CN115594802A - Unsaturated polyester insulating resin and preparation method thereof - Google Patents
Unsaturated polyester insulating resin and preparation method thereof Download PDFInfo
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- CN115594802A CN115594802A CN202211368705.XA CN202211368705A CN115594802A CN 115594802 A CN115594802 A CN 115594802A CN 202211368705 A CN202211368705 A CN 202211368705A CN 115594802 A CN115594802 A CN 115594802A
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- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F283/00—Macromolecular compounds obtained by polymerising monomers on to polymers provided for in subclass C08G
- C08F283/01—Macromolecular compounds obtained by polymerising monomers on to polymers provided for in subclass C08G on to unsaturated polyesters
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Abstract
The invention discloses an unsaturated polyester insulating resin, which consists of 49-62 percent of unsaturated polyester solid resin, 36-49 percent of acrylate reactive diluent, 1-2 percent of peroxide thermal initiator and 0.01-0.03 percent of free radical polymerization inhibitor; the preparation method comprises the steps of preheating unsaturated polyester solid resin to 90-110 ℃, weighing and pouring the unsaturated polyester solid resin into a beaker, adding an acrylate reactive diluent and a free radical polymerization inhibitor, stirring the unsaturated polyester solid resin at a high speed for 0.5-1 hour when the unsaturated polyester solid resin is hot, uniformly stirring the unsaturated polyester solid resin and cooling the unsaturated polyester solid resin to 30-40 ℃, adding a peroxide thermal initiator, and uniformly stirring and mixing the unsaturated polyester insulating resin to obtain the low-volatility and low-shrinkage unsaturated polyester insulating resin which has the advantages of low curing volatile content, low curing shrinkage, high heat resistance, good cold and heat shock resistance, good storage stability, excellent electrical insulating property, convenience in use and the like, and can be used for the impregnation and insulation treatment of coil windings and iron cores of various motor and electrical appliance parts.
Description
Technical Field
The invention belongs to the technical field of insulating impregnating resin, and particularly relates to low-volatility and low-shrinkage unsaturated polyester insulating resin and a preparation method thereof.
Background
The insulating impregnating resin is one of three main insulating materials for electrical product winding insulation, and is permeated and filled into gaps and air holes of a coil, a wire slot or other insulators through an impregnating procedure, then the coil wires are bonded into an insulating whole through curing, and a continuous insulating layer is formed on the surface of the insulating whole, so that the dielectric property, the mechanical property, the heat conducting property and the protective property of an insulating structure can be improved. Therefore, the quality of the insulating impregnating resin directly determines the service life of the electrical equipment.
There are two main types of insulation impregnating resins currently in use, one being epoxy insulation resin and the other being unsaturated polyester insulation resin. Among them, unsaturated polyester insulating resin is widely used for the impregnation and insulation treatment of coil windings and iron cores of various types of electric and mechanical parts due to its characteristics of short curing time, high heat resistance, good storage stability, excellent electrical insulating property, single-component packaging, convenient use and the like.
However, in terms of cost, most of the conventional unsaturated polyester insulating resins commonly used at present are styrene or vinyl toluene with low boiling point, high saturated vapor pressure, low flash point and large curing shrinkage, so that the conventional unsaturated polyester insulating resins prepared from the conventional unsaturated polyester insulating resins have the defects of large smell, high curing volatile content, large curing shrinkage, large brittleness and easy cracking of cured products (particularly thick-layer curing or coating metal curing), poor cold and heat shock resistance and the like, and the use of the conventional unsaturated polyester insulating resins in the insulating treatment field (such as high-voltage motors, new energy automobile driving motors and the like) with low emission of organic volatile components, thick cured paint film requirements or high cold and heat shock resistance requirements is limited.
Therefore, it is required to develop a novel unsaturated polyester insulating resin with low volatility, low shrinkage, safety and environmental protection.
Disclosure of Invention
The invention aims to overcome the technical defects, provides the unsaturated polyester insulating resin with low volatilization and low shrinkage, and solves the technical problems of large smell, high curing volatile component, large curing shrinkage, large brittleness and easy cracking of a cured product and poor cold and heat shock resistance of the traditional unsaturated polyester insulating resin at present.
