CN109337572A - A kind of new-energy automobile anti-flaming dope and preparation method thereof - Google Patents
A kind of new-energy automobile anti-flaming dope and preparation method thereof Download PDFInfo
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- CN109337572A CN109337572A CN201811008830.3A CN201811008830A CN109337572A CN 109337572 A CN109337572 A CN 109337572A CN 201811008830 A CN201811008830 A CN 201811008830A CN 109337572 A CN109337572 A CN 109337572A
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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
- C09D179/00—Coating compositions based on macromolecular compounds obtained by reactions forming in the main chain of the macromolecule a linkage containing nitrogen, with or without oxygen, or carbon only, not provided for in groups C09D161/00 - C09D177/00
- C09D179/04—Polycondensates having nitrogen-containing heterocyclic rings in the main chain; Polyhydrazides; Polyamide acids or similar polyimide precursors
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F220/00—Copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and only one being terminated by only one carboxyl radical or a salt, anhydride ester, amide, imide or nitrile thereof
- C08F220/02—Monocarboxylic acids having less than ten carbon atoms; Derivatives thereof
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- C08F220/34—Esters containing nitrogen, e.g. N,N-dimethylaminoethyl (meth)acrylate
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- C09D5/00—Coating compositions, e.g. paints, varnishes or lacquers, characterised by their physical nature or the effects produced; Filling pastes
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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
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- 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
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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
- C08L2201/00—Properties
- C08L2201/02—Flame or fire retardant/resistant
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Abstract
The present invention provides a kind of new-energy automobile anti-flaming dope, the raw material components including following parts by weight: 40-50 parts of sulfonic group benzophenone tetrazine class condensation polymer, 20-30 parts of cyano acrylate containing fluorine copolymer, Ti-O-B-F15-25 parts of surface modification, 1-3 parts of defoaming agent, 1-3 parts of dispersing agent, 15-20 parts of cosolvent；The sulfonic group benzophenone tetrazine class condensation polymer is to be prepared by 2,2' dihydroxy 4,4' dimethoxy benzophenone -5,5'- sodium disulfonate and clofentezine by polycondensation reaction.The invention also discloses the preparation methods and its application method of the new-energy automobile anti-flaming dope.Disclosed by the invention preparation method is simple, not high to device dependence, and raw material is easy to get, it is cheap, it is suitble to industrialized production, the new-energy automobile being prepared has preparation cost cheap with anti-flaming dope, the advantages of fire retardant insulating good heat conduction effect, stability is good, high mechanical strength.
Description
Technical field
The present invention relates to technical field of new energy more particularly to a kind of new-energy automobile anti-flaming dope and its preparations
Method.
Background technique
In recent years, with the rapid development of society, global energy crisis constantly aggravates, environmental pollution is getting worse,
And orthodox car is gone on a journey the indispensable vehicles as people, usually relies on oil firing driving, can aggravate the energy and environment danger
Machine.Exactly in this case, as the new energy vapour that may advantageously facilitate environmental protection and the short crisis of alleviation traditional energy
Vehicle causes the extensive concern of people, has a vast market development prospect.
New-energy automobile is the automobile using cleaning new energy as driving, mainly includes fuel cell car, hybrid power
Automobile, hydrogen-powered vehicles and solar telephone etc..These automobiles are a little exactly jointly that discharge amount of exhaust gas is relatively low, to ring
Border pollution is few, does not use conventional fossil raw material, is conducive to energy saving.Wherein, electronic vapour is referred to as with the automobile being driven by electricity
Vehicle, safety in utilization, comfort level and the service life of electric car be unable to do without the safe operation of electric system.Ensure electric system
Safe operation beneficial measure be in power-driven gear enclosure coater insulating coating, but during long-play, warp
It often will appear apparatus overheat phenomenon, superheating phenomenon will lead to insulating coating aging or even burn insulating coating, cause short trouble
And heavy economic losses.Therefore, the anti-flammability for improving insulating coating becomes focus of attention in the industry.
