CN110885543B - Organic silicon modified unsaturated resin insulation impregnating resin and preparation method thereof - Google Patents

Organic silicon modified unsaturated resin insulation impregnating resin and preparation method thereof Download PDF

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CN110885543B
CN110885543B CN201911202930.4A CN201911202930A CN110885543B CN 110885543 B CN110885543 B CN 110885543B CN 201911202930 A CN201911202930 A CN 201911202930A CN 110885543 B CN110885543 B CN 110885543B
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resin
organic silicon
modified unsaturated
unsaturated resin
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CN110885543A (en
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王亚飞
张凯
唐勇军
程浩
易辉
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Hubei Greatsea Newpower Technology Co ltd
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    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L67/00—Compositions of polyesters obtained by reactions forming a carboxylic ester link in the main chain; Compositions of derivatives of such polymers
    • C08L67/06—Unsaturated polyesters
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
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    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
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    • C08L2203/20—Applications use in electrical or conductive gadgets

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Abstract

The invention discloses an organic silicon modified unsaturated resin insulation impregnating resin and a preparation method thereof, wherein the organic silicon modified unsaturated resin insulation impregnating resin comprises the following components in parts by weight: 70-85 parts of organic silicon modified unsaturated resin, 5-15 parts of epoxy resin, 5-20 parts of epoxy curing agent, 0.1-1 part of accelerator, 0.1-2 parts of initiator and 0.01-0.5 part of polymerization inhibitor. The organic silicon modified unsaturated resin insulation impregnating resin provided by the invention contains unsaturated bonds and silicon-oxygen bonds, generates a cross-linking curing reaction under a free radical high-temperature initiation system to generate a reticular three-dimensional macromolecular resin, and has the advantages of the unsaturated resin and the organic silicon resin; the organic silicon modified unsaturated resin insulation impregnating resin provided by the invention has the characteristics of low volatile content, no odor, high storage stability, high bonding strength, low dielectric loss factor and good heat resistance.

