CN107903774A - A kind of flame retardant type wire enamel - Google Patents
A kind of flame retardant type wire enamel Download PDFInfo
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- CN107903774A CN107903774A CN201711104726.XA CN201711104726A CN107903774A CN 107903774 A CN107903774 A CN 107903774A CN 201711104726 A CN201711104726 A CN 201711104726A CN 107903774 A CN107903774 A CN 107903774A
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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
- C09D167/02—Polyesters derived from dicarboxylic acids and dihydroxy compounds
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- 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
- C08G63/02—Polyesters derived from hydroxycarboxylic acids or from polycarboxylic acids and polyhydroxy compounds
- C08G63/12—Polyesters derived from hydroxycarboxylic acids or from polycarboxylic acids and polyhydroxy compounds derived from polycarboxylic acids and polyhydroxy compounds
- C08G63/16—Dicarboxylic acids and dihydroxy compounds
- C08G63/18—Dicarboxylic acids and dihydroxy compounds the acids or hydroxy compounds containing carbocyclic rings
- C08G63/181—Acids containing aromatic rings
- C08G63/183—Terephthalic acids
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- 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
- C08G63/91—Polymers modified by chemical after-treatment
- C08G63/914—Polymers modified by chemical after-treatment derived from polycarboxylic acids and polyhydroxy compounds
- C08G63/916—Dicarboxylic acids and dihydroxy compounds
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- 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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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01B—CABLES; CONDUCTORS; INSULATORS; SELECTION OF MATERIALS FOR THEIR CONDUCTIVE, INSULATING OR DIELECTRIC PROPERTIES
- H01B3/00—Insulators or insulating bodies characterised by the insulating materials; Selection of materials for their insulating or dielectric properties
- H01B3/18—Insulators or insulating bodies characterised by the insulating materials; Selection of materials for their insulating or dielectric properties mainly consisting of organic substances
- H01B3/30—Insulators or insulating bodies characterised by the insulating materials; Selection of materials for their insulating or dielectric properties mainly consisting of organic substances plastics; resins; waxes
- H01B3/308—Wires with resins
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Abstract
The invention discloses a kind of flame retardant type wire enamel, belong to technical field of coatings.The flame retardant type wire enamel that the present invention develops includes matrix resin, solvent, auxiliary agent, diluent and filler, wherein matrix resin is by after self-control polyester resin, self-control imine biatomic acid and the reaction of silane coupling agent high-temperature stirring, product and polyallylamine are mixed to get, it is to react to obtain by dimethyl terephthalate (DMT), Sai Ke, ethylene glycol and dimethylbenzene to make polyester resin by oneself, and self-control imine biatomic acid is to react to obtain by trimellitic anhydride and 4 ' 4 diaminodiphenylmethane；And auxiliary agent is then by silane coupling agent KH 570, ether, ethyl orthosilicate and butyl titanate composition；In addition, filler mixes for modified meerschaum and sodium acid carbonate.Flame retardant type wire enamel prepared by technical solution of the present invention has the characteristics that excellent fire resistance and film forming stability.
Description
Technical field
The invention discloses a kind of flame retardant type wire enamel, belong to technical field of coatings.
