CN110724400A - Low-volatility polyesterimide impregnating resin wire enamel and preparation method thereof - Google Patents
Low-volatility polyesterimide impregnating resin wire enamel and preparation method thereof Download PDFInfo
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- CN110724400A CN110724400A CN201911162222.2A CN201911162222A CN110724400A CN 110724400 A CN110724400 A CN 110724400A CN 201911162222 A CN201911162222 A CN 201911162222A CN 110724400 A CN110724400 A CN 110724400A
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- volatility
- wire enamel
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09D—COATING 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
- C09D4/00—Coating compositions, e.g. paints, varnishes or lacquers, based on organic non-macromolecular compounds having at least one polymerisable carbon-to-carbon unsaturated bond ; Coating compositions, based on monomers of macromolecular compounds of groups C09D183/00 - C09D183/16
- C09D4/06—Organic non-macromolecular compounds having at least one polymerisable carbon-to-carbon unsaturated bond in combination with a macromolecular compound other than an unsaturated polymer of groups C09D159/00 - C09D187/00
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- 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
Abstract
The invention relates to the field of wire enamel preparation, and particularly discloses a low-volatility polyesterimide impregnating resin wire enamel and a preparation method thereof. The preparation method is simple, and the prepared wire enamel has the advantages of stable storage, short gelation time, low volatilization, low toxicity and environmental friendliness, reduces the discharge amount of VOC (volatile organic compounds) and has less harm to human bodies.
Description
Technical Field
The invention relates to the field of wire enamel preparation, in particular to low-volatility polyesterimide impregnating resin wire enamel and a preparation method thereof.
Background
Environmental protection and energy conservation are important subjects of current socioeconomic development, and the nation has made definite strategic deployment aiming at the two aspects and implemented an industrial strategic development plan. According to the national industrial policy, one of the key points of the future development of the insulating material industry is to adjust the product structure and research and develop an environment-friendly and energy-saving insulating material; the development of a large amount of environment-friendly low-carbon type insulating materials with wide range is prioritized, such as the development of solvent-free insulating paint, water-based insulating paint and powder coating, and the development of low-grade solvent paint and high-toxicity solvent paint is limited, so the development of pollution-free and less-pollution products is the requirement of enterprise development under the current economy.
The insulating impregnating resin is a liquid resin system, and because the low-volatility solvent-free impregnating resin has good manufacturability (good stability and quick solidification), obvious environmental protection characteristic and production and transportation safety, the demand of a plurality of industries (such as automobile motors, wind driven generators and the like) on the market at present is more and more large, and the insulating impregnating resin is emphasized and applied in large quantity at home and abroad.
Most of the insulating impregnating varnish in the styrene system is applied in the market at the present stage, but styrene has low boiling point, is volatile, has an irritation effect on skin and respiratory tract, is not easy to decompose and excrete after entering a human body, has a certain accumulative effect, has high VOC discharge amount in the using process, and has certain harm to the environment and personnel.
Disclosure of Invention
The invention aims to provide the low-volatility polyesterimide impregnated resin wire enamel and the preparation method thereof, so that the prepared wire enamel has the advantages of stable storage, short gelling time, low volatility, low toxicity and environmental friendliness, reduces the discharge amount of VOC (volatile organic compounds) and has less harm to human bodies.
In order to solve the problems, the invention is realized by the following technical scheme:
on one hand, the invention provides a low-volatility polyesterimide impregnating resin wire enamel, which comprises the following raw materials in mass: 8.5-12 parts of tetrahydrophthalic anhydride, 0.5-1.0 part of trimellitic anhydride, 2.0-3.0 parts of dimethylbenzene, 4.0-5.5 parts of monoethanolamine, 5.0-6.5 parts of tetrahydrophthalic anhydride, 1.0-2.0 parts of castor oil, 0.5-1.5 parts of trimethylolpropane, 2.0-3.5 parts of neopentyl glycol, 0.01-0.03 part of zinc acetate, 7.0-10.05 parts of acrylate diluent, 0.01-0.03 part of benzoquinone solution, 1.0-2.5 parts of acrylate diluent and 0.15-0.40 part of curing agent.