The technical scheme adopted by the invention for solving the technical problems is as follows: the unsaturated polyester insulating resin consists of unsaturated polyester solid resin 49-62 wt%, acrylate reactive diluent 36-49 wt%, peroxide as thermal initiator 1-2 wt% and free radical polymerization inhibitor 0.01-0.03 wt%.
The unsaturated polyester solid resin is unsaturated polyester resin with an acid value of 30-35 mgKOH/g and a melting point of 40-60 ℃.
The acrylate reactive diluent is one or a mixture of two of cyclohexyl methacrylate, isobornyl methacrylate, dicyclopentadiene methacrylate, tricyclodecane dimethanol dimethacrylate and propylene oxide neopentyl glycol dimethacrylate (NPG 2 PODMA) with high boiling point, low saturated vapor pressure and low curing shrinkage.
Further, the peroxide thermal initiator is one or a mixture of two of tert-butyl peroxybenzoate and dicumyl peroxide.
Further, the free radical polymerization inhibitor is one or a mixture of two of p-methoxyphenol, hydroquinone, p-tert-butylcatechol and 2,5-di-tert-butylhydroquinone.
Another aspect of the present invention is to provide a method for preparing a low-volatility, low-shrinkage unsaturated polyester insulating resin, comprising the steps of:
(1) Preheating 200-240 g of unsaturated polyester solid resin to 90-110 ℃ in advance, preserving heat for 2-4 h, weighing and pouring into a beaker after the unsaturated polyester solid resin is completely melted;
(2) Then 160-200 g of acrylate active diluent and 0.08-0.09 g of free radical polymerization inhibitor are added, and the mixture is stirred at high speed for 0.5-1 hour when the mixture is hot;
(3) Stirring and mixing evenly, cooling to 30-40 ℃, adding 4-6 g of peroxide thermal initiator, stirring for 0.5-2 h, mixing evenly, and cooling to room temperature to obtain the low-volatility and low-shrinkage unsaturated polyester insulating resin.
Compared with the prior art, the invention has the beneficial effects that:
the acid value requirement of the unsaturated polyester solid resin selected in the invention is lower (30-35 mgKOH/g), thus ensuring higher esterification reaction degree and higher molecular weight, and further ensuring that the unsaturated polyester insulating resin prepared by the unsaturated polyester solid resin has better mechanical properties (such as bonding strength) and high-temperature dielectric loss after being cured; in addition, the melting point of the unsaturated polyester insulating resin is required to be lower (40-60 ℃), which is beneficial to rapid melting and liquefaction at a lower preheating temperature (90-110 ℃), so that the unsaturated polyester insulating resin is easy to dissolve in the reactive diluent (the dissolving temperature is reduced, the stirring and dissolving time is shortened, the solubility is increased or the solution viscosity is reduced), the consumption of the reactive diluent can be reduced, the curing volatile and the curing shrinkage rate of the unsaturated polyester insulating resin can be reduced to a certain extent, and the brittleness of a cured product is improved.
2, the invention uses the acrylate reactive diluent with low odor, high boiling point, low saturated vapor pressure and low curing shrinkage to replace the prior common styrene or vinyl toluene with large odor, low boiling point, high saturated vapor pressure, low flash point and large curing shrinkage, solves the problems of large odor, flammability and explosiveness, high curing volatile component, large curing shrinkage, large brittleness and easy cracking of a cured product, poor cold and heat shock resistance and the like of the traditional unsaturated polyester insulating resin, and can prepare the novel unsaturated polyester insulating resin with safety, environmental protection, low volatilization, low shrinkage, difficult cracking of the cured product and good cold and heat shock resistance.
3, the curing rate (such as gel time) of the unsaturated polyester insulating resin is properly delayed by controlling the type or the adding proportion of the free radical initiator, so that the phenomenon that the final cured product is fragile and easy to crack because the curing shrinkage stress is not released in time when the curing rate of the insulating resin is too high (the gel time is too short) is prevented.