Background technology
With the raising of economy and living standards of the people, wire enamel is all increasing rapidly in military and people's livelihood field demand
It is long.The wire enamel on plain conductor surface forms insulating protective layer after high temperature bakees in wire surface, due to the technique system
Simplicity is made, insulation thickness is moderate, advantageous etc. in terms of shaping, is had a wide range of applications in fields such as electrician, electronics, electric appliances.Make
For a kind of excellent coating of electrical insulation capability, wire enamel is essential material in electrical equipment, its quality direct relation
To the economic and technical norms and service life of electrical equipment.Since electrical equipment and electrical is towards small, high-power trend development, and line
Circle can produce big heat in operation, therefore the temperature classification requirement to insulating materials is higher and higher, and nuclear power and universe
The development of space technology proposes winding wire harsher high temperature resistant requirement, meanwhile, the mechanization of winding and high speed process
It is required that winding wire has good surface property.Enameled wire is made of bare conductor and the insulation paint film two parts being coated on outside it,
By applying coil is coiled into after line dip-coating binding resin is bonded together each circle conducting wire again.Quality, the technique of wire enamel performance
The stabilization of the size of nargin and quality or not it can all directly affect the performance of enameled wire.In production of enamel wire process and motor
Can be produced in electric operation various complicated mechanical stresses such as rub, bend, stretching, compressing, impact stress, so paint
Film should have elasticity and pliability.In addition, paint film will also be amenable to thermal shocking and heat, electricity, mechanical stress under stress state
Synergy.Therefore, the stability after its film forming also becomes focus of attention.In addition, enameled wire is widely used in
In household electrical appliance, its security and people's daily life are closely bound up.Although fire incident occurs for many household electrical appliance
Completely as caused by enameled wire, but the material that household electrical appliances manufacturer uses it proposes non-ignitable or fire retardant requirement including enameled wire
The surface insulation processing mode of plain conductor generally has wrapped film, wrapped mica tape and surface coating insulated paint etc..
Therefore, it is the shortcomings that how improving traditional wire enamel fire resistance and bad film forming stability, comprehensive to obtain higher
The wire enamel of performance is closed, is that it is promoted and applies, meets industrial production demand urgent problem to be solved.
The content of the invention
The present invention solves the technical problem of：It is bad for traditional wire enamel fire resistance and film forming stability
A kind of shortcoming, there is provided flame retardant type wire enamel.
In order to solve the above-mentioned technical problem, the technical solution adopted in the present invention is：
A kind of flame retardant type wire enamel, includes the raw material composition of following parts by weight：
30~40 parts of matrix resin
60~80 parts of solvent
10~15 parts of auxiliary agent
10~20 parts of diluent
8~10 parts of filler
It is characterized in that：
Described matrix resin preparation process is：
（1）Count in parts by weight, take 20~30 parts of dimethyl terephthalate (DMT)s, 8~10 parts of matches gram, 20~30 parts of second two successively
Alcohol, 13~15 parts of dimethylbenzene, high-temperature stirring is reacted after mixing, obtains polyester resin；
（2）It is 1 in mass ratio：1~3：After 1 mixes trimellitic anhydride and 4 ' 4- diaminodiphenylmethane, heating stirring reaction,
Obtain imine biatomic acid；
（3）Count in parts by weight, take 40~50 parts of polyester resin successively, 20~30 parts of imine biatomic acids, 4~8 parts silane coupled
Agent, high-temperature stirring reaction, obtains polyester imine resin, and is 10 in mass ratio by gained polyester imine resin and polyallylamine：1~
20：1 mixing, up to matrix resin；
The auxiliary agent is made of following parts by weight raw material：8~10 parts of Silane coupling reagent KH-570s, 0.3~0.5 part of ether,
20~30 parts of ethyl orthosilicates, 8~10 parts of butyl titanates；
The filler is that modified meerschaum and calcium bicarbonate are 10 in mass ratio：1~15：1 mixes.
The solvent is any one or two kinds of mixtures in toluene, dimethylbenzene and cresols.
The diluent is by acetone and dimethicone is 3 in mass ratio：1~5：1 configuration forms.
Step（3）The silane coupling agent is silane resin acceptor kh-550, silane coupling agent KH-560 or silane coupling agent
Any one in KH-570.
The modified meerschaum modifying process is：It is 1 in mass ratio by sepiolite and hydrochloric acid：10~1：It is permanent after 20 mixing
Temperature stirring reaction, filtering, washing, dry, roasting, obtains modified meerschaum.
