CN106967354A - A kind of corona resistance NCO unsaturated polyester (UP) impregnated insulating paint and preparation method thereof - Google Patents

A kind of corona resistance NCO unsaturated polyester (UP) impregnated insulating paint and preparation method thereof Download PDF

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Publication number
CN106967354A
CN106967354A CN201710259556.6A CN201710259556A CN106967354A CN 106967354 A CN106967354 A CN 106967354A CN 201710259556 A CN201710259556 A CN 201710259556A CN 106967354 A CN106967354 A CN 106967354A
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unsaturated polyester
parts
nanometer
nco
corona
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沈必亮
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Anhui Chunhui Instrument Cable Group Co Ltd
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Anhui Chunhui Instrument Cable Group Co Ltd
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Priority to CN201710259556.6A priority Critical patent/CN106967354A/en
Publication of CN106967354A publication Critical patent/CN106967354A/en
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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
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
    • C08G63/00—Macromolecular compounds obtained by reactions forming a carboxylic ester link in the main chain of the macromolecule
    • C08G63/68—Polyesters containing atoms other than carbon, hydrogen and oxygen
    • C08G63/685—Polyesters containing atoms other than carbon, hydrogen and oxygen containing nitrogen
    • C08G63/6854—Polyesters containing atoms other than carbon, hydrogen and oxygen containing nitrogen derived from polycarboxylic acids and polyhydroxy compounds
    • C08G63/6858—Polycarboxylic acids and polyhydroxy compounds in which at least one of the two components contains aliphatic unsaturation
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
    • C08G63/00—Macromolecular compounds obtained by reactions forming a carboxylic ester link in the main chain of the macromolecule
    • C08G63/78—Preparation processes
    • C08G63/82—Preparation processes characterised by the catalyst used
    • C08G63/85—Germanium, tin, lead, arsenic, antimony, bismuth, titanium, zirconium, hafnium, vanadium, niobium, tantalum, or compounds thereof
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K3/00—Use of inorganic substances as compounding ingredients
    • C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
    • C08K3/20—Oxides; Hydroxides
    • C08K3/22—Oxides; Hydroxides of metals
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K9/00—Use of pretreated ingredients
    • C08K9/04—Ingredients treated with organic substances
    • 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
    • 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
    • C09D7/61—Additives non-macromolecular inorganic
    • C09D7/62—Additives non-macromolecular inorganic modified by treatment with other compounds
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K3/00—Use of inorganic substances as compounding ingredients
    • C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
    • C08K3/20—Oxides; Hydroxides
    • C08K3/22—Oxides; Hydroxides of metals
    • C08K2003/2227—Oxides; Hydroxides of metals of aluminium
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K2201/00—Specific properties of additives
    • C08K2201/011—Nanostructured additives

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  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Health & Medical Sciences (AREA)
  • Medicinal Chemistry (AREA)
  • Polymers & Plastics (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Materials Engineering (AREA)
  • Wood Science & Technology (AREA)
  • Inorganic Chemistry (AREA)
  • Macromonomer-Based Addition Polymer (AREA)

Abstract

The invention discloses a kind of corona resistance NCO unsaturated polyester (UP) impregnated insulating paint, it is prepared first by nanometer Al2O3Activation process is carried out, 2,4 toluene di-isocyanate(TDI)s are reused by its isocyanate functional groupization, afterwards with isocyanation esterification modified Nano Al2O3It is Material synthesis unsaturated polyester (UP) with ethylene glycol, butanediol, phthalic anhydride, cis-butenedioic anhydride etc., isocyanates is introduced in unsaturated polyester (UP) segment, improve product air-drying property, while improves the corona-resistance property of product.The present invention is by isocyanation esterification modified Nano Al2O3It is introduced into unsaturated polyester (UP) segment, can effectively captures charged particle, forms stable space charge field, this space charge field is in material surface one equipotential surface of formation, external electric field can be effectively shielded, so that the corona-resistance property of material is improved, while improving the air-drying property of material.

