CN109054601B - Humidity-heat-resistant high-toughness modified unsaturated polyester solvent-free impregnating varnish and preparation method thereof - Google Patents
Humidity-heat-resistant high-toughness modified unsaturated polyester solvent-free impregnating varnish and preparation method thereof Download PDFInfo
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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
- C09D167/00—Coating compositions based on polyesters obtained by reactions forming a carboxylic ester link in the main chain; Coating compositions based on derivatives of such polymers
- C09D167/06—Unsaturated polyesters having carbon-to-carbon unsaturation
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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
- C09D5/00—Coating compositions, e.g. paints, varnishes or lacquers, characterised by their physical nature or the effects produced; Filling pastes
- C09D5/18—Fireproof paints including high temperature resistant paints
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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
- C09D7/00—Features of coating compositions, not provided for in group C09D5/00; Processes for incorporating ingredients in coating compositions
- C09D7/40—Additives
- C09D7/60—Additives non-macromolecular
- C09D7/63—Additives non-macromolecular organic
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
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Abstract
The invention discloses a damp-heat resistant high-toughness modified unsaturated polyester solvent-free impregnating varnish which is mainly prepared from the following raw materials in parts by weight: 2-8 parts of polyol A, 12-30 parts of polyol B, 15-35 parts of polybasic acid, 8-25 parts of oil, 8-25 parts of epoxy resin, 15-35 parts of reactive diluent, 0.5-4 parts of curing agent, 0.8-1.5 parts of initiator and 0.1-0.4 part of polymerization inhibitor. According to the invention, the impregnating varnish is modified by oil, so that a large number of hydrophobic groups are introduced, the water resistance of the impregnating varnish is improved, and the toughness of the impregnating varnish is improved. The epoxy resin is added in the process of synthesizing the unsaturated resin, and the epoxy resin has excellent moisture and heat resistance, and is equivalent to introducing a blocking monomer into the unsaturated polyester, so that polar groups are reduced, and the moisture and heat resistance of the impregnating varnish is improved.
Description
Technical Field
The invention belongs to the field of insulating materials, and particularly relates to a humidity-heat-resistant high-toughness modified unsaturated polyester solvent-free impregnating varnish and a preparation method thereof.
Background
The impregnating varnish is used for impregnating the coils of motors and electric appliances, filling gaps and micropores in an insulation system and forming a continuous paint film on the surface of an impregnated object, so that the coils are bonded into a solid whole, and the integrity, the thermal conductivity, the moisture resistance, the dielectric strength and the mechanical strength of the insulation system are effectively improved. Currently, the main development direction of impregnating insulating paints is the environmentally friendly high performance products. Face increasingly higher performance requirements, especially environmental resistance requirements, for electrical products. The common unsaturated polyester solvent-free impregnating varnish has the defects of large brittleness and poor environment resistance of a paint film, and particularly, the paint film of the common unsaturated polyester solvent-free impregnating varnish cracks, turns white and even pulverizes in a damp-heat alternating environment, the electrical property is sharply reduced, and the safe operation of a motor is seriously influenced.
Disclosure of Invention
The technical problem to be solved by the invention is to overcome the defects and shortcomings in the background technology and provide the humidity-heat-resistant high-toughness modified unsaturated polyester solvent-free impregnating varnish and the preparation method thereof.
In order to solve the technical problems, the technical scheme provided by the invention is as follows:
a modified unsaturated polyester solvent-free impregnating varnish with high humidity and heat resistance and high toughness is mainly prepared from the following raw materials in parts by weight:
preferably, the polybasic acid is one or more of isophthalic acid, terephthalic acid, glutaric acid, adipic acid, sebacic acid, phthalic anhydride, maleic anhydride, methyl tetrahydrophthalic anhydride, maleic acid and dimer fatty acid. The polybasic acid is used for esterification, and the combination of different polybasic acids can ensure the comprehensive performance of the impregnating varnish.
In the above solventless impregnating varnish, preferably, the polyol a is one or two of glycerol and pentaerythritol; the polyol B is one or more of ethylene glycol, propylene glycol, butanediol, neopentyl glycol and tris (2-hydroxyethyl) isocyanurate. The polyhydric alcohol is used for esterification, and the combination of different alcohols can ensure the comprehensive performance of the impregnating varnish.
Preferably, the oil is one or more of linseed oil, tung oil and soybean oil. The introduction of oil can improve the humidity resistance and the toughness of the impregnating varnish.