The beneficial effects of the invention are as follows：
（1）Technical solution of the present invention in system by adding modified meerschaum and calcium bicarbonate, as filler systems, Liang Zhe
Under hot conditions, calcium bicarbonate is decomposed first produces carbon dioxide and water, plays the role of tentatively isolating oxygen, so as to rise
To flame retardant effect, in addition, the part silane coupling agent disperseed in system can be contacted with water and hydrolyzed, and high temperature can further promote
Into its hydrolysis generation silanol, generation siloxanes is dehydrated each other in enamelled wire surface after silanol spilling, so as to by sepiolite and divide
The calcium carbonate that solution produces is fixed on enamelled wire surface, further improves that system is fire-retardant and smoke suppressing effect；
（2）The many places of silane coupling agent use in technical solution of the present invention, can play different-effect, can improve inorganic filler first
With the compatibility of matrix resin, while avoiding inorganic filler from too reuniting, it is set to be well dispersed in resin matrix, so that
Raising system mechanical property, secondly, the silane coupling agent added in matrix resin preparation process can be played to matrix resin
Modifying function, so that adulterating soft segment in rigid matrix resin strand, the presence of soft segment can make inside system
Certain locomitivity is kept, product wire enamel is had rigidity and flexibility concurrently, so that product can be good in enamelled wire surface
Film forming, so as to further improve product film forming stability.
Embodiment
It is 1 in mass ratio：10~1：20 pour into sepiolite and mass fraction in beaker for 8~10% mixed in hydrochloric acid, and will
Beaker moves into digital display and tests the speed constant temperature blender with magnetic force, in temperature be 65~75 DEG C, it is permanent under the conditions of rotating speed is 600~800r/min
After 45~60min of temperature stirring reaction, filtering, obtains filter cake, and filter cake is washed with deionized 3~5 times, then by the filter cake after washing
It is transferred in baking oven, is dried under the conditions of being 105~110 DEG C in temperature to constant weight, obtain dry cake, then gained dry cake is transferred to
Tube furnace, under the conditions of temperature is 280~300 DEG C, insulation 1~2h of roasting, cools to room temperature with the furnace, discharges, obtain modified Hai Pao
Stone；It is again 10 in mass ratio by modified meerschaum and calcium bicarbonate：1~15：1 is stirred 45~60min, obtains filler；By weight
Number meter is measured, takes 20~30 parts of dimethyl terephthalate (DMT)s successively, 8~10 parts of matches gram, 20~30 parts of ethylene glycol, 13~15 part two
No. 1 three-necked flask is poured into toluene, mixing, and No. 1 three-necked flask is moved into digital display and is tested the speed constant temperature blender with magnetic force, is in temperature
150~170 DEG C, under the conditions of rotating speed is 400~500r/min, high-temperature stirring reacts 3~5h, and discharging, obtains polyester resin；By quality
Than for 1：1~3：Trimellitic anhydride and 4 ' 4- diaminodiphenylmethane are poured into No. 2 three-necked flasks by 1, and No. 2 three-necked flasks are moved
Enter digital display to test the speed constant temperature blender with magnetic force, in temperature be 80~90 DEG C, under the conditions of rotating speed is 400~600r/min, constant temperature stirring
2~4h is reacted, discharging, obtains imine biatomic acid；Count in parts by weight, take 40~50 parts of polyester resin, 20~30 parts of imines successively
Binary acid, 4~8 parts of silane coupling agents pour into No. 3 three-necked flasks, and No. 3 three-necked flasks are moved into the digital displays constant temperature magnetic force that tests the speed and are stirred
Device is mixed, is 175~180 DEG C in temperature, under the conditions of rotating speed is 600~800r/min, high-temperature stirring reacts 3~5h, and discharging, obtains poly-
Ester imide resin, then by gained polyester imine resin and polyallylamine be 10 in mass ratio：1~20：Batch mixer is poured into 1 mixing,
Under the conditions of rotating speed is 800~1200r/min, 2~4h is stirred, discharges, obtains matrix resin；Count in parts by weight, successively
30~40 parts of matrix resins are taken, 60~80 parts of solvents, 10~15 parts of auxiliary agents, 10~20 parts of diluents, 8~10 parts of fillers, first will
Matrix resin, solvent, auxiliary agent and diluent pour into batch mixer, and under the conditions of rotating speed is 1800~2000r/min, high-speed stirred is mixed
2~4h is closed, adds filler, continues high-speed stirred and mixes 3~5h, discharging is filling, up to flame retardant type wire enamel.It is described to help
Agent is made of following parts by weight raw material：8~10 parts of Silane coupling reagent KH-570s, 0.3~0.5 part of ether, 20~30 parts just
Silester, 8~10 parts of butyl titanates.The solvent is any one or two kinds of mixing in toluene, dimethylbenzene and cresols
Thing.The diluent is by acetone and dimethicone is 3 in mass ratio：1~5：1 configuration forms.The silane coupling agent is
Any one in silane resin acceptor kh-550, silane coupling agent KH-560 or Silane coupling reagent KH-570.