On the other hand, the invention provides a preparation method of the low-volatility polyesterimide impregnating resin wire enamel, which comprises the following steps:
s1, cleaning a reaction kettle in advance, and introducing nitrogen into the reaction kettle for protection;
s2, adding tetrahydrophthalic anhydride, trimellitic anhydride and xylene in a reaction kettle under a stirring state, and dropwise adding monoethanolamine in three batches;
s3, after the three batches of monoethanolamine are added, heating the reaction kettle to 160 ℃ for 150-;
s4, after the acid value is qualified, reducing the temperature of the reaction kettle to 60-70 ℃, quickly adding tetrahydrophthalic anhydride, castor oil, trimethylolpropane, neopentyl glycol and zinc acetate, and then heating the reaction kettle to 180-200 ℃;
s5, preserving heat for 3 hours when the temperature of the kettle rises to 200 ℃, measuring the water yield at intervals, sampling to measure the acid value of the reaction liquid when the water yield reaches about 80% of a theoretical value, and vacuumizing to completely pump out the dimethylbenzene as a water-carrying agent after the acid value is qualified;
s6, reducing the temperature of the kettle to 90-105 ℃, and adding an acrylate diluent and a benzoquinone solution into the reaction kettle to prepare unsaturated polyester-imide resin;
s7, adding an acrylate diluent and a curing agent into the S6, and adjusting the viscosity and the gel time of the paint to finally obtain the polyester-imide impregnated resin finished paint.
Further, the temperature of the reaction kettle in the S1 is lower than 120 ℃;
further, during the temperature rise of the reactor in S3 to 150 ℃ and 160 ℃, the temperature rise rate is maintained at 10-12 ℃/h.
Further, the theoretical value in S3 is a value of 1.9% of the total amount of the fed water.
Further, the acid value in S4 is qualified when the acid value is 38-43 mgKOH/g.
Further, during the temperature rise of the reactor in S4 to 180-200 ℃, the temperature rise rate is maintained at 10-15 ℃/h.
Further, the theoretical value in S5 is a value of 5.5% of the total input amount of the water yield, and the acid value in S5 is qualified at 10-30 mgKOH/g.
Further, the viscosity standard of the paint in S7 is adjusted to be 1200-1500mpa.s, and the gel time standard is 8-15 min.
The invention has the following beneficial effects:
1. the high-flash-point acrylate diluent is selected to replace styrene, and then the curing agent is added, so that the prepared polyester-imide impregnated resin paint has low volatility, low toxicity and environmental protection, reduces VOC (volatile organic compound) emission and has less harm to human bodies.
2. The invention well solves the problem of complete reaction by designing and improving the process; and the low-volatile and low-toxicity diluent is combined to develop the low-VOC-emission polyesterimide low-solvent impregnating resin. Therefore, the products have good market space and development prospect, and also favorably support the development of the electronic transformer industry in China.
Detailed Description
The following description will be given with reference to specific examples, and all other examples obtained by those skilled in the art without any inventive step will fall within the scope of the present invention.
Example 1:
the raw materials are calculated according to the following mass: 8.5-12 parts of tetrahydrophthalic anhydride, 0.5-1.0 part of trimellitic anhydride, 2.0-3.0 parts of dimethylbenzene, 4.0-5.5 parts of monoethanolamine, 5.0-6.5 parts of tetrahydrophthalic anhydride, 1.0-2.0 parts of castor oil, 0.5-1.5 parts of trimethylolpropane, 2.0-3.5 parts of neopentyl glycol, 0.01-0.03 part of zinc acetate, 7.0-10.05 parts of acrylate diluent, 0.01-0.03 part of benzoquinone solution, 1.0-2.5 parts of acrylate diluent and 0.15-0.40 part of curing agent.