The low-volatility and low-shrinkage unsaturated polyester insulating resin prepared by the invention has the advantages of safety, environmental protection, low curing volatile component, low curing shrinkage, good toughness of a cured product, high heat resistance temperature, good cold and heat shock resistance, excellent electrical insulating property and the like, can be applied to the dipping insulation treatment of coil windings and iron cores of various motor electrical parts, and is particularly suitable for the field of large high-voltage motors and new energy automobile driving motors which have low curing volatile component and thick curing paint film requirements or have high cold and heat shock resistance requirements.
Detailed Description
The invention provides a low-volatility and low-shrinkage unsaturated polyester insulating resin, which comprises, by weight, 49-62% of unsaturated polyester solid resin, 36-49% of acrylate reactive diluent, 1-2% of peroxide thermal initiator and 0.01-0.03% of free radical polymerization inhibitor.
Wherein the unsaturated polyester solid resin is unsaturated polyester resin with an acid value of 30-35 mgKOH/g and a melting point of 40-60 ℃.
Wherein the acrylate reactive diluent is one or two of cyclohexyl methacrylate, isobornyl methacrylate, dicyclopentadiene methacrylate, tricyclodecane dimethanol dimethacrylate and propoxylated neopentyl glycol dimethacrylate (NPG 2 PODMA) with high boiling point, low saturated vapor pressure and low curing shrinkage
Wherein the peroxide thermal initiator is one or a mixture of tert-butyl peroxybenzoate and dicumyl peroxide.
Wherein the free radical polymerization inhibitor is one or a mixture of two of p-methoxyphenol, hydroquinone, p-tert-butylcatechol and 2,5-di-tert-butylhydroquinone.
In order to make the objects, technical solutions and advantages of the present invention more clearly understood, the following will explain in detail the preparation method of the low-volatility and low-shrinkage unsaturated polyester insulating resin provided by the present invention with reference to the following examples. The experimental procedures in the following examples are conventional unless otherwise specified. It should be understood that the specific embodiments described herein are merely illustrative of the invention and are not intended to limit the invention.
The experimental materials used in the present invention were all purchased from the market unless otherwise specified.
Example 1
Embodiment 1 of the present invention provides a method for preparing low-volatility and low-shrinkage unsaturated polyester insulating resin, comprising the steps of: firstly, preheating unsaturated polyester solid resin with the acid value of 30-35 mgKOH/g and the melting point of 40-60 ℃ to 90-110 ℃, preserving heat for 2-4 h, and pouring 240g of melting liquid into a beaker after the unsaturated polyester solid resin is completely melted; then 160g of cyclohexyl methacrylate and 0.09g of p-methoxyphenol are added, and the mixture is stirred at high speed for 0.5 to 1 hour when the mixture is hot; stirring and mixing evenly, cooling to 30-40 ℃, adding 4g of tert-butyl peroxybenzoate, stirring for 0.5-1 h, and cooling to room temperature to obtain the finished product of the low-volatility and low-shrinkage unsaturated polyester insulating resin.
Example 2
Embodiment 2 of the present invention provides a method for preparing low-volatility and low-shrinkage unsaturated polyester insulating resin, comprising the steps of: firstly, preheating unsaturated polyester solid resin with the acid value of 30-35 mgKOH/g and the melting point of 40-60 ℃ to 90-110 ℃, preserving heat for 2-4 h, and pouring 215g of melting liquid into a beaker after the unsaturated polyester solid resin is completely melted; then 185g of isobornyl methacrylate and 0.08g of hydroquinone are added, and the mixture is stirred at high speed for 0.5 to 1 hour when the mixture is hot; stirring and mixing evenly, cooling to 30-40 ℃, adding 6g of dicumyl peroxide, stirring for 1-2 h, and cooling to room temperature to obtain the finished product of the low-volatility and low-shrinkage unsaturated polyester insulating resin.
Example 3
Embodiment 3 of the present invention provides a method for preparing low-volatility and low-shrinkage unsaturated polyester insulating resin, comprising the steps of: firstly, preheating unsaturated polyester solid resin with the acid value of 30-35 mgKOH/g and the melting point of 40-60 ℃ to 90-110 ℃, preserving heat for 2-4 h, and pouring 213g of melting liquid into a beaker after the unsaturated polyester solid resin is completely melted; then 187g of dicyclopentadiene methacrylate and 0.09g of p-tert-butyl catechol are added, and the mixture is stirred at high speed for 0.5 to 1 hour when the mixture is hot; stirring and mixing evenly, cooling to 30-40 ℃, adding 6g of dicumyl peroxide, stirring for 0.5-1 h, and cooling to room temperature to obtain the finished product of the low-volatility and low-shrinkage unsaturated polyester insulating resin.