Example 1
It is 1 in mass ratio：20 pour into sepiolite and mass fraction in beaker for 10% mixed in hydrochloric acid, and beaker is moved into digital display
Test the speed constant temperature blender with magnetic force, in temperature be 75 DEG C, rotating speed be 800r/min under the conditions of, constant temperature stirring reaction 60min after, mistake
Filter, obtains filter cake, and filter cake is washed with deionized 5 times, then the filter cake after washing is transferred in baking oven, in temperature be 110 DEG C of bars
Dried under part to constant weight, obtain dry cake, then gained dry cake is transferred to tube furnace, under the conditions of temperature is 300 DEG C, insulation
2h is roasted, cools to room temperature with the furnace, discharges, obtains modified meerschaum；It is again 15 in mass ratio by modified meerschaum and calcium bicarbonate：
1 is stirred 60min, obtains filler；Count in parts by weight, take 30 parts of dimethyl terephthalate (DMT)s, 10 parts of matches gram, 30 parts of second successively
No. 1 three-necked flask is poured into glycol, 15 parts of dimethylbenzene, mixing, and No. 1 three-necked flask is moved into digital display and is tested the speed temperature constant magnetic stirring
Device, is 170 DEG C in temperature, under the conditions of rotating speed is 500r/min, high-temperature stirring reaction 5h, discharging, obtains polyester resin；In mass ratio
For 3：Trimellitic anhydride and 4 ' 4- diaminodiphenylmethane are poured into No. 2 three-necked flasks by 1, and No. 2 three-necked flasks are moved into digital display
Test the speed constant temperature blender with magnetic force, is 90 DEG C in temperature, under the conditions of rotating speed is 600r/min, constant temperature stirring reaction 4h, discharging, obtains sub-
Amine binary acid；Count in parts by weight, take 50 parts of polyester resin successively, 30 parts of imine biatomic acids, 8 parts of silane coupling agents, pour into No. 3
Three-necked flask, and No. 3 three-necked flasks are moved into digital displays and are tested the speed constant temperature blender with magnetic force, in temperature be 180 DEG C, rotating speed 800r/
Under the conditions of min, high-temperature stirring reaction 5h, discharging, obtains polyester imine resin, then gained polyester imine resin and polyallylamine are pressed
Mass ratio is 20：Batch mixer is poured into 1 mixing, under the conditions of rotating speed is 1200r/min, is stirred 4h, discharges, obtain matrix tree
Fat；Count in parts by weight, take 40 parts of matrix resins successively, 80 parts of solvents, 15 parts of auxiliary agents, 20 parts of diluents, 10 parts of fillers, first will
Matrix resin, solvent, auxiliary agent and diluent pour into batch mixer, under the conditions of rotating speed is 2000r/min, high-speed stirred mixing 4h,
Filler is added, continues high-speed stirred mixing 5h, discharging is filling, up to flame retardant type wire enamel.The auxiliary agent is by following heavy
Measure number raw material composition：10 parts of Silane coupling reagent KH-570s, 0.5 part of ether, 30 parts of ethyl orthosilicates, 10 parts of butyl titanates.
The solvent is toluene.The diluent is by acetone and dimethicone is 5 in mass ratio：1 configuration forms.The silane is even
Connection agent is silane resin acceptor kh-550.