Description

Organic silicon modified unsaturated resin insulation impregnating resin and preparation method thereof
Technical Field
The invention relates to the technical field of insulating impregnating resin, in particular to organic silicon modified unsaturated resin insulating impregnating resin and a preparation method thereof.
Background
With the rapid development of high-voltage large motors and variable-frequency motors in China, the requirements on insulating materials are gradually improved, the comprehensive properties such as electrical properties and mechanical properties are required to be excellent, and meanwhile, higher requirements on heat resistance and weather resistance of the insulating materials are provided. At present, unsaturated resin and organic silicon resin are widely applied in the field of solvent-free impregnating resin, the unsaturated resin is cheap, has strong universality and strong adhesive force with different base materials, but the heat-resistant grade is generally difficult to reach more than 200 ℃; the organic silicon resin has excellent heat resistance, weather resistance and insulating property, but has the problems of low adhesive force and poor adhesive force.
Disclosure of Invention
The invention aims to overcome the technical defects, provides an organic silicon modified unsaturated resin insulating impregnating resin and a preparation method thereof, and solves the technical problem that the insulating impregnating resin in the prior art cannot have good heat resistance and cohesiveness.
In order to achieve the technical purpose, the first solution of the invention provides an organosilicon modified unsaturated resin insulation impregnating resin, which comprises the following components in parts by weight: 70-85 parts of organic silicon modified unsaturated resin, 5-15 parts of epoxy resin, 5-20 parts of epoxy curing agent, 0.1-1 part of accelerator, 0.1-2 parts of initiator and 0.01-0.5 part of polymerization inhibitor.
The second solution of the invention provides a preparation method of organic silicon modified unsaturated resin insulation impregnating resin, which comprises the following steps:
dissolving the weighed polymerization inhibitor by absolute ethyl alcohol, adding the polymerization inhibitor into organic silicon modified unsaturated resin cooled to be less than or equal to 80 ℃, and mechanically stirring and uniformly mixing to obtain mixed liquid;
and sequentially adding the weighed liquid epoxy resin, epoxy curing agent, accelerator and initiator into the mixed solution, stirring for 30-60 min, uniformly mixing, and cooling to obtain the organic silicon modified unsaturated resin insulation impregnating resin.
The preparation method of the organic silicon modified unsaturated resin insulation impregnating resin is used for preparing the organic silicon modified unsaturated resin insulation impregnating resin provided in the first solution of the invention.
Compared with the prior art, the invention has the beneficial effects that:
the organic silicon modified unsaturated resin insulation impregnating resin provided by the invention contains unsaturated bonds and silicon-oxygen bonds, generates a cross-linking curing reaction under a free radical high-temperature initiation system to generate a reticular three-dimensional macromolecular resin, and has the advantages of the unsaturated resin and the organic silicon resin;
the organic silicon modified unsaturated resin insulation impregnating resin provided by the invention has the characteristics of low volatile content, no odor, high storage stability, high bonding strength, low dielectric loss factor and good heat resistance.
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention more apparent, the present invention is further described in detail with reference to the following embodiments. It should be understood that the specific embodiments described herein are merely illustrative of the invention and are not intended to limit the invention.
For the first solution of the invention, the invention provides an organosilicon modified unsaturated resin insulation impregnating resin, which comprises the following components in parts by weight: 70-85 parts of organic silicon modified unsaturated resin, 5-15 parts of epoxy resin, 5-20 parts of epoxy curing agent, 0.1-1 part of accelerator, 0.1-2 parts of initiator and 0.01-0.5 part of polymerization inhibitor. The organic silicon modified unsaturated resin is prepared from dibasic acid, dihydric alcohol, acid anhydride and an organic silicon prepolymer containing vinyl by a two-step melt polycondensation method, and the molecular weight of the obtained organic silicon modified unsaturated resin is less than or equal to 5000. Specifically, the two-step melt polycondensation comprises the following specific steps:
(1) adding dibasic acid, dihydric alcohol and anhydride, heating, and then carrying out reflux reaction and normal pressure distillation reaction to obtain an unsaturated resin prepolymer with hydroxyl; wherein the dihydric alcohol comprises dihydric alcohol A and dihydric alcohol B;
(2) and then adding an organosilicon prepolymer containing vinyl to carry out distillation reaction, and finally obtaining the organosilicon modified unsaturated resin with the molecular weight less than or equal to 5000.
