CN102942815B - 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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- CN102942815B CN102942815B CN201210418508.4A CN201210418508A CN102942815B CN 102942815 B CN102942815 B CN 102942815B CN 201210418508 A CN201210418508 A CN 201210418508A CN 102942815 B CN102942815 B CN 102942815B
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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, resistance to refrigerant performance are good etc. outstanding, is widely used in producing the high heat-resisting high performance enameled wire that requires, such as having the composite enameled wire etc. of resistance to refrigerant performance.
But there is again following shortcoming in the polyamide-imide enamelled wire varnishes of producing at present simultaneously, 1) cost is high, because its main solvent N-Methyl pyrrolidone price in wire enamel solvent species used is the highest, as solvent, it is equally also that catalyzed burning converts heat in Production of Enamel Wires process, and after N-Methyl pyrrolidone (NMP) burning, the heat of gained be it would be better cresols (combustion heat: NMP=3010kJ/mol, cresols=3706kJ/mol).2) toxicity is large, and the main solvent N-Methyl pyrrolidone of using in 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) just comprised N-Methyl pyrrolidone (1-methyl-2-pyrrolidone, CAS 872-50-4) in showing great attention to material (REACH).3) deficiency in enamelling technique process, because polyamidoimide paint is taking N-Methyl pyrrolidone as primary solvent, N-Methyl pyrrolidone is intensive polar solvent, the easily moisture absorption, wire enamel is in paint is exposed to air in cylinder and the moisture absorption, particularly under the processing condition of felt japanning, after the moisture absorption, cause resin to be separated out in felt, block flowing of painting in felt, affect the japanning of enameled wire, the felt that will more renew in time like this, often takes two or three days moist day time and changes once, both affect working efficiency, also increased the pollution to environment.4) immiscible with other kind enameled wire, current polyamide-imide enamelled wire varnishes all can not mix mutually with the wire enamel taking cresols as primary solvent such as polyester-imide, after mixing if careless, can muddiness separate out immediately, bring very inconvenient to enamel-cover process, such as, cleaning when enamelling machine conversion production kind is clean especially, can produce so a large amount of cleaning solvents; While producing composite enameled wire, also want SC, pay special attention to finish paint and can not mix with priming paint.
Current 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 environment protection aspect; just must change the main solvent of polyamide-imide enamelled wire varnishes, with other main solvent replacement N-Methyl pyrrolidone.
Summary of the invention
The invention provides a kind of preparation method who does not prepare polyamide-imide enamelled wire varnishes taking 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, taking boiling point higher than 150 DEG C of esters solvents as main solvent, its preparation method comprises the steps: to add main solvent in reactor, stir, be warmed up to 50～60 DEG C of dissolvings, drop into again isocyanic ester and acid anhydrides, control temperature of reaction within the scope of 80～85 DEG C, keep 1 hour to 3 hours; In 1 hour, temperature is elevated within the scope of 120～125 DEG C, keep 1 hour to 3 hours; In 1 hour, then temperature is elevated within the scope of 155～160 DEG C, reaction is to transparent; Now, reduce the temperature within the scope of 130～135 DEG C, again add main solvent, and the while adds the mixture of encapsulant and catalyzer fast, 100～115 DEG C of insulations 1～1.5 hour, finally add thinner to carry out paint, adjust the solids content 36% to 20% of paint;
According to ratio of quality and the number of copies meter, the consumption of said components respectively:
Described main solvent is selected: at least one in dimethyl adipate, diethyl malonate or DBE;
Described isocyanic ester is selected: 4, and 4 '-diphenylmethanediisocyanate (MDI);
Described acid anhydrides is selected: benzoic anhydride partially;
Described encapsulant is selected: 3,5-xylenol;
Described catalyzer is selected at least one in organo-metallic zinc, isocaprylic acid zinc or zinc naphthenate;
Described thinner is selected at least one in ester class, lactone, aromatic hydrocarbons, phenols or propylene carbonate solvent;
Described lactone is selected: butyrolactone;
Described hydro carbons is selected: the one in dimethylbenzene or trimethylbenzene;
Described phenols is selected: cresols.
In technical scheme of the present invention, encapsulant and catalyzer use simultaneously, can ensure the sealing of encapsulant.The present invention adopts encapsulant to seal unreacted isocyanate groups, both ensured that wire enamel had crosslinking activity in the time of enamel-cover, meet the requirement of polyamide acid imide enamelled wire, can ensure again the package stability of wire enamel, the DBE selecting is the product of Dupont, can meet 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 the enamel-cover production process that coats enameled wire, reach 1-3 doubly the duration of service that increases japanning felt, reduced labour intensity and reduced environmental pollution.
Embodiment
Below in conjunction with example, the invention will be further described, but be not limited to this.
Embodiment 1
In reactor, add 120 grams of DBE, start stirring, then drop into the MDI of 160 grams and the inclined to one side benzoic anhydride of 122.9 grams, heating, 80 DEG C are reacted 1 hour, are warmed up to 120 DEG C of reactions 1 hour, be warmed up to 155～160 DEG C of reactions, until transparent, cool to 130 DEG C, add 110 grams of DBE, add fast the mixture of 150 grams of xylenols and 0.1 gram of isocaprylic acid zinc, 115 DEG C of insulations 1.5 hours, finally add 230 grams of cresols and 120 grams of dimethylbenzene thinners, adjust solids content 25% left and right of paint.