Description

A kind of corona resistance NCO unsaturated polyester (UP) impregnated insulating paint and its preparation Method
Technical field
The present invention relates to a kind of impregnating varnish, and in particular to a kind of corona resistance NCO unsaturated polyester (UP) varnished insulation Paint and preparation method thereof.
Background technology
Unsaturated polyester (UP) impregnated insulating paint be used for impregnation process motor, electric apparatus coil, filling insulation system in gap and Micropore, and continuous paint film is formed on impregnated thing surface, and coil is bonded to a solid entirety, effectively improve insulation system The performance of the globality of system, thermal conductivity, moisture resistivity, dielectric strength and mechanical strength.
Unsaturated polyester (UP) is that occur Raolical polymerizable to realize solidification by styrene and its unsaturated double-bond, by Oxygen in air has strong inhibitory action to Raolical polymerizable（Anaerobism phenomenon）I.e. its air-drying property is poor, due to oxygen Inhibition, reacts incomplete on the resin surface of ingress of air, tacky phenomenon often occurs, have impact on the performance of paint film.
Chen Erfan, Fu Haijun et al. are at it《The research of unsaturated polyester (UP) air-drying property》In one text, by introducing " air-drying property base Group-NCO ", has synthesized the good unsaturated polyester (UP) of air-drying property, TDI tripolymers is introduced, because of its free isocyanate High activity, greatly reduces oxygen inhibition influence, the anaerobic of unsaturated polyester (UP) is solved, while the mechanical strength of material is also obtained Improve.
Under ac high frequency high pressure, the macromolecule of insulation paint film is also easy to produce partial ionization, when electric-field intensity reaches critical field Partial ionization can occur for Qiang Shi, neighbouring gas, blue-fluorescence electric discharge occur, while producing ozone.Prevent partial ionization and draw The paint film destruction risen, it is necessary to improve the formula of existing paint, introduces quantum shielding particle in paint based high molecular, and the electricity for improving paint is old Change performance, high voltage pulse is dispersed neutralizing, be unlikely to ionization and cause paint film to puncture.Included by adding inorganic filler TiO2、Al2O3、SiO2Deng, internal field and scattered heat are homogenized, so that the generation of shelf depreciation is prevented to a certain extent, To the effect for improving insulating materials corona-resistance property.
The content of the invention
In view of the shortcomings of the prior art, the present invention provides a kind of corona resistance NCO unsaturated polyester (UP) varnished insulation Paint and preparation method thereof.
A kind of corona resistance NCO unsaturated polyester (UP) impregnated insulating paint, it is prepared first by nanometer Al2O3Lived Change is handled, and 2,4- toluene di-isocyanate(TDI)s is reused by its isocyanate functional groupization, afterwards with isocyanation esterification modified Nano Al2O3It is Material synthesis unsaturated polyester (UP) with ethylene glycol, butanediol, phthalic anhydride, cis-butenedioic anhydride etc., introduces different in unsaturated polyester (UP) segment Cyanate, improves product air-drying property, while improving the corona-resistance property of product.
Comprise the following steps that：
（1）Nanometer Al2O3Activation process：
Take 7-14 parts by weight nanometer Al2O3In beaker, 100-200 parts of distilled water immersions are added, 8-18 parts of hydrochloric acid are added Mix ultrasound 10-18 minutes, stand 2 days, impurity of the absorption in particle surface is removed, then in 2000-5000r/min centrifugation Centrifuged 10-18 minutes in machine, centrifuge washing products therefrom is dried under vacuum to constant weight at 110-130 DEG C afterwards, lived Nanometer Al after change processing2O3, it is stand-by；
（2）Isocyanation esterification modified Nano Al2O3Preparation：
The nanometer Al added in three-necked flask after above-mentioned activated processing2O3, solvent is done with toluene, and in the protection of nitrogen Under, add 22-30 parts 2,4- toluene di-isocyanate(TDI)s, then in Ultrasound Instrument under the conditions of 40kHz ultrasound 25-45 minutes, make Nanometer Al2O3Spread out, after ultrasound is finished, then instill dibutyl tin laurate as catalyst, under nitrogen protection in Reacted 3-5 hours at 55-75 DEG C, the color of reaction solution gradually bleaches and no longer transparent；
（3）By 40-60 parts of maleic anhydrides, 10-20 parts of phthalic anhydrides, 25-35 parts of ethylene glycol, 15-20 parts of propane diols And 2-6 parts of p-methyl benzenesulfonic acid are added in the four-hole bottle equipped with a point water condenser, agitator, thermometer and nitrogen ingress pipe, are passed through Nitrogen, is heated to starting stirring after material melting, and is warming up to 140-160 DEG C, insulation reaction 1-2 hours, afterwards slow heating To 180-200 DEG C, continue insulation reaction until acid number reaches below 30mg/KOH；