Preferably, the epoxy resin is one or more of bisphenol a epoxy resin E20, epoxy resin E44 and epoxy resin E51. The introduction of the epoxy resin can improve the wet and heat resistance of the impregnating varnish. The viscosity of the impregnating varnish can be effectively controlled by adopting the selected epoxy resin.
Preferably, the reactive diluent is one or more of vinyl toluene, 1, 4-butanediol diacrylate, diallyl phthalate (DAP), neopentyl glycol diacrylate and styrene. The reactive diluent functions to control viscosity. The selected diluent has good activity and dilutability.
Preferably, the curing agent is one or more of zinc isooctanoate, zinc naphthenate, cobalt naphthenate and calcium naphthenate. The curing agent mainly plays a role in participating in crosslinking of the impregnating resin. The above curing agent is selected according to the reaction temperature.
Preferably, the initiator is one or more of dicumyl peroxide, tert-butyl peroxybenzoate and ethyl-3, 3-di (tert-butylperoxy) butyrate. The initiator mainly serves to initiate crosslinking of the impregnating resin. The above initiators are selected according to the reaction temperature.
Preferably, the polymerization inhibitor is one or more of methyl hydroquinone, hydroquinone and 2, 5-di-tert-butyl hydroquinone. The polymerization inhibitor is used for preventing the polymerization of the impregnating varnish and ensuring the stability of the impregnating varnish. The above polymerization inhibitor is selected according to the reaction temperature.
As a general inventive concept, the invention also provides a preparation method of the humidity-heat-resistant high-toughness modified unsaturated polyester solvent-free impregnating varnish, which comprises the following steps:
(1) alcoholysis: adding oil and polyol A into a reaction kettle, uniformly mixing, gradually heating to 230-250 ℃, and carrying out heat preservation reaction for 1.5-3 hours to obtain an alcoholysis product;
(2) esterification: cooling the alcoholysis product to 150-170 ℃, adding the polyol B and the polybasic acid into a reaction kettle of the alcoholysis product, uniformly mixing, gradually heating to 180-215 ℃ for esterification, when the acid value is reduced to 30-40 mgKOH/g, vacuumizing until the acid value is reduced to 20-25mgKOH/g, cooling to 150-165 ℃, adding the epoxy resin, preserving the temperature for 30-50 min, then adding the polymerization inhibitor, uniformly mixing, cooling to 70-90 ℃, adding the active diluent, finally cooling to 30-60 ℃, adding the initiator and the curing agent, and uniformly mixing to obtain the moisture-heat-resistant high-toughness modified unsaturated polyester solvent-free impregnating varnish.
In the preparation method of the invention, the polyol is added in two steps, so that the reaction process can be controlled.
In the preparation method, preferably, in the step (1), the gradual temperature rise is performed by temperature programming at a temperature rise rate of 1.5-3.5 ℃/min; in the step (2), the pressure for vacuumizing is 100-500 Pa.
According to the invention, the modification of the impregnating varnish by the oil not only introduces a large amount of hydrophobic groups, increases the water resistance of the impregnating varnish, but also increases the toughness of the impregnating varnish; the epoxy resin is added in the unsaturated resin synthesis process, and the epoxy resin has excellent moisture and heat resistance, and is equivalent to that an end-capping monomer is introduced into unsaturated polyester, so that polar groups are reduced, and the moisture and heat resistance of the impregnating varnish is improved.
Compared with the prior art, the invention has the advantages that:
1. the modified unsaturated polyester solvent-free impregnating varnish with high humidity resistance, high toughness and high reaction activity has large molecular weight.
2. According to the invention, the impregnating varnish is modified by oil, so that a large number of hydrophobic groups are introduced, the water resistance of the impregnating varnish is improved, and the toughness of the impregnating varnish is improved.
3. The epoxy resin is added in the process of synthesizing the unsaturated resin, and the epoxy resin has excellent moisture and heat resistance, and is equivalent to introducing a blocking monomer into the unsaturated polyester, so that polar groups are reduced, and the moisture and heat resistance of the impregnating varnish is improved.
4. The modified unsaturated polyester solvent-free impregnating varnish with the characteristics of humidity resistance, high toughness, low viscosity, good permeability, low volatile matter content, quick curing, good humidity resistance, good cold and heat shock resistance and the like.
Detailed Description
In order to facilitate an understanding of the present invention, the present invention will be described more fully and in detail with reference to the preferred embodiments, but the scope of the present invention is not limited to the specific embodiments below.
Unless otherwise defined, all terms of art used hereinafter have the same meaning as commonly understood by one of ordinary skill in the art. The terminology used herein is for the purpose of describing particular embodiments only and is not intended to limit the scope of the present invention.