Example 2
It is again 15 in mass ratio by sepiolite and calcium bicarbonate：1 is stirred 60min, obtains filler；Count in parts by weight, successively
30 parts of dimethyl terephthalate (DMT)s are taken, 10 parts of matches gram, 30 parts of ethylene glycol, 15 parts of dimethylbenzene, mix and pour into No. 1 three-necked flask, and
No. 1 three-necked flask is moved into digital display to test the speed constant temperature blender with magnetic force, in temperature be 170 DEG C, it is high under the conditions of rotating speed is 500r/min
Temperature stirring reaction 5h, discharging, obtains polyester resin；It is 3 in mass ratio：1 falls trimellitic anhydride and 4 ' 4- diaminodiphenylmethane
Enter No. 2 three-necked flasks, and No. 2 three-necked flasks are moved into digital displays and are tested the speed constant temperature blender with magnetic force, be 90 DEG C in temperature, rotating speed is
Under the conditions of 600r/min, constant temperature stirring reaction 4h, discharging, obtains imine biatomic acid；Count in parts by weight, take 50 parts of polyester trees successively
Fat, 30 parts of imine biatomic acids, 8 parts of silane coupling agents pour into No. 3 three-necked flasks, and No. 3 three-necked flasks are moved into digital displays and are tested the speed perseverance
Warm magnetic stirring apparatus, is 180 DEG C in temperature, under the conditions of rotating speed is 800r/min, high-temperature stirring reaction 5h, discharging, obtains polyester Asia
Polyimide resin, then by gained polyester imine resin and polyallylamine be 20 in mass ratio：Batch mixer is poured into 1 mixing, is in rotating speed
Under the conditions of 1200r/min, 4h is stirred, discharges, obtains matrix resin；Count in parts by weight, take 40 parts of matrix resins successively, 80
Part solvent, 15 parts of auxiliary agents, 20 parts of diluents, 10 parts of fillers, first pour into batch mixer by matrix resin, solvent, auxiliary agent and diluent,
Under the conditions of rotating speed is 2000r/min, high-speed stirred mixing 4h, adds filler, continues high-speed stirred mixing 5h, discharges, fill
Dress, up to flame retardant type wire enamel.The auxiliary agent is made of following parts by weight raw material：10 parts of Silane coupling reagent KH-570s,
0.5 part of ether, 30 parts of ethyl orthosilicates, 10 parts of butyl titanates.The solvent is toluene.The diluent be by acetone and two
Methyl-silicone oil is 5 in mass ratio：1 configuration forms.The silane coupling agent is silane resin acceptor kh-550.
Example 3
It is 1 in mass ratio：20 pour into sepiolite and mass fraction in beaker for 10% mixed in hydrochloric acid, and beaker is moved into digital display
Test the speed constant temperature blender with magnetic force, in temperature be 75 DEG C, rotating speed be 800r/min under the conditions of, constant temperature stirring reaction 60min after, mistake
Filter, obtains filter cake, and filter cake is washed with deionized 5 times, then the filter cake after washing is transferred in baking oven, in temperature be 110 DEG C of bars
Dried under part to constant weight, obtain dry cake, then gained dry cake is transferred to tube furnace, under the conditions of temperature is 300 DEG C, insulation
2h is roasted, cools to room temperature with the furnace, discharges, modified meerschaum is obtained, up to filler；Count in parts by weight, take 30 parts successively to benzene
Dicarboxylic acid dimethyl ester, 10 parts of matches gram, 30 parts of ethylene glycol, 15 parts of dimethylbenzene, No. 1 three-necked flask is poured into mixing, and No. 1 three mouthfuls are burnt
Bottle moves into digital display and tests the speed constant temperature blender with magnetic force, in temperature be 170 DEG C, under the conditions of rotating speed is 500r/min, high-temperature stirring reaction
5h, discharging, obtains polyester resin；It is 3 in mass ratio：Trimellitic anhydride and 4 ' 4- diaminodiphenylmethane are poured into No. 2 three mouthfuls of burnings by 1
Bottle, and No. 2 three-necked flasks are moved into digital displays and are tested the speed constant temperature blender with magnetic force, it is 90 DEG C in temperature, rotating speed is 600r/min conditions
Under, constant temperature stirring reaction 4h, discharging, obtains imine biatomic acid；Count in parts by weight, take 50 parts of polyester resin, 30 parts of imines successively
Binary acid, 8 parts of silane coupling agents pour into No. 3 three-necked flasks, and No. 3 three-necked flasks are moved into digital displays and are tested the speed temperature constant magnetic stirring
