According to the ratio of quality and the number of copies meter, the consumption of said components is respectively:
Described main solvent is selected: at least a among dimethyl adipate, diethyl malonate or the DBE;
Described isocyanic ester is selected: 4, and 4 '-diphenylmethanediisocyanate (MDI);
Described acid anhydrides is selected: inclined to one side benzoic anhydride;
Described encapsulant is selected: 3,5-xylenol;
Described catalyzer is selected at least a in organo-metallic zinc, isocaprylic acid zinc or the zinc naphthenate;
Described thinner is selected at least a in ester class, lactone, aromatic hydrocarbons, phenols or the propylene carbonate solvent;
Described lactone is selected: butyrolactone;
Described hydro carbons is selected: a kind of in dimethylbenzene or the trimethylbenzene;
Described phenols is selected: cresols.
In technical scheme of the present invention, encapsulant and catalyzer use simultaneously, can guarantee the sealing of encapsulant.The present invention adopts encapsulant to seal unreacted isocyanate groups, both guaranteed that wire enamel had crosslinking activity when enamel-cover, satisfy the requirement of polyamide acid imide enamelled wire, can guarantee again the package stability of wire enamel, the DBE that selects is the product of Dupont, can satisfy performance required for the present invention.
The polyamide-imide enamelled wire varnishes of gained of the present invention does not use N-Methyl pyrrolidone, its performance is identical with common polyamide-imide enamelled wire varnishes, can mix mutually with the wire enamel of other kind again simultaneously, as: polyesterimide wire enamel, polyester wire enamel, polyurethane wire enamel.In coating the enamel-cover production process of enameled wire, reach 1-3 doubly the duration of service that increases the japanning felt, reduced labour intensity and reduced environmental pollution.
Embodiment
The invention will be further described below in conjunction with example, but be not limited to this.
Embodiment 1
In reactor, add 120 gram DBE, start stirring, drop into again the MDI of 160 grams and the inclined to one side benzoic anhydride of 122.9 grams, heating, 80 ℃ were reacted 1 hour, were warmed up to 120 ℃ of reactions 1 hour, be warmed up to 155～160 ℃ of reactions, until transparent, cool to 130 ℃, add 110 gram DBE, the mixture that adds fast 150 gram xylenols and 0.1 gram isocaprylic acid zinc, 115 ℃ of insulations 1.5 hours, add at last 230 gram cresols and 120 gram dimethylbenzene thinners, adjust the solids content about 25% of lacquer.
Embodiment 2
In reactor, add 120 gram diethyl malonates, start stirring, drop into again the MDI of 160 grams and the inclined to one side benzoic anhydride of 122.9 grams, heating, 85 ℃ were reacted 1 hour, be warmed up to 125 ℃ of reactions 1 hour, be warmed up to 160 ℃ of reactions, until transparent, cool to 130 ℃, add 110 gram DBE, add fast the mixture of 150 gram xylenols and 0.1 gram isocaprylic acid zinc, 120 ℃ of insulations 1.5 hours.Add at last 230 gram cresols and 120 gram dimethylbenzene thinners, adjust the solids content about 25% of lacquer.
Embodiment 3
In reactor, add 120 gram butyrolactone, start stirring, drop into again the MDI of 160 grams and the inclined to one side benzoic anhydride of 122.9 grams, heating, 83 ℃ were reacted 1 hour, be warmed up to 122 ℃ of reactions 1 hour, be warmed up to 155～160 ℃ of reactions, until transparent, cool to 130 ℃, add 110 gram DBE, add fast the mixture of 150 gram xylenols and 0.1 gram isocaprylic acid zinc, 118 ℃ of insulations 1.5 hours.Add at last 230 gram cresols and 120 gram dimethylbenzene thinners, adjust the solids content about 25% of lacquer.
Comparative example 1
In reactor, add 277 gram N-Methyl pyrrolidone and the inclined to one side benzoic anhydride of 106.4 grams, be warmed up to 70 ℃, and then drop into 140 MDI that restrain, according to the discharging amount control temperature of carbonic acid gas, after the carbonic acid gas that produces obviously reduces, be warmed up to 85 ℃ of insulations 3 hours, be warmed up to 120 ℃ of insulations after 1.5 hours, afterwards cooling that viscosimetric, viscosity reach 80 seconds, and add 92 gram dimethylbenzene and 20 gram phenylcarbinols, stirred 1 hour at 90～95 ℃.Cooling adds the N-Methyl pyrrolidone of 280 grams and the dimethylbenzene of 130 grams, and the solids content of adjusting lacquer is about 25%.
1. shelf test:
| Test number | Outward appearance | The normal temperature opening is deposited | The normal temperature sealing is deposited |
| Comparative example 1 | The red-brown transparent liquid | Layering appearred in 2 days | Half a year is constant |
| Embodiment 1 | The red-brown transparent liquid | First quarter moon has no layering | Half a year is constant |
| Embodiment 2 | The red-brown transparent liquid | First quarter moon has no layering | Half a year is constant |
| Embodiment 3 | The red-brown transparent liquid | First quarter moon has no layering | Half a year is constant |
Description of test comparative example 1 relatively in being exposed to air easily the moisture absorption separate out resin, when enamel-cover is applied to, be prone in the lacquer cylinder the easily undesired image such as wet of gel, felt.
2. with the solvent compatibility test:
Description of test embodiment can mix with the solvent phase that other wire enamel is commonly used, and uses at enamel-cover to bring convenience, and the work such as cleaning of enamel-cover board bring convenience during the conversion kind.