Further, in the step (1), firstly adding the dibasic acid and the dihydric alcohol A, wherein the molar ratio of the dibasic acid to the dihydric alcohol A is less than 1, refluxing for 1h at 140-160 ℃, heating to 190 ℃, and continuing to react for 4 h; then cooling to 100 deg.C, adding anhydride and dihydric alcohol B, cooling to 160 deg.C and N2And under the protection condition, carrying out reflux reaction for 4 hours, then gradually heating to 200-210 ℃, and carrying out distillation reaction for 2-3 hours under normal pressure to obtain the unsaturated resin prepolymer with hydroxyl. Specifically, the adding amount of the dihydric alcohol is 1.1 to 1.3 times of the total molar amount of the dibasic acid and the anhydride, the adding amount of the dibasic acid accounts for 30 to 50 percent of the total molar amount of the dibasic acid and the anhydride, the dihydric alcohol A accounts for 30 to 50 percent of the total molar amount of the dihydric alcohol, and the dihydric alcohol B accounts for 50 to 70 percent of the total molar amount of the dihydric alcohol.
In the system, because the activity of the dibasic acid is different from that of the anhydride, the dibasic acid with lower activity and the dihydric alcohol A are added firstly to react to generate a saturated ester prepolymer with a hydroxyl end group, and then the anhydride with higher activity and the dihydric alcohol B are added to react; meanwhile, in the process, the proportion of the dibasic acid and the anhydride is strictly controlled, so that the density of unsaturated bonds is controlled, and the influence on the product performance caused by overhigh crosslinking density in the subsequent reaction process is avoided.
Further, in the step (2), the unsaturated resin prepolymer having hydroxyl group obtained in the step (1) is cooled to 120 ℃, and a vinyl group-containing silicone prepolymer is added thereto, and then the mixture is heated under N2And (3) heating to 210 ℃ under protection, distilling at normal pressure for 2-3 h, then distilling at reduced pressure for 1-2 h, and cooling to less than or equal to 80 ℃ when the acid value of the reaction system is less than or equal to 5mg KOH/g to obtain the organic silicon modified unsaturated resin with the molecular weight less than or equal to 5000.
Among them, the method for detecting the acid value is a method commonly used by those skilled in the art.
In the invention, the dibasic acid is one or more of terephthalic acid, isophthalic acid and adipic acid; the dihydric alcohol is one or more of ethylene glycol, propylene glycol, neopentyl glycol and diethylene glycol; the acid anhydride is one or more of maleic anhydride, nadic anhydride and phthalic anhydride; the organosilicon prepolymer containing vinyl is one or more of polymethylphenyl vinyl siloxane, polyvinyl phenyl siloxane and polymethylvinyl siloxane; the epoxy resin is one or more of bisphenol F type epoxy resin (such as F170) and bisphenol A type epoxy resin (such as E51 and E54); the epoxy curing agent is one or more of tung oil anhydride, methyl hexahydrophthalic anhydride, methyl nadic anhydride and hydrogenated methyl nadic anhydride; the epoxy accelerant is one or more of zinc naphthenate, zinc isooctanoate, chromium acetylacetonate and boron trifluoride ethylamine; the initiator is a high-temperature initiator with the critical temperature of more than 100 ℃, so that the system can be kept stable for a long time within the range of 25-60 ℃, and specifically, the initiator is one or more of dicumyl peroxide, tert-butyl peroxybenzoate, di-tert-butyl peroxyisopropylbenzene and 1, 1-di-tert-butyl peroxycyclohexane; the polymerization inhibitor is one or more of hydroquinone, tert-butyl catechol, copper naphthenate and p-methoxyphenol.
For the second solution of the invention, the invention provides a preparation method of organic silicon modified unsaturated resin insulation impregnating resin, which comprises the following steps:
s1, dissolving the weighed polymerization inhibitor by absolute ethyl alcohol, adding the polymerization inhibitor into the organic silicon modified unsaturated resin cooled to be less than or equal to 80 ℃, and mechanically stirring and uniformly mixing; wherein the weight ratio of the polymerization inhibitor to the absolute ethyl alcohol is (0.8-1.2): 1
And S2, sequentially adding the weighed liquid epoxy resin, epoxy curing agent, accelerator and initiator into the mixed solution obtained in the step S1, stirring for 30-60 min, uniformly mixing, and cooling to obtain the organic silicon modified unsaturated resin insulation impregnating resin.
The preparation method of the organic silicon modified unsaturated resin insulation impregnating resin is used for preparing the organic silicon modified unsaturated resin insulation impregnating resin provided in the first solution of the invention.
In order to avoid redundancy, the specific steps for preparing the silicone modified unsaturated resin insulation impregnating resin in the following examples and comparative examples of the invention are summarized as follows:
synthesizing organic silicon modified unsaturated polyester: firstly adding 0.4mol of dibasic acid and 0.45mol of dihydric alcohol, heating to 150 ℃, refluxing for 1h, then heating to 190 ℃, reacting for 4h, then cooling to 100 ℃, adding 0.60mol of acid anhydride and 0.65mol of dihydric alcohol, introducing N at 160 ℃, and introducing N2Carrying out reflux reaction for 4h under the condition, then gradually heating to 210 ℃ and carrying out distillation reaction for 2h under normal pressure to obtain an unsaturated resin prepolymer with a certain amount of hydroxyl groups; cooling the unsaturated resin prepolymer with a certain amount of hydroxyl groups to 120 ℃, adding an organic silicon prepolymer containing vinyl into the cooled unsaturated resin prepolymer, and adding the organic silicon prepolymer into the mixture in the presence of N2Heating to 210 ℃ under protection, carrying out atmospheric distillation reaction for 3h, carrying out reduced pressure distillation reaction for 1.5h, discharging at the temperature of less than or equal to 80 ℃ after the reaction is finished, controlling the molecular weight to be less than or equal to 5000, and controlling the acid value to be less than or equal to 5mg KOH/g.