Example 4
Embodiment 4 of the present invention provides a method for preparing low-volatility and low-shrinkage unsaturated polyester insulating resin, comprising the steps of: firstly, preheating unsaturated polyester solid resin with an acid value of 30-35 mgKOH/g and a melting point of 40-60 ℃ to 90-110 ℃, preserving heat for 2-4 h, and pouring 210g of melting liquid into a beaker after the unsaturated polyester solid resin is completely melted; then 190g of tricyclodecane dimethanol dimethacrylate and 0.09g of 2, 5-di-tert-butyl hydroquinone are added and stirred at high speed for 0.5 to 1 hour when the mixture is hot; stirring and mixing evenly, cooling to 30-40 ℃, adding 6g of dicumyl peroxide, stirring for 0.5-1 h, and cooling to room temperature to obtain the finished product of the low-volatility and low-shrinkage unsaturated polyester insulating resin.
Example 5
Embodiment 5 of the present invention provides a method for preparing a low-volatility and low-shrinkage unsaturated polyester insulating resin, comprising the steps of: firstly, preheating unsaturated polyester solid resin with the acid value of 30-35 mgKOH/g and the melting point of 40-60 ℃ to 90-110 ℃, preserving heat for 2-4 h, and pouring 200g of melting liquid into a beaker after the unsaturated polyester solid resin is completely melted; then 200g of propylene oxide neopentyl glycol dimethacrylate and 0.09g of 2, 5-di-tert-butyl hydroquinone are added and stirred at high speed for 0.5 to 1 hour when the mixture is hot; stirring and mixing evenly, cooling to 30-40 ℃, adding 4g of tert-butyl peroxybenzoate, stirring for 0.5-1 h, and cooling to room temperature to obtain the finished product of the low-volatility and low-shrinkage unsaturated polyester insulating resin.
Example 6
Embodiment 6 of the present invention provides a method for preparing a low-volatility and low-shrinkage unsaturated polyester insulating resin, comprising the steps of: firstly, preheating unsaturated polyester solid resin with the acid value of 30-35 mgKOH/g and the melting point of 40-60 ℃ to 90-110 ℃, preserving heat for 2-4 h, and pouring 208g of melting liquid into a beaker after the unsaturated polyester solid resin is completely melted; then 100g of dicyclopentadiene methacrylate, 92g of propoxylated neopentyl glycol dimethacrylate and 0.09g of 2, 5-di-tert-butyl hydroquinone are added and stirred at high speed for 0.5 to 1 hour when the mixture is hot; stirring and mixing evenly, cooling to 30-40 ℃, adding 6g of dicumyl peroxide, stirring for 0.5-1 h, and cooling to room temperature to obtain the finished product of the low-volatility and low-shrinkage unsaturated polyester insulating resin.
Example 7
Embodiment 7 of the present invention provides a method for preparing a low-volatility, low-shrinkage unsaturated polyester insulating resin, comprising the steps of: firstly, preheating unsaturated polyester solid resin with an acid value of 30-35 mgKOH/g and a melting point of 40-60 ℃ to 90-110 ℃, preserving heat for 2-4 h, and pouring 205g of melting liquid into a beaker after the unsaturated polyester solid resin is completely melted; then 100g of tricyclodecane dimethanol dimethacrylate, 95g of propylene oxide neopentyl glycol dimethacrylate and 0.09g of 2, 5-di-tert-butyl hydroquinone are added and stirred at high speed for 0.5 to 1 hour when the mixture is hot; stirring and mixing evenly, cooling to 30-40 ℃, adding 6g of dicumyl peroxide, stirring for 0.5-1 h, and cooling to room temperature to obtain the finished product of the low-volatility and low-shrinkage unsaturated polyester insulating resin.