Device, is 180 DEG C in temperature, under the conditions of rotating speed is 800r/min, high-temperature stirring reaction 5h, discharging, obtains polyester imine resin, then will
Gained polyester imine resin and polyallylamine are 20 in mass ratio：1 mixing pour into batch mixer, in rotating speed be 1200r/min conditions
Under, 4h is stirred, discharges, obtains matrix resin；Count in parts by weight, take 40 parts of matrix resins successively, 80 parts of solvents, 15 parts are helped
Agent, 20 parts of diluents, 10 parts of fillers, first pour into batch mixer by matrix resin, solvent, auxiliary agent and diluent, are in rotating speed
Under the conditions of 2000r/min, high-speed stirred mixing 4h, adds filler, continues high-speed stirred mixing 5h, and discharging is filling, up to hindering
Combustion type wire enamel.The auxiliary agent is made of following parts by weight raw material：10 parts of Silane coupling reagent KH-570s, 0.5 part of ether,
30 parts of ethyl orthosilicates, 10 parts of butyl titanates.The solvent is toluene.The diluent be by acetone and dimethicone by
Mass ratio is 5：1 configuration forms.The silane coupling agent is silane resin acceptor kh-550.
Example 4
It is 1 in mass ratio：20 pour into sepiolite and mass fraction in beaker for 10% mixed in hydrochloric acid, and beaker is moved into digital display
Test the speed constant temperature blender with magnetic force, in temperature be 75 DEG C, rotating speed be 800r/min under the conditions of, constant temperature stirring reaction 60min after, mistake
Filter, obtains filter cake, and filter cake is washed with deionized 5 times, then the filter cake after washing is transferred in baking oven, in temperature be 110 DEG C of bars
Dried under part to constant weight, obtain dry cake, then gained dry cake is transferred to tube furnace, under the conditions of temperature is 300 DEG C, insulation
2h is roasted, cools to room temperature with the furnace, discharges, obtains modified meerschaum；It is again 15 in mass ratio by modified meerschaum and calcium bicarbonate：
1 is stirred 60min, obtains filler；Count in parts by weight, take 30 parts of dimethyl terephthalate (DMT)s, 10 parts of matches gram, 30 parts of second successively
No. 1 three-necked flask is poured into glycol, 15 parts of dimethylbenzene, mixing, and No. 1 three-necked flask is moved into digital display and is tested the speed temperature constant magnetic stirring
Device, is 170 DEG C in temperature, under the conditions of rotating speed is 500r/min, high-temperature stirring reaction 5h, discharging, obtains polyester resin；In mass ratio
For 3：Trimellitic anhydride and 4 ' 4- diaminodiphenylmethane are poured into No. 2 three-necked flasks by 1, and No. 2 three-necked flasks are moved into digital display
Test the speed constant temperature blender with magnetic force, is 90 DEG C in temperature, under the conditions of rotating speed is 600r/min, constant temperature stirring reaction 4h, discharging, obtains sub-
Amine binary acid；To count in parts by weight, take 50 parts of polyester resin successively, 30 parts of imine biatomic acids pour into No. 3 three-necked flasks, and by 3
Number three-necked flask moves into digital display and tests the speed constant temperature blender with magnetic force, in temperature be 180 DEG C, under the conditions of rotating speed is 800r/min, high temperature
Stirring reaction 5h, discharging, obtains polyester imine resin, then by gained polyester imine resin and polyallylamine is 20 in mass ratio：1 is mixed
Batch mixer is poured into conjunction, under the conditions of rotating speed is 1200r/min, is stirred 4h, discharges, obtain matrix resin；Count in parts by weight,
Take 40 parts of matrix resins successively, 80 parts of solvents, 15 parts of auxiliary agents, 20 parts of diluents, 10 parts of fillers, first by matrix resin, solvent, help
Agent and diluent pour into batch mixer, and under the conditions of rotating speed is 2000r/min, high-speed stirred mixing 4h, adds filler, continue high
Speed is stirred 5h, discharging, filling, up to flame retardant type wire enamel.The auxiliary agent is made of following parts by weight raw material：10
Part Silane coupling reagent KH-570,0.5 part of ether, 30 parts of ethyl orthosilicates, 10 parts of butyl titanates.The solvent is toluene.Institute
State diluent be by acetone and dimethicone in mass ratio be 5：1 configuration forms.