The preparation method of the low-volatility polyesterimide impregnating resin wire enamel comprises the following steps:
1. raw material preparation (by mass)
a. Cleaning a 20L reaction kettle in advance and introducing nitrogen for protection;
b. sequentially adding dimethylbenzene, tetrahydrophthalic anhydride and trimellitic anhydride into a reaction kettle under a stirring state, dropwise adding ethanolamine in three batches, automatically heating the kettle to about 110 ℃ in the dropwise adding process, and then heating to 155 ℃ at the speed of 10 ℃/h. During the period, when the temperature of the kettle reaches 130 ℃, the water separator begins to have a layering phenomenon, and when the water yield reaches about 230g, a sample is taken to determine that the acid value is 41.57 mgKOH/g;
c. after the acid value is qualified, well recording the water yield, reducing the kettle temperature to 70 ℃, adding tetrahydrophthalic anhydride, castor oil, neopentyl glycol, trimethylolpropane and zinc acetate, and heating to 200 ℃ at the speed of 15 ℃/h. During the period, when the temperature of the kettle reaches 160 ℃, the layering phenomenon begins to occur in the water separator;
d. when the temperature of the kettle rises to 200 ℃, preserving the heat for 3 hours, measuring the water yield at intervals, and when the water yield reaches about 650g, sampling to measure that the acid value is 34.9mgKOH/g, wherein the acid value does not meet the requirement;
e. the reaction kettle is kept at the temperature of 200 ℃, and after 30min, a sample is taken to determine that the acid value is 27.63mgKOH/g, and the acid value meets the requirement;
f. vacuumizing to completely pump out the dimethylbenzene as a water-carrying agent, and sampling to determine that the acid value is 25.49mgKOH/g and the viscosity is 535 mpa.s;
g. reducing the temperature of the kettle to 100 ℃, and then adding an acrylate diluent and a benzoquinone solution to prepare unsaturated polyester-imide resin;
h. and adding an acrylate diluent and a curing agent into the resin for paint mixing to finally prepare the polyester-imide impregnated resin finished paint, wherein the viscosity is 1370mpa.s, and the gel time is 14min11 s.
The above disclosure is only one preferred embodiment of the present invention, and certainly should not be construed as limiting the scope of the invention, which is defined by the claims and their equivalents.
Claims (10)
1. The low-volatility polyesterimide impregnating resin wire enamel is characterized by comprising the following raw materials in mass: 8.5-12 parts of tetrahydrophthalic anhydride, 0.5-1.0 part of trimellitic anhydride, 2.0-3.0 parts of dimethylbenzene, 4.0-5.5 parts of monoethanolamine, 5.0-6.5 parts of tetrahydrophthalic anhydride, 1.0-2.0 parts of castor oil, 0.5-1.5 parts of trimethylolpropane, 2.0-3.5 parts of neopentyl glycol, 0.01-0.03 part of zinc acetate, 7.0-10.05 parts of acrylate diluent, 0.01-0.03 part of benzoquinone solution, 1.0-2.5 parts of acrylate diluent and 0.15-0.40 part of curing agent.
2. A method for preparing a low volatile polyester imide impregnated resin wire enamel for making the low volatile polyester imide impregnated resin wire enamel of claim 1, comprising the steps of:
s1, cleaning a reaction kettle in advance, and introducing nitrogen into the reaction kettle for protection;
s2, adding tetrahydrophthalic anhydride, trimellitic anhydride and xylene in a reaction kettle under a stirring state, and dropwise adding monoethanolamine in three batches;
s3, after the three batches of monoethanolamine are added, heating the reaction kettle to 160 ℃ for 150-;
s4, after the acid value is qualified, reducing the temperature of the reaction kettle to 60-70 ℃, adding tetrahydrophthalic anhydride, castor oil, trimethylolpropane, neopentyl glycol and zinc acetate, and then heating the reaction kettle to 180-200 ℃;
s5, preserving heat for 3 hours when the temperature of the kettle rises to 200 ℃, measuring the water yield, sampling and measuring the acid value of the reaction liquid when the water yield reaches about 80% of a theoretical value, and vacuumizing to completely pump out the dimethylbenzene as a water-carrying agent after the acid value is qualified;
s6, reducing the temperature of the kettle to 90-105 ℃, and adding an acrylate diluent and a benzoquinone solution into the reaction kettle to prepare unsaturated polyester-imide resin;
and S7, adding an acrylate diluent and a curing agent into the unsaturated polyester-imide resin obtained in the step S6, and adjusting the viscosity and the gel time of the paint to finally obtain the polyester-imide impregnated resin finished paint.