3. there is polyamide-imide enamelled wire varnishes to be coated with the toe-in fruit
Claims (10)
1. the preparation method of environment-friendly type polyamide-imide enamelled wire varnishes, it is characterized in that: be higher than 150 ℃ of esters solvents as main solvent take boiling point, its preparation method comprises the steps: to add main solvent in reactor, stir, be warmed up to 50～60 ℃ of dissolvings, drop into isocyanic ester and acid anhydrides, the control temperature of reaction kept 1 hour to 3 hours in 80～85 ℃ of scopes again; In 1 hour, temperature is elevated in 120～125 ℃ of scopes, kept 1 hour to 3 hours; In 1 hour, again temperature is elevated in 155～160 ℃ of scopes, reaction is to transparent; At this moment, reduce the temperature in 130～135 ℃ of scopes, again add main solvent, and the while adds the mixture of encapsulant and catalyzer fast, 100～115 ℃ of insulations 1～1.5 hour, add at last thinner and carry out paint, adjust the solids content 36% to 20% of lacquer;
According to the ratio of quality and the number of copies meter, the consumption of said components is respectively:
2. the preparation method of environment-friendly type polyamide-imide enamelled wire varnishes according to claim 1 is characterized in that, described main solvent is selected: at least a among dimethyl adipate, diethyl malonate or the DBE.
3. the preparation method of environment-friendly type polyamide-imide enamelled wire varnishes according to claim 1 is characterized in that, described isocyanic ester is selected: 4, and 4 '-diphenylmethanediisocyanate.
4. the preparation method of environment-friendly type polyamide-imide enamelled wire varnishes according to claim 1 is characterized in that, described acid anhydrides is selected: inclined to one side benzoic anhydride.
5. the preparation method of environment-friendly type polyamide-imide enamelled wire varnishes according to claim 1 is characterized in that, described encapsulant is selected: 3,5-xylenol.
6. the preparation method of environment-friendly type polyamide-imide enamelled wire varnishes according to claim 1 is characterized in that, described catalyzer is selected at least a in organo-metallic zinc, isocaprylic acid zinc or the zinc naphthenate.
7. the preparation method of environment-friendly type polyamide-imide enamelled wire varnishes according to claim 1 is characterized in that, described thinner is selected at least a in ester class, lactone, aromatic hydrocarbons, phenols or the propylene carbonate solvent.
8. the preparation method of environment-friendly type polyamide-imide enamelled wire varnishes according to claim 1 is characterized in that, described lactone is selected: butyrolactone.
9. the preparation method of environment-friendly type polyamide-imide enamelled wire varnishes according to claim 1 is characterized in that, described hydro carbons is selected: a kind of in dimethylbenzene or the trimethylbenzene.
10. the preparation method of environment-friendly type polyamide-imide enamelled wire varnishes according to claim 1 is characterized in that, described phenols is selected: cresols.
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| CN201210418508.4A CN102942815B (en) | 2012-10-26 | 2012-10-26 | Preparation method for environmental protection type polyamide-imide wire enamel |
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| CN201210418508.4A CN102942815B (en) | 2012-10-26 | 2012-10-26 | Preparation method for environmental protection type polyamide-imide wire enamel |
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| CN102942815A true CN102942815A (en) | 2013-02-27 |
| CN102942815B CN102942815B (en) | 2014-07-09 |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110628320A (en) * | 2019-10-30 | 2019-12-31 | 安徽晟然绝缘材料有限公司 | Special polyamideimide enameled wire insulating varnish for small flat wire and preparation method thereof |
| CN110698977A (en) * | 2019-10-30 | 2020-01-17 | 安徽晟然绝缘材料有限公司 | Layered inorganic nano-material modified corona-resistant polyamideimide wire enamel and preparation method thereof |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2008243677A (en) * | 2007-03-28 | 2008-10-09 | Hitachi Chem Co Ltd | Resin composition for electric insulation, and coating and enamel wire using it |
| CN102024937A (en) * | 2009-09-14 | 2011-04-20 | 信越化学工业株式会社 | Negative electrode for nonaqueous electrolyte secondary batteries and lithium ion secondary battery |
-
2012
- 2012-10-26 CN CN201210418508.4A patent/CN102942815B/en active Active
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2008243677A (en) * | 2007-03-28 | 2008-10-09 | Hitachi Chem Co Ltd | Resin composition for electric insulation, and coating and enamel wire using it |
| CN102024937A (en) * | 2009-09-14 | 2011-04-20 | 信越化学工业株式会社 | Negative electrode for nonaqueous electrolyte secondary batteries and lithium ion secondary battery |
Non-Patent Citations (1)
| Title |
|---|
| 刘德辉等: "端基封闭法合成聚酰胺酰亚胺", 《绝缘材料》, no. 1, 28 February 2002 (2002-02-28), pages 9 - 11 * |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110628320A (en) * | 2019-10-30 | 2019-12-31 | 安徽晟然绝缘材料有限公司 | Special polyamideimide enameled wire insulating varnish for small flat wire and preparation method thereof |
| CN110698977A (en) * | 2019-10-30 | 2020-01-17 | 安徽晟然绝缘材料有限公司 | Layered inorganic nano-material modified corona-resistant polyamideimide wire enamel and preparation method thereof |
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| CN102942815B (en) | 2014-07-09 |
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Effective date of registration: 20211110 Address after: 226000 No. 30 Binshui Road, development zone, Nantong City, Jiangsu Province Patentee after: Nantong Bolian Material Technology Co., Ltd Address before: 213033 No. 588, Weitang Street West, Chunjiang Town, Xinbei District, Changzhou City, Jiangsu Province Patentee before: Changzhou Zhitong resin Co., Ltd |