Example 5
It is 1 in mass ratio：20 pour into sepiolite and mass fraction in beaker for 10% mixed in hydrochloric acid, and beaker is moved into digital display
Test the speed constant temperature blender with magnetic force, in temperature be 75 DEG C, rotating speed be 800r/min under the conditions of, constant temperature stirring reaction 60min after, mistake
Filter, obtains filter cake, and filter cake is washed with deionized 5 times, then the filter cake after washing is transferred in baking oven, in temperature be 110 DEG C of bars
Dried under part to constant weight, obtain dry cake, then gained dry cake is transferred to tube furnace, under the conditions of temperature is 300 DEG C, insulation
2h is roasted, cools to room temperature with the furnace, discharges, obtains modified meerschaum；It is again 15 in mass ratio by modified meerschaum and calcium bicarbonate：
1 is stirred 60min, obtains filler；Count in parts by weight, take 30 parts of dimethyl terephthalate (DMT)s, 10 parts of matches gram, 30 parts of second successively
No. 1 three-necked flask is poured into glycol, 15 parts of dimethylbenzene, mixing, and No. 1 three-necked flask is moved into digital display and is tested the speed temperature constant magnetic stirring
Device, is 170 DEG C in temperature, under the conditions of rotating speed is 500r/min, high-temperature stirring reaction 5h, discharging, obtains polyester resin；In mass ratio
For 3：Trimellitic anhydride and 4 ' 4- diaminodiphenylmethane are poured into No. 2 three-necked flasks by 1, and No. 2 three-necked flasks are moved into digital display
Test the speed constant temperature blender with magnetic force, is 90 DEG C in temperature, under the conditions of rotating speed is 600r/min, constant temperature stirring reaction 4h, discharging, obtains sub-
Amine binary acid；Count in parts by weight, take 50 parts of polyester resin successively, 30 parts of imine biatomic acids, 8 parts of silane coupling agents, pour into No. 3
Three-necked flask, and No. 3 three-necked flasks are moved into digital displays and are tested the speed constant temperature blender with magnetic force, in temperature be 180 DEG C, rotating speed 800r/
Under the conditions of min, high-temperature stirring reaction 5h, discharging, obtains polyester imine resin, then gained polyester imine resin and polyallylamine are pressed
Mass ratio is 20：Batch mixer is poured into 1 mixing, under the conditions of rotating speed is 1200r/min, is stirred 4h, discharges, obtain matrix tree
Fat；Count in parts by weight, take 40 parts of matrix resins successively, 80 parts of solvents, 15 parts of auxiliary agents, 20 parts of diluents, 10 parts of fillers, first will
Matrix resin, solvent, auxiliary agent and diluent pour into batch mixer, under the conditions of rotating speed is 2000r/min, high-speed stirred mixing 4h,
Filler is added, continues high-speed stirred mixing 5h, discharging is filling, up to flame retardant type wire enamel.The auxiliary agent is by following heavy
Measure number raw material composition：10 parts of Silane coupling reagent KH-570s, 0.5 part of ether.The solvent is toluene.The diluent is by third
Ketone and dimethicone are 5 in mass ratio：1 configuration forms.The silane coupling agent is silane resin acceptor kh-550.
Comparative example：The wire enamel of Guangdong new material Co., Ltd production.
The flame retardant type wire enamel of the gained of example 1 to 5 and comparative example product are subjected to performance detection, specific detection method is such as
Under：
1. fire resistance：Test specimen fire resistance is detected according to ZBG51001, detects the test specimen resistance to combustion time；
Specific testing result is as shown in table 1：
2. film forming stability：Test specimen minimum scraping force is detected according to GB/T6109.22；
Table 1
| Detection project | Example 1 | Example 2 | Example 3 | Example 4 | Example 5 | Comparative example |
| Resistance to combustion time/min | 160 | 105 | 88 | 83 | 74 | 13 |
| Minimum scraping force/N | 4.31 | 3.85 | 3.14 | 2.84 | 2.79 | 2.65 |
From 1 testing result of table, flame retardant type wire enamel prepared by technical solution of the present invention have excellent fire resistance and
The characteristics of film forming stability, have broad prospects in the development of wire enamel industry.