Preparing organic silicon modified unsaturated resin insulation impregnating resin: dissolving weighed polymerization inhibitor in absolute ethyl alcohol according to the raw material proportion of table 1, adding the dissolved polymerization inhibitor into organic silicon modified unsaturated resin, and mechanically stirring and uniformly mixing to obtain a mixture; and (2) sequentially adding the epoxy resin, the epoxy curing agent, the accelerator and the initiator into the mixture according to the table 1, stirring for 30-60 min, uniformly mixing, and cooling to obtain the organic silicon modified unsaturated resin insulation impregnating resin.
Examples 1-3 and comparative examples 1-2 provide five different insulating impregnating resins, the raw material compositions and parts by weight of which are shown in table 1.
TABLE 1 compositions and parts by weight of respective raw materials of insulating impregnating resins in examples 1 to 3 and comparative examples 1 to 2
Figure BDA0002296323120000051
Figure BDA0002296323120000061
Performance testing
The resin insulating impregnating resins of examples 1 to 3 and comparative examples 1 to 2 were tested for their performance, and the test results are shown in Table 2.
TABLE 2 Performance test results of the insulating impregnating resins in examples 1 to 3 and comparative examples 1 to 2
Figure BDA0002296323120000062
Figure BDA0002296323120000071
As can be seen from Table 2, the organic silicon modified unsaturated resin insulation impregnating resin obtained in the embodiments 1-3 is environment-friendly and odorless, and can reduce the pollution to the environment and the damage to operators in the use process, and the curing volatile matter is less than 1% under the condition of being placed at 150 ℃ for 3 hours; the organic silicon modified unsaturated resin insulation impregnating resin obtained in the embodiments 1-3 has excellent electrical performance, the electrical strength is more than 27kV/mm, and the high-temperature dielectric loss factor can be reduced to below 2%; the organic silicon modified unsaturated resin insulation impregnating resin has good mechanical property, the normal temperature bonding strength is more than 200N, and the high temperature bonding strength is more than 50N; the organic silicon modified unsaturated resin insulation impregnating resin has excellent high temperature resistance, and the initial thermal decomposition temperature is more than 300 ℃; the organic silicon modified unsaturated resin insulation impregnating resin has good storage stability and long service cycle.
It can also be seen from table 2 that the properties of the insulating impregnating resins obtained in comparative examples 1-2 do not fully meet the index requirements. The reasons are that F170, E54 and tung oil anhydride have good flexibility, the heat-resistant grade after curing is generally lower, and the heat resistance is poor, while in comparative examples 1-2, the proportion of the components of epoxy resin and anhydride is higher, so that the heat resistance of the cured insulating impregnating resin is reduced, the initial decomposition temperature is less than 300 ℃, and the bonding strength is less than 50N under the condition of 180 ℃; meanwhile, in the comparative example 1, the ratio of the epoxy resin to the acid anhydride is high, and if the curing is insufficient, the dielectric loss factor at 180 ℃ is correspondingly increased; in comparative example 2, the viscosity of the tung oil anhydride is high and the proportion is high in the whole system, so that the viscosity is remarkably increased, and the index requirement cannot be met.
In conclusion, in the range provided by the invention, the insulating impregnating resin with various performances meeting the performance indexes can be synthesized; therefore, in the actual production process, in order to control the performance of the obtained insulating impregnating resin, the proportion of the raw material components is strictly controlled within the range provided by the invention.
Compared with the prior art, the invention has the beneficial effects that:
the organic silicon modified unsaturated resin insulation impregnating resin provided by the invention contains unsaturated bonds and silicon-oxygen bonds, generates a cross-linking curing reaction under a free radical high-temperature initiation system to generate a reticular three-dimensional macromolecular resin, and has the advantages of the unsaturated resin and the organic silicon resin;
the organic silicon modified unsaturated resin insulation impregnating resin provided by the invention has the characteristics of low volatile content, no odor, high storage stability, high bonding strength, low dielectric loss factor and good heat resistance;
the preparation method of the organic silicon modified unsaturated resin insulating impregnating resin provided by the invention has the advantages of simple process, effectiveness, feasibility and lower raw material cost;
the organic silicon modified unsaturated resin insulation impregnating resin provided by the invention can be generally used for VPI insulation treatment of equipment such as high-voltage motors, wind power, variable frequency motors, low-voltage high-power motors and the like.
The above description is only for the purpose of illustrating the preferred embodiments of the present invention and is not to be construed as limiting the invention, and any modifications, equivalents, improvements and the like that fall within the spirit and principle of the present invention are intended to be included therein.