Unless otherwise specifically stated, various raw materials, reagents, instruments, equipment and the like used in the present invention are commercially available or can be prepared by existing methods.
Example 1
A modified unsaturated polyester solvent-free impregnating varnish with high humidity and heat resistance and high toughness is mainly prepared from the following raw materials in parts by weight:
23kg of polyol (3kg of tris (2-hydroxyethyl) isocyanurate (sak), 10kg of neopentyl glycol, 4kg of propylene glycol, 6kg of glycerol)
24kg of polybasic acid (5kg of isophthalic acid, 5kg of methyl tetrahydrophthalic anhydride, 14kg of maleic acid)
23kg of oil (Tung oil)
8kg of epoxy resin (bisphenol A type E44)
17kg of reactive diluent (vinyltoluene)
0.5kg curing agent (Zinc naphthenate)
1.2kg of initiator (dicumyl peroxide)
0.15kg polymerization inhibitor (hydroquinone)
The preparation method of the modified unsaturated polyester solvent-free impregnating varnish with high resistance to heat and humidity of the embodiment comprises the following steps:
(1) alcoholysis: adding 23kg of tung oil and 6kg of glycerol into a reaction kettle, uniformly mixing, heating to 235-245 ℃ at a heating rate of 3 ℃/min, and carrying out heat preservation reaction for 3 hours to obtain an alcoholysis product;
(2) esterification: cooling the alcoholysis product to 160-165 ℃, adding 3kg of tris (2-hydroxyethyl) isocyanurate, 10kg of neopentyl glycol, 4kg of propylene glycol, 5kg of isophthalic acid, 5kg of methyl tetrahydrophthalic anhydride and 14kg of maleic acid into a reaction kettle of the alcoholysis product, after being mixed evenly, the temperature is raised to 190-200 ℃ according to the temperature rise rate of 2 ℃/min to carry out esterification reaction, when the acid value is reduced to 35-40 mgKOH/g, vacuumizing until the acid value is reduced to 20-25mgKOH/g, cooling to 160-165 ℃, adding 8kg E44 epoxy resin, keeping the temperature for 30min, then 0.15kg of hydroquinone is added and mixed evenly, 17kg of vinyl toluene is added after the mixture is cooled to 75 ℃, finally the mixture is cooled to 50 ℃, 1.2kg of dicumyl peroxide and 0.5kg of zinc naphthenate are added and mixed evenly, and the humidity-heat-resistant high-toughness modified unsaturated polyester solvent-free impregnating varnish is obtained.
Example 2
A modified unsaturated polyester solvent-free impregnating varnish with high humidity and heat resistance and high toughness is mainly prepared from the following raw materials in parts by weight:
34kg of polyol (5kg of saxok, 25kg of neopentyl glycol, 4kg of pentaerythritol)
32kg of polybasic acid (6kg of isophthalic acid, 9kg of sebacic acid, 17kg of maleic anhydride)
15kg of oil (Soybean oil)
15kg of epoxy resin (E51)
25kg of reactive diluent (diallyl phthalate)
1.8kg curing agent (Zinc isooctanoate)
1.4kg of initiator (dicumyl peroxide)
0.32kg of polymerization inhibitor (2, 5-di-tert-butylhydroquinone)
The preparation method of the modified unsaturated polyester solvent-free impregnating varnish with high resistance to heat and humidity of the embodiment comprises the following steps:
(1) alcoholysis: adding 15kg of soybean oil and 4kg of pentaerythritol into a reaction kettle, uniformly mixing, heating to 230-240 ℃ at a heating rate of 3 ℃/min, and carrying out heat preservation reaction for 2 hours to obtain an alcoholysis product;
(2) esterification: cooling the alcoholysis product to 150-160 ℃, adding 5kg of seek, 25kg of neopentyl glycol, 6kg of isophthalic acid, 9kg of sebacic acid and 17kg of maleic anhydride into a reaction kettle of the alcoholysis product, uniformly mixing, heating to 185-195 ℃ at the heating rate of 2 ℃/min to perform esterification reaction, vacuumizing until the acid value is reduced to 20-25mgKOH/g when the acid value is reduced to 30-35mgKOH/g, cooling to 155-160 ℃, adding 15kg of E51 epoxy resin, preserving heat for 40min, adding 0.32kg of 2 and 5-di-tert-butyl hydroquinone, uniformly mixing, cooling to 85 ℃, adding 25kg of diallyl phthalate, cooling to 40 ℃, adding 1.4kg of dicumyl peroxide and 1.8kg of zinc isooctoate, and uniformly mixing to obtain the wet-heat-resistant high-toughness modified unsaturated polyester solventless impregnating varnish.