（4）Then by step（3）Reaction mass is cooled to 100-130 DEG C, adds 2-5 parts of hydroquinones, treats that temperature is down to 100 DEG C 2-7 parts of styrene are added below, and above-mentioned isocyanation esterification modified Nano Al is added to less than 80 DEG C2O3, 20-40 points of stirring reaction Clock, stops stirring and discharging, ground slurry after cooling, filtering is produced.
Wherein, the step（2）The consumption of middle catalyst dibutyltin dilaurylate is the 0.02% of reaction system.
Wherein, the step（4）Middle ground slurry is to 20-40 μm.
Compared with prior art, the present invention has advantages below：
（1）The present invention soaks nanometer Al by using hydrochloric acid solution2O3, depart from the impurity of its adsorption, make surface hydroxyl naked Expose, can effectively solve the cluster states of nano-particle, redisperse is carried out under ultrasound condition, reach its size and receive Meter level scope, afterwards using the hydroxyl of nanoparticle surface, reacts with the contraposition isocyano of 2,4- toluene di-isocyanate(TDI)s, makes Nanometer Al2O3Surface grafting has isocyano, participates in the conjunction of unsaturated polyester (UP) using remaining unreacted ortho position isocyano afterwards Into reaction, isocyanate groups are introduced, because of the high activity of free isocyanate, the influence of oxygen is greatly reduced, improves material Air-drying property.
（2）The present invention is by nanometer Al2O3It is introduced into unsaturated polyester (UP) segment, by nanometer Al2O3It is homogeneously dispersed in matrix tree In fat, the chemical constitution of aluminum oxide has very strong corona resistance in itself, after adulterating in addition between nano-particle and resin matrix Special chemical structure of trap is formd, both, which act synergistically, can effectively capture charged particle, form stable space electricity Charged field, this space charge field can effectively shield external electric field, so as to improve in material surface one equipotential surface of formation The corona-resistance property of material.
Embodiment
A kind of corona resistance NCO unsaturated polyester (UP) impregnated insulating paint, it is prepared first by nanometer Al2O3Lived Change is handled, and 2,4- toluene di-isocyanate(TDI)s is reused by its isocyanate functional groupization, afterwards with isocyanation esterification modified Nano Al2O3It is Material synthesis unsaturated polyester (UP) with ethylene glycol, butanediol, phthalic anhydride, cis-butenedioic anhydride etc., introduces different in unsaturated polyester (UP) segment Cyanate, improves product air-drying property, while improving the corona-resistance property of product.
Comprise the following steps that：
（1）Nanometer Al2O3Activation process：
Take 10 parts by weight nanometer Al2O3In beaker, 120 parts of distilled water immersions are added, 9 parts of mixed in hydrochloric acid ultrasounds 15 are added Minute, 2 days are stood, impurity of the absorption in particle surface is removed, 15 points is then centrifuged in 4000r/min centrifuge Clock, centrifuge washing products therefrom is dried under vacuum to constant weight at 120 DEG C afterwards, obtains the nanometer Al after activation process2O3, treat With；
（2）Isocyanation esterification modified Nano Al2O3Preparation：
The nanometer Al added in three-necked flask after above-mentioned activated processing2O3, solvent is done with toluene, and in the protection of nitrogen Under, 28 parts of 2,4- toluene di-isocyanate(TDI)s are added, it is then ultrasonic 35 minutes under the conditions of 40kHz in Ultrasound Instrument, make nanometer Al2O3Spread out, after ultrasound is finished, then dibutyl tin laurate is instilled as catalyst, under nitrogen protection at 65 DEG C Reaction 4 hours, the color of reaction solution gradually bleaches and no longer transparent；
（3）By 55 parts of maleic anhydrides, 16 parts of phthalic anhydrides, 26 parts of ethylene glycol, 16 parts of propane diols and 5 parts to toluene sulphur Acid is added in the four-hole bottle equipped with a point water condenser, agitator, thermometer and nitrogen ingress pipe, is passed through nitrogen, is heated to material Start stirring after fusing, and be warming up to 150 DEG C, insulation reaction 1.5 hours is to slowly warm up to 190 DEG C afterwards, continues insulation reaction Until acid number reaches below 30mg/KOH；
（4）Then by step（3）Reaction mass is cooled to 120 DEG C, adds 3 parts of hydroquinones, treats that temperature is down to less than 100 DEG C and added Enter 5 parts of styrene, above-mentioned isocyanation esterification modified Nano Al is added to less than 80 DEG C2O3, stirring reaction 30 minutes, stopping stirring And discharge, ground slurry after cooling, filtering is produced.
Wherein, the step（2）The consumption of middle catalyst dibutyltin dilaurylate is the 0.02% of reaction system.
Wherein, the step（4）Middle ground slurry is to 20-40 μm.