Claims (5)
- A kind of 1. flame retardant type wire enamel, it is characterised in that the raw material composition including following parts by weight：30~40 parts of matrix resin60~80 parts of solvent10~15 parts of auxiliary agent10~20 parts of diluent8~10 parts of fillerIt is characterized in that：Described matrix resin preparation process is：（1）Count in parts by weight, take 20~30 parts of dimethyl terephthalate (DMT)s, 8~10 parts of matches gram, 20~30 parts of second two successively Alcohol, 13~15 parts of dimethylbenzene, high-temperature stirring is reacted after mixing, obtains polyester resin；（2）It is 1 in mass ratio：1~3：After 1 mixes trimellitic anhydride and 4 ' 4- diaminodiphenylmethane, heating stirring reaction, Obtain imine biatomic acid；（3）Count in parts by weight, take 40~50 parts of polyester resin successively, 20~30 parts of imine biatomic acids, 4~8 parts silane coupled Agent, high-temperature stirring reaction, obtains polyester imine resin, and is 10 in mass ratio by gained polyester imine resin and polyallylamine：1~ 20：1 mixing, up to matrix resin；The auxiliary agent is made of following parts by weight raw material：8~10 parts of Silane coupling reagent KH-570s, 0.3~0.5 part of ether, 20~30 parts of ethyl orthosilicates, 8~10 parts of butyl titanates；The filler is that modified meerschaum and calcium bicarbonate are 10 in mass ratio：1~15：1 mixes.
- A kind of 2. flame retardant type wire enamel according to claim 1, it is characterised in that：The solvent is toluene, dimethylbenzene With any one in cresols or two kinds of mixtures.
- A kind of 3. flame retardant type wire enamel according to claim 1, it is characterised in that：The diluent be by acetone and two Methyl-silicone oil is 3 in mass ratio：1~5：1 configuration forms.
- A kind of 4. flame retardant type wire enamel according to claim 1, it is characterised in that：Step（3）The silane coupling agent Any one for silane resin acceptor kh-550, in silane coupling agent KH-560 or Silane coupling reagent KH-570.
- A kind of 5. flame retardant type wire enamel according to claim 1, it is characterised in that：The modified meerschaum modifying process For：It is 1 in mass ratio by sepiolite and hydrochloric acid：10~1：After 20 mixing, constant temperature stirring reaction, filtering, washing, dry, roasting, Obtain modified meerschaum.
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| CN109096887A (en) * | 2018-08-01 | 2018-12-28 | 江苏恒兴制漆有限公司 | A kind of dual purpose polyester wire enamel and preparation method thereof |
| CN109535889A (en) * | 2018-11-01 | 2019-03-29 | 惠州市三民实业有限公司 | A kind of fireproof coating and preparation method thereof |
| CN112011218A (en) * | 2020-10-07 | 2020-12-01 | 赵元梅 | Novel environment-friendly odorless printing ink and preparation method thereof |
| CN113257479A (en) * | 2021-05-15 | 2021-08-13 | 江西华尔达线缆股份有限公司 | Novel polyesterimide enameled wire and preparation method thereof |
| CN113292909A (en) * | 2021-05-22 | 2021-08-24 | 江西华尔达线缆股份有限公司 | Moisture-resistant polyester enameled wire and preparation method thereof |
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| CN109096887A (en) * | 2018-08-01 | 2018-12-28 | 江苏恒兴制漆有限公司 | A kind of dual purpose polyester wire enamel and preparation method thereof |
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| CN113292909A (en) * | 2021-05-22 | 2021-08-24 | 江西华尔达线缆股份有限公司 | Moisture-resistant polyester enameled wire and preparation method thereof |
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Application publication date: 20180413 |