Example 3
A modified unsaturated polyester solvent-free impregnating varnish with high humidity and heat resistance and high toughness is mainly prepared from the following raw materials in parts by weight:
16kg of polyol (3kg of saxok, 8kg of neopentyl glycol, 3kg of butanediol, 2kg of pentaerythritol)
16kg of polybasic acid (4kg of phthalic anhydride, 6kg of sebacic acid, 6kg of maleic anhydride)
8kg of oil (Tung oil)
23kg of epoxy resin (E51)
32kg of reactive diluent (styrene)
3.4kg curing agent (Zinc isooctanoate)
0.8kg of initiator (ethyl-3, 3-di (t-butylperoxy) butyrate)
0.1kg polymerization inhibitor (methyl hydroquinone)
The preparation method of the modified unsaturated polyester solvent-free impregnating varnish with high resistance to heat and humidity of the embodiment comprises the following steps:
(1) alcoholysis: adding 8kg of tung oil and 2kg of pentaerythritol into a reaction kettle, uniformly mixing, heating to 235-240 ℃ at a heating rate of 3 ℃/min, and carrying out heat preservation reaction for 1.5 hours to obtain an alcoholysis product;
(2) esterification: cooling the alcoholysis product to 160-170 ℃, adding 3kg of seek, 8kg of neopentyl glycol, 3kg of butanediol, 4kg of phthalic anhydride, 6kg of sebacic acid and 6kg of maleic anhydride into a reaction kettle of the alcoholysis product, uniformly mixing, heating to 200-210 ℃ at the heating rate of 2 ℃/min for esterification reaction, vacuumizing until the acid value is reduced to 20-25mgKOH/g when the acid value is reduced to 35-40 mgKOH/g, cooling to 150-155 ℃, adding 23kg of E51 epoxy resin, preserving heat for 45min, then adding 0.1kg of methyl hydroquinone, uniformly mixing, cooling to 75 ℃, adding 32kg of styrene, finally cooling to 45 ℃, adding 0.8kg of ethyl-3, 3-di (tert-butyl peroxide) butyrate and 3.4kg of zinc isooctanoate, and uniformly mixing to obtain the modified unsaturated polyester solventless impregnating varnish with high heat resistance.
Comparative example 1
A common unsaturated polyester solvent-free impregnating varnish is mainly prepared from the following raw materials in parts by weight:
33kg of polyol (5kg of saxok, 17kg of neopentyl glycol, 9kg of butanediol, 2kg of propylene glycol)
34kg of polybasic acid (8kg of isophthalic acid, 8kg of adipic acid, 18kg of maleic anhydride)
32kg of reactive diluent (vinyltoluene)
1.2kg of initiator (dicumyl peroxide)
0.1kg polymerization inhibitor (hydroquinone)
The preparation method of the ordinary unsaturated polyester solvent-free impregnating varnish of the comparative example 1 comprises the following steps:
adding 8kg of isophthalic acid, 5kg of seek and 12kg of neopentyl glycol into a reaction kettle, uniformly mixing, gradually heating to 190-200 ℃ for esterification reaction, heating the rest part of the neopentyl glycol 5kg, 9kg of butanediol, 2kg of propylene glycol, 8kg of adipic acid and 18kg of maleic anhydride in the formula to 200-210 ℃ when the acid value is reduced to 20-25mgKOH/g, vacuumizing until the acid value is reduced to 20-25mgKOH/g, and cooling to 170 ℃; then adding 0.1kg of hydroquinone serving as a polymerization inhibitor, uniformly mixing, cooling to 70 ℃, adding 32kg of vinyl toluene serving as an active diluent, cooling to 60 ℃, finally adding 1.2kg of dicumyl peroxide serving as an initiator, and uniformly mixing to obtain the common solvent-free impregnating varnish.
The heat and humidity resistant high-toughness solvent-free impregnating varnish of the above examples 1-3 and the ordinary solvent-free impregnating varnish of the comparative example 1 were subjected to conventional performance tests; meanwhile, the wire rod dip coating experiment is carried out on the heat and humidity resistant high-toughness solvent-free dip coating of the embodiment 1-3 and the common solvent-free dip coating of the comparative example 1, and the specific method comprises the following steps: semi-overlapping and wrapping 2 layers of less-glue mica tapes on a copper wire rod, flatly wrapping a layer of polyester heat-shrinkable tape on the mica tapes, preheating for 2h at 105 ℃, cooling to below (60 +/-5) DEG C, performing vacuum dipping and dripping paint, finally performing high-temperature curing at 160 ℃ for 6h on the copper wire rod, and performing a damp-heat experiment under the conditions of 85% of humidity and 85 ℃ of temperature; in a high-temperature and low-temperature environment, the normal temperature is quickly reduced to-40 ℃, the temperature is maintained at-40 ℃ for 2h, the temperature is increased to 130 ℃, the temperature rising time is 1.5h, the temperature is maintained for 1h, the temperature is reduced to-40 ℃, the temperature reduction time is 1.5h, a cold-hot circulation experiment is carried out in one period, and the detection results are shown in table 1.