Example 8
Embodiment 7 of the present invention provides a method for preparing a low-volatility, low-shrinkage unsaturated polyester insulating resin, comprising the steps of: firstly, preheating unsaturated polyester solid resin with the acid value of 30-35 mgKOH/g and the melting point of 40-60 ℃ to 90-110 ℃, preserving heat for 2-4 h, and pouring 206g of melting liquid into a beaker after the unsaturated polyester solid resin is completely melted; then adding 50g of dicyclopentadiene methacrylate, 50g of tricyclodecane dimethanol dimethacrylate, 94g of propoxylated neopentyl glycol dimethacrylate and 0.09g of 2, 5-di-tert-butyl hydroquinone, and stirring at high speed for 0.5-1 h while the mixture is hot; stirring and mixing evenly, cooling to 30-40 ℃, adding 6g of dicumyl peroxide, stirring for 0.5-1 h, and cooling to room temperature to obtain the finished product of the low-volatility and low-shrinkage unsaturated polyester insulating resin.
The properties of the low-volatility, low-shrinkage unsaturated polyester insulating resins prepared in examples 1 to 8 were measured, and the results are shown in the following table.
As can be seen from Table 1, the unsaturated polyester insulating resin with low volatility and low shrinkage prepared in the embodiments 1 to 8 of the present invention has the advantages of moderate viscosity, moderate gelling time, low curing volatile matter, low curing shrinkage, good thick-layer curing performance, high bonding strength and good electrical insulating performance, which indicates that the unsaturated polyester insulating resin provided by the present invention has excellent comprehensive performance; among them, the performance of each aspect of example 7 is better.
The above examples 1 to 8 are preferred embodiments for obtaining the low-volatility and low-shrinkage unsaturated polyester insulating resin, but the specific embodiments of the present invention are not intended to limit the scope of the present invention. Any other corresponding changes and modifications made according to the technical idea of the present invention should be included in the protection scope of the claims of the present invention.
Claims (4)
1. An unsaturated polyester insulating resin characterized in that: the high-performance polyester resin comprises, by weight, 49-62% of unsaturated polyester solid resin, 36-49% of acrylate reactive diluent, 1-2% of peroxide thermal initiator and 0.01-0.03% of free radical polymerization inhibitor; the unsaturated polyester solid resin is unsaturated polyester resin with an acid value of 30-35 mgKOH/g and a melting point of 40-60 ℃; the acrylate reactive diluent is one or a mixture of two of cyclohexyl methacrylate, isobornyl methacrylate, dicyclopentadiene methacrylate, tricyclodecane dimethanol dimethacrylate and propylene oxide neopentyl glycol dimethacrylate.
2. The unsaturated polyester insulating resin according to claim 1, wherein said peroxide thermal initiator is one or a mixture of t-butyl peroxybenzoate and dicumyl peroxide.
3. The unsaturated polyester insulating resin of claim 1, wherein the radical polymerization inhibitor is one or a mixture of two of p-methoxyphenol, hydroquinone, p-tert-butylcatechol, 2,5-di-tert-butylhydroquinone.
4. A method for preparing the unsaturated polyester insulating resin according to claim 1, comprising the steps of:
(1) Preheating unsaturated polyester solid resin to 90-110 ℃ in advance, weighing and pouring into a beaker;
(2) Then adding acrylic ester active diluent and free radical polymerization inhibitor, and stirring at high speed for 0.5-1 hour when the mixture is hot;
(3) Stirring and mixing evenly, cooling to 30-40 ℃, adding a peroxide thermal initiator, stirring for 0.5-2 h, mixing evenly, and cooling to room temperature to obtain the low-volatility and low-shrinkage unsaturated polyester insulating resin.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202211368705.XA CN115594802A (en) | 2022-11-03 | 2022-11-03 | Unsaturated polyester insulating resin and preparation method thereof |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202211368705.XA CN115594802A (en) | 2022-11-03 | 2022-11-03 | Unsaturated polyester insulating resin and preparation method thereof |
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| CN115594802A true CN115594802A (en) | 2023-01-13 |
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| CN202211368705.XA Pending CN115594802A (en) | 2022-11-03 | 2022-11-03 | Unsaturated polyester insulating resin and preparation method thereof |
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