Embodiment 2
In reactor, add 120 grams of diethyl malonates, start stirring, then drop into the MDI of 160 grams and the inclined to one side benzoic anhydride of 122.9 grams, heating, 85 DEG C are reacted 1 hour, be warmed up to 125 DEG C of reactions 1 hour, be warmed up to 160 DEG C of reactions, until transparent, cool to 130 DEG C, add 110 grams of DBE, add fast the mixture of 150 grams of xylenols and 0.1 gram of isocaprylic acid zinc, 120 DEG C of insulations 1.5 hours.Finally add 230 grams of cresols and 120 grams of dimethylbenzene thinners, adjust solids content 25% left and right of paint.
Embodiment 3
In reactor, add 120 grams of butyrolactone, start stirring, then drop into the MDI of 160 grams and the inclined to one side benzoic anhydride of 122.9 grams, heating, 83 DEG C are reacted 1 hour, be warmed up to 122 DEG C of reactions 1 hour, be warmed up to 155～160 DEG C of reactions, until transparent, cool to 130 DEG C, add 110 grams of DBE, add fast the mixture of 150 grams of xylenols and 0.1 gram of isocaprylic acid zinc, 118 DEG C of insulations 1.5 hours.Finally add 230 grams of cresols and 120 grams of dimethylbenzene thinners, adjust solids content 25% left and right of paint.
Comparative example 1
In reactor, add 277 grams of N-Methyl pyrrolidone and 106.4 grams of inclined to one side benzoic anhydrides, be warmed up to 70 DEG C, and then drop into the MDI of 140 grams, according to the discharging amount control temperature of carbonic acid gas, after the carbonic acid gas producing obviously reduces, be warmed up to 85 DEG C of insulations 3 hours, be warmed up to 120 DEG C of insulations after 1.5 hours, viscosimetric, viscosity is cooling after reaching 80 seconds, and add 92 grams of dimethylbenzene and 20 grams of phenylcarbinols, stir 1 hour at 90～95 DEG C.Cooling, add the N-Methyl pyrrolidone of 280 grams and the dimethylbenzene of 130 grams, the solids content of adjusting paint is 25% left and right.
1. shelf test:
| Test number | Outward appearance | Normal temperature opening is deposited | Normal temperature sealing is deposited |
| Comparative example 1 | Red-brown transparent liquid | Within 2 days, there is layering | Half a year is constant |
| Embodiment 1 | Red-brown transparent liquid | First quarter moon has no layering | Half a year is constant |
| Embodiment 2 | Red-brown transparent liquid | First quarter moon has no layering | Half a year is constant |
| Embodiment 3 | Red-brown transparent liquid | First quarter moon has no layering | Half a year is constant |
Description of test comparative example 1 is separated out resin being exposed in air the easily moisture absorption relatively, is prone in paint cylinder the easily undesired image such as wet of gel, felt in the time that enamel-cover is applied to.
2. with solvent compatibility test:
Description of test embodiment all can be conventional with other wire enamel solvent phase mix, in enamel-cover application, bring convenience, when conversion kind, the work such as the cleaning of enamel-cover board brings convenience.
3. there is polyamide-imide enamelled wire varnishes to be coated with toe-in fruit
Claims (7)
1. the preparation method of environment-friendly type polyamide-imide enamelled wire varnishes, it is characterized in that: taking boiling point higher than 150 DEG C of esters solvents as main solvent, described main solvent is selected: at least one in dimethyl adipate, diethyl malonate or DBE, its preparation method comprises the steps: to add main solvent in reactor, stir, be warmed up to 50～60 DEG C of dissolvings, drop into again 4,4 '-diphenylmethanediisocyanate and partially benzoic anhydride, control temperature of reaction within the scope of 80～85 DEG C, keep 1 hour to 3 hours; In 1 hour, temperature is elevated within the scope of 120～125 DEG C, keep 1 hour to 3 hours; In 1 hour, then temperature is elevated within the scope of 155～160 DEG C, reaction is to transparent; Now, reduce the temperature within the scope of 130～135 DEG C, again add main solvent, and the while adds the mixture of encapsulant and catalyzer fast, 100～115 DEG C of insulations 1～1.5 hour, finally add thinner to carry out paint, adjust the solids content 36% to 20% of paint;
According to ratio of quality and the number of copies meter, the consumption of said components respectively:
2. 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.
3. 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 one in organo-metallic zinc, isocaprylic acid zinc or zinc naphthenate.
4. 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 one in ester class, lactone, aromatic hydrocarbons, phenols or propylene carbonate solvent.
5. the preparation method of environment-friendly type polyamide-imide enamelled wire varnishes according to claim 4, is characterized in that, described lactone is selected: butyrolactone.
6. the preparation method of environment-friendly type polyamide-imide enamelled wire varnishes according to claim 4, is characterized in that, described aromatic hydrocarbons is selected: the one in dimethylbenzene or trimethylbenzene.
7. the preparation method of environment-friendly type polyamide-imide enamelled wire varnishes according to claim 4, 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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| CN102942815B true CN102942815B (en) | 2014-07-09 |
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| 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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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 |