TABLE 1 Performance test results for solventless impregnating varnishes
As can be seen from the data in the table, the heat and humidity resistant high-toughness solvent-free impregnating varnish disclosed by the invention has the advantages of low viscosity, good permeability, low volatility, fast curing and good heat and humidity resistance, the appearance and electrical property retention rate of the impregnating varnish are good after a 1000-hour damp and heat experiment is carried out on the impregnating varnish in the examples 1-3, and the appearance of the varnish film is good after a cold and heat cycle experiment.
Claims (7)
1. A preparation method of humidity-heat-resistant high-toughness modified unsaturated polyester solvent-free impregnating varnish is characterized by comprising the following steps:
(1) alcoholysis: adding 8-25 parts by mass of oil and 2-8 parts by mass of polyol A into a reaction kettle, uniformly mixing, gradually heating to 230-250 ℃, and carrying out heat preservation reaction for 1.5-3 hours to obtain an alcoholysis product; the polyol A is one of glycerol and pentaerythritol;
(2) esterification: cooling the alcoholysis product to 150-170 ℃, adding 12-30 parts by mass of polyol B and 15-35 parts by mass of polyacid into a reaction kettle of the alcoholysis product, mixing uniformly, gradually heating to 180-215 ℃ for esterification, vacuumizing until the acid value is reduced to 20-25mgKOH/g when the acid value is reduced to 30-40 mgKOH/g, cooling to 150-165 ℃, adding 8-25 parts by mass of epoxy resin, preserving heat for 30-50 min, adding 0.1-0.4 part by mass of polymerization inhibitor, mixing uniformly, cooling to 70-90 ℃, adding 15-35 parts by mass of active diluent, cooling to 30-60 ℃, adding 0.8-1.5 parts by mass of initiator and 0.5-4 parts by mass of curing agent, and mixing uniformly to obtain the high-toughness modified unsaturated polyester solventless impregnating varnish; the polyol B is selected from ethylene glycol, propylene glycol, butanediol, neopentyl glycol and tris (2-hydroxyethyl) isocyanurate.
2. The method for preparing the wet heat resistant high toughness modified unsaturated polyester solventless impregnating varnish according to claim 1, wherein the polybasic acid is one or more of isophthalic acid, terephthalic acid, glutaric acid, adipic acid, sebacic acid, phthalic anhydride, maleic anhydride, methyl tetrahydrophthalic anhydride, maleic acid and dimer fatty acid.
3. The method for preparing the wet heat resistant high toughness modified unsaturated polyester solvent-free impregnating varnish according to claim 1, wherein the oil is one or more of linseed oil, tung oil and soybean oil.
4. The method for preparing the wet heat resistant high toughness modified unsaturated polyester solvent-free impregnating varnish according to claim 1, wherein the epoxy resin is one or more of bisphenol A type epoxy resin E20, epoxy resin E44 and epoxy resin E51.
5. The method for preparing the wet heat resistant high toughness modified unsaturated polyester solvent-free impregnating varnish according to claim 1, wherein the reactive diluent is one or more of vinyl toluene, 1, 4-butanediol diacrylate, diallyl phthalate, neopentyl glycol diacrylate and styrene.
6. The method for preparing the wet heat resistant high toughness modified unsaturated polyester solventless impregnating varnish as claimed in claim 1, wherein the curing agent is one or more of zinc isooctanoate, zinc naphthenate, cobalt naphthenate and calcium naphthenate; the initiator is one or more of dicumyl peroxide, tert-butyl peroxybenzoate and ethyl-3, 3-di (tert-butyl peroxybutyrate); the polymerization inhibitor is one or more of methyl hydroquinone, hydroquinone and 2, 5-di-tert-butyl hydroquinone.
7. The method for preparing the moisture-heat-resistant high-toughness modified unsaturated polyester solvent-free impregnating varnish according to claim 1, wherein in the step (1), the gradual temperature rise is performed by a temperature rise rate of 1.5-3.5 ℃/min; in the step (2), the pressure for vacuumizing is 100-500 Pa.
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