Claims (9)

1. The organic silicon modified unsaturated resin insulation impregnating resin is characterized by comprising the following components in parts by weight:
70-85 parts of organic silicon modified unsaturated resin, 5-15 parts of epoxy resin, 5-20 parts of epoxy curing agent, 0.1-1 part of accelerator, 0.1-2 parts of initiator and 0.01-0.5 part of polymerization inhibitor; the organic silicon modified unsaturated resin is prepared from dibasic acid, dihydric alcohol, acid anhydride and an organic silicon prepolymer containing vinyl by a two-step melt polycondensation method, and the molecular weight of the obtained organic silicon modified unsaturated resin is less than or equal to 5000.
2. The silicone modified unsaturated resin insulation impregnating resin according to claim 1, wherein said two-step melt polycondensation comprises the following specific steps:
adding dibasic acid, dihydric alcohol and anhydride, heating, and then carrying out reflux reaction and normal pressure distillation reaction to obtain an unsaturated resin prepolymer with hydroxyl; wherein the dihydric alcohol comprises dihydric alcohol A and dihydric alcohol B;
and then adding an organosilicon prepolymer containing vinyl to carry out distillation reaction, and finally obtaining the organosilicon modified unsaturated resin with the molecular weight less than or equal to 5000.
3. The organic silicon modified unsaturated resin insulation impregnating resin according to claim 2, wherein the specific steps of obtaining the unsaturated resin prepolymer with hydroxyl group are as follows: firstly, adding dibasic acid and dihydric alcohol A, wherein the molar ratio of the dibasic acid to the dihydric alcohol A is less than 1, refluxing for 1h at 140-160 ℃, heating to 190 ℃, and continuing to react for 4 h; then cooling to 100 deg.C, adding anhydride and dihydric alcohol B, cooling to 160 deg.C and N2Protection ofAnd under the condition, carrying out reflux reaction for 4 hours, then gradually heating to 200-210 ℃, and carrying out atmospheric distillation reaction for 2-3 hours to obtain the unsaturated resin prepolymer with hydroxyl.
4. The insulation impregnating resin of organosilicon modified unsaturated resin according to claim 3, wherein the amount of said diol added is 1.1-1.3 times of the total molar amount of diacid and anhydride, the amount of said diacid added is 30-50% of the total molar amount of diacid and anhydride, said diol A is 30-50% of the total molar amount of diol, and said diol B is 50-70% of the total molar amount of diol.
5. The organic silicon modified unsaturated resin insulation impregnating resin according to claim 2, wherein the specific steps of finally obtaining the organic silicon modified unsaturated resin with the molecular weight less than or equal to 5000 are as follows: cooling the unsaturated resin prepolymer with hydroxyl to 120 ℃, adding an organic silicon prepolymer containing vinyl into the unsaturated resin prepolymer, and adding the organic silicon prepolymer into the mixture in the presence of N2And (3) heating to 210 ℃ under protection, distilling at normal pressure for 2-3 h, then distilling at reduced pressure for 1-2 h, and cooling to less than or equal to 80 ℃ when the acid value of the reaction system is less than or equal to 5mg KOH/g to obtain the organic silicon modified unsaturated resin with the molecular weight less than or equal to 5000.
6. The insulation impregnating resin of organosilicon modified unsaturated resin according to claim 1, wherein said dibasic acid is one or more of terephthalic acid, isophthalic acid, adipic acid; the dihydric alcohol is one or more of ethylene glycol, propylene glycol, neopentyl glycol and diethylene glycol; the acid anhydride is one or more of maleic anhydride, nadic anhydride and phthalic anhydride; the organic silicon prepolymer containing vinyl is one or more of polymethylphenyl vinyl siloxane, polyvinyl phenyl siloxane and polymethylvinyl siloxane.
7. The insulation impregnating resin of organosilicon modified unsaturated resin according to claim 1, wherein said epoxy resin is one or more of bisphenol F type epoxy resin and bisphenol A type epoxy resin; the epoxy curing agent is one or more of tung oil anhydride, methyl hexahydrophthalic anhydride, methyl nadic anhydride and hydrogenated methyl nadic anhydride; the accelerant is one or more of zinc naphthenate, zinc isooctanoate, chromium acetylacetonate and boron trifluoride ethylamine.
8. The insulation-impregnating resin of organosilicon modified unsaturated resin according to claim 1, wherein said initiator is one or more of dicumyl peroxide, t-butyl peroxybenzoate, di-t-butyl peroxycumene, 1-di-t-butyl peroxycyclohexane; the polymerization inhibitor is one or more of hydroquinone, tert-butyl catechol, copper naphthenate and p-methoxyphenol.
9. A preparation method of the organic silicon modified unsaturated resin insulation impregnating resin as described in any one of claims 1-8, characterized by comprising the following steps:
dissolving the weighed polymerization inhibitor by absolute ethyl alcohol, adding the polymerization inhibitor into organic silicon modified unsaturated resin cooled to be less than or equal to 80 ℃, and mechanically stirring and uniformly mixing to obtain mixed liquid;
and sequentially adding the weighed liquid epoxy resin, epoxy curing agent, accelerator and initiator into the mixed solution, stirring for 30-60 min, uniformly mixing, and cooling to obtain the organic silicon modified unsaturated resin insulation impregnating resin.
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CN102124054B (en) * 2008-08-12 2013-01-30 株式会社钟化 Unsaturated ester resin composition, unsaturated ester-cured product, and manufacturing method therefor
CN102225986A (en) * 2011-04-21 2011-10-26 苏州巨峰电气绝缘***股份有限公司 Environmentally-friendly type solvent-free impregnating resin and preparation method thereof
CN103113526B (en) * 2013-02-01 2015-04-15 海宁永大电气新材料有限公司 Solvent-less impregnating resin for high-voltage motor and curing method
CN105778386A (en) * 2016-03-10 2016-07-20 江西省科学院应用化学研究所 Preparation method for organic silicone modified unsaturated polyester ternary nano-composite material
CN106811023B (en) * 2016-12-06 2019-08-06 浙江博菲电气股份有限公司 A kind of environment-friendly type wind-driven generator VPI impregnating resin and preparation method thereof

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