3. The method for preparing low-volatility polyesterimide impregnated resin wire enamel according to claim 2, wherein the temperature of the reaction kettle in S1 is lower than 120 ℃.
4. The method for preparing low-volatility polyesterimide impregnating resin wire enamel according to claim 2, wherein the temperature rising rate is maintained at 10-12 ℃/h during the pot temperature rising in S3 to 150-160 ℃.
5. The method for preparing low-volatility polyesterimide impregnated resin wire enamel according to claim 2, wherein the theoretical value in S3 is the value of water yield accounting for 1.9% of total input amount.
6. The method for preparing low-volatility polyesterimide impregnating resin wire enamel according to claim 2, wherein said acid value in S4 is 38-43 mgKOH/g.
7. The method for preparing low-volatility polyesterimide impregnating resin wire enamel according to claim 2, wherein the temperature rising rate is maintained at 10-15 ℃/h during the pot temperature rising in S4 to 180-200 ℃.
8. The method for preparing low-volatility polyesterimide impregnated resin wire enamel according to claim 2, wherein the theoretical value in S5 is the value of 5.5% of the water yield in the total input amount.
9. The method for preparing low-volatility polyesterimide impregnating resin wire enamel according to claim 2, wherein said acid value of S5 is 10-30 mgKOH/g.
10. The method for preparing low-volatility polyesterimide impregnating resin wire enamel according to claim 2, wherein the viscosity standard of said enamel in S7 is 1200-1500mpa.s, and the gel time standard is 8-15 min.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201911162222.2A CN110724400A (en) | 2019-11-25 | 2019-11-25 | Low-volatility polyesterimide impregnating resin wire enamel and preparation method thereof |
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| CN201911162222.2A CN110724400A (en) | 2019-11-25 | 2019-11-25 | Low-volatility polyesterimide impregnating resin wire enamel and preparation method thereof |
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Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101514276A (en) * | 2008-12-30 | 2009-08-26 | 上海新天和树脂有限公司 | Method for preparing solventless unsaturated polyester-imide wire coating enamel |
| CN102604384A (en) * | 2012-02-29 | 2012-07-25 | 苏州巨峰电气绝缘系统股份有限公司 | Universal refrigerant resistant solvent-free impregnating resin for high and low voltage motor and preparation method thereof |
| CN105295041A (en) * | 2015-12-03 | 2016-02-03 | 苏州太湖电工新材料股份有限公司 | Polyoxazolidone resin, preparation method of polyoxazolidone resin and application of polyoxazolidone resin in dip varnish |
| CN108102367A (en) * | 2018-01-15 | 2018-06-01 | 苏州巨峰电气绝缘系统股份有限公司 | A kind of high heat conduction environment-friendly type polyester imines trickle resin and its preparation method and application |
| CN109735142A (en) * | 2018-12-12 | 2019-05-10 | 苏州太湖电工新材料股份有限公司 | A kind of environment-friendly type insulated impregnating varnish and its preparation method and application |
-
2019
- 2019-11-25 CN CN201911162222.2A patent/CN110724400A/en active Pending
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101514276A (en) * | 2008-12-30 | 2009-08-26 | 上海新天和树脂有限公司 | Method for preparing solventless unsaturated polyester-imide wire coating enamel |
| CN102604384A (en) * | 2012-02-29 | 2012-07-25 | 苏州巨峰电气绝缘系统股份有限公司 | Universal refrigerant resistant solvent-free impregnating resin for high and low voltage motor and preparation method thereof |
| CN105295041A (en) * | 2015-12-03 | 2016-02-03 | 苏州太湖电工新材料股份有限公司 | Polyoxazolidone resin, preparation method of polyoxazolidone resin and application of polyoxazolidone resin in dip varnish |
| CN108102367A (en) * | 2018-01-15 | 2018-06-01 | 苏州巨峰电气绝缘系统股份有限公司 | A kind of high heat conduction environment-friendly type polyester imines trickle resin and its preparation method and application |
| CN109735142A (en) * | 2018-12-12 | 2019-05-10 | 苏州太湖电工新材料股份有限公司 | A kind of environment-friendly type insulated impregnating varnish and its preparation method and application |
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