Claims (4)

1. a kind of corona resistance NCO unsaturated polyester (UP) impregnated insulating paint, it is characterised in that it is prepared first by nanometer Al2O3Activation process is carried out, 2,4- toluene di-isocyanate(TDI)s are reused by its isocyanate functional groupization, afterwards with isocyanates Change modified Nano Al2O3It is Material synthesis unsaturated polyester (UP) with ethylene glycol, butanediol, phthalic anhydride, cis-butenedioic anhydride etc., in unsaturated polyester (UP) chain Isocyanates is introduced in section, product air-drying property is improved, while improving the corona-resistance property of product.
2. a kind of preparation side of corona resistance NCO unsaturated polyester (UP) impregnated insulating paint according to claims 1 Method, it is characterised in that comprise the following steps that：
（1）Nanometer Al2O3Activation process：
Take 7-14 parts by weight nanometer Al2O3In beaker, 100-200 parts of distilled water immersions are added, 8-18 parts of hydrochloric acid is added and mixes Close ultrasound 10-18 minutes, stand 2 days, impurity of the absorption in particle surface is removed, then in 2000-5000r/min centrifuge Middle centrifugation 10-18 minutes, centrifuge washing products therefrom is dried under vacuum to constant weight at 110-130 DEG C afterwards, activated Nanometer Al after processing2O3, it is stand-by；
（2）Isocyanation esterification modified Nano Al2O3Preparation：
The nanometer Al added in three-necked flask after above-mentioned activated processing2O3, solvent is done with toluene, and under the protection of nitrogen, Add 22-30 parts 2,4- toluene di-isocyanate(TDI)s, then in Ultrasound Instrument under the conditions of 40kHz ultrasound 25-45 minutes, make nanometer Al2O3Spread out, after ultrasound is finished, then dibutyl tin laurate is instilled as catalyst, under nitrogen protection in 55-75 Reacted 3-5 hours at DEG C, the color of reaction solution gradually bleaches and no longer transparent；
（3）By 40-60 parts of maleic anhydrides, 10-20 parts of phthalic anhydrides, 25-35 parts of ethylene glycol, 15-20 parts of propane diols And 2-6 parts of p-methyl benzenesulfonic acid are added in the four-hole bottle equipped with a point water condenser, agitator, thermometer and nitrogen ingress pipe, are passed through Nitrogen, is heated to starting stirring after material melting, and is warming up to 140-160 DEG C, insulation reaction 1-2 hours, afterwards slow heating To 180-200 DEG C, continue insulation reaction until acid number reaches below 30mg/KOH；
（4）Then by step（3）Reaction mass is cooled to 100-130 DEG C, adds 2-5 parts of hydroquinones, treats that temperature is down to 100 DEG C 2-7 parts of styrene are added below, and above-mentioned isocyanation esterification modified Nano Al is added to less than 80 DEG C2O3, 20-40 points of stirring reaction Clock, stops stirring and discharging, ground slurry after cooling, filtering is produced.
3. a kind of preparation side of corona resistance NCO unsaturated polyester (UP) impregnated insulating paint according to claims 2 Method, it is characterised in that the step（2）The consumption of middle catalyst dibutyltin dilaurylate is the 0.02% of reaction system.
4. a kind of preparation of corona resistance NCO unsaturated polyester (UP) impregnated insulating paint according to claims 1,2 Method, it is characterised in that the step（4）Middle ground slurry is to 20-40 μm.
CN201710259556.6A 2017-04-20 2017-04-20 A kind of corona resistance NCO unsaturated polyester (UP) impregnated insulating paint and preparation method thereof Pending CN106967354A (en)

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Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1454931A (en) * 2002-04-30 2003-11-12 章浩龙 Method of preparing unsaturated polyester resin nano composite material
CN1793221A (en) * 2005-11-25 2006-06-28 南京理工大学 Process for preparing superfine oxide polyformol engineering plastic
CN102942839A (en) * 2012-12-11 2013-02-27 广州贝特新材料有限公司 Nanofiller modified solvent-free insulating paint and preparation method thereof
CN104744988A (en) * 2015-04-15 2015-07-01 合肥学院 Preparation method of nanometer aluminum oxide (AL2O3) dispersoid for improving wear-resisting property of polyurethane paint and preparation method of super wear-resisting polyurethane paint

Patent Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1454931A (en) * 2002-04-30 2003-11-12 章浩龙 Method of preparing unsaturated polyester resin nano composite material
CN1793221A (en) * 2005-11-25 2006-06-28 南京理工大学 Process for preparing superfine oxide polyformol engineering plastic
CN102942839A (en) * 2012-12-11 2013-02-27 广州贝特新材料有限公司 Nanofiller modified solvent-free insulating paint and preparation method thereof
CN104744988A (en) * 2015-04-15 2015-07-01 合肥学院 Preparation method of nanometer aluminum oxide (AL2O3) dispersoid for improving wear-resisting property of polyurethane paint and preparation method of super wear-resisting polyurethane paint

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