Mostly function is added by resins such as polyimide resin, polyether-ketone or epoxy modified silicones in insulating coating in the prior art
Energy filler is made, but these materials poor flame retardant properties itself, heat conductive insulating performance need to be further increased, and is filled out by adding function
Material can improve comprehensive performance to a certain extent, but the functional stuffing being added is excessive, will lead to manufacturing cost rising, viscosity of the coating
Excessive, mobility is poor, and matrix resin poor compatibility, and in the long-term use, these functional stuffings will appear extravasation
Phenomenon, so that service life is shortened, and they cannot realize adherency on base material well, thus in new-energy automobile industry
Use receive very big limitation.
Chinese patent CN201010137556 discloses a kind of flame-retarding and heat-conducting silicon rubber insulating paint, it is by terminal hydroxy group silicon
Oxygen alkane, reinforcing agent, nano montmorillonite, composite flame-retardant agent, heat filling and pigment, crosslinking agent, catalysts and solvents；Due to having
It is filled with more fire-retardant, heat filling in machine silicon insulating materials, easily leads to that its mechanical strength is poor, and heating conduction also fails to reach
To more satisfactory requirement.
Therefore, the defect for overcoming coatings in the prior art develops a kind of fire-retardant, insulation, good heat conduction effect, comprehensive
Excellent new-energy automobile is had very important significance with anti-flaming dope.
Summary of the invention
The main purpose of the present invention is to provide a kind of new-energy automobile anti-flaming dope and preparation method thereof, the preparation sides
Method is simple and easy, not high to device dependence, and raw material is easy to get, cheap, is suitble to industrialized production.The new energy being prepared
It is higher that automobile anti-flaming dope overcomes traditional anti-flaming dope preparation cost in the prior art, poor flame retardant properties, heat conductive insulating
Performance needs to be further increased, and in the long-term use, these functional stuffings will appear exosmose, to shorten using the longevity
The technical issues of life, have preparation cost it is cheap, fire retardant insulating good heat conduction effect, stability is good, high mechanical strength it is excellent
Point.
To achieve the above objectives, the present invention provides a kind of new-energy automobile anti-flaming dope, the original including following parts by weight
Expect component: 40-50 parts of sulfonic group benzophenone tetrazine class condensation polymer, 20-30 parts of cyano acrylate containing fluorine copolymer, surface
Modify Ti-O-B-F15-25 parts, 1-3 parts of defoaming agent, 1-3 parts of dispersing agent, 15-20 parts of cosolvent.
Further, the sulfonic group benzophenone tetrazine class condensation polymer is by 2,2'- dihydroxy -4,4'- dimethoxy
Benzophenone -5,5'- sodium disulfonate and clofentezine are prepared by polycondensation reaction.
Preferably, the defoaming agent be selected from tributyl phosphate, defoaming agent moral be modest 3100, one of defoaming agent BYK088 or
It is several；The dispersing agent is selected from least one of calgon, polycarboxylate sodium；The cosolvent is selected from ethyl alcohol, isopropyl
One or more of alcohol, isobutanol, n-butanol, propylene glycol monomethyl ether, ethylene glycol ethyl ether, butyl.
Further, the preparation method of the sulfonic group benzophenone tetrazine class condensation polymer includes the following steps: 2,
2'- dihydroxy -4,4'- dimethoxy-benzophenone -5,5'- sodium disulfonate, clofentezine, basic catalyst are added to and are connected to water segregator
There-necked flask in, then increase boiling point solvent and toluene, reaction system be heated to 135-145 DEG C, nitrogen or inert gas shielding
Under be stirred to react 8-10 hours, the water and toluene that generate in reaction process are removed by water segregator, eliminating will reaction temperature after water
Degree is slowly increased to 155-165 DEG C, continues to be stirred to react 8-10 hours, is after reaction cooled to room temperature reaction system, then to
The hydrochloric acid that mass fraction is 36-38% is wherein added, reaction 4-6 hours is stirred at room temperature, revolving removes unreacted hydrochloric acid, rear mistake
The inorganic salts of dereaction generation are filtered out, then are precipitated in acetone, by the polymer of precipitation with ethanol washing 3-5 times, are placed on 80-
It is 20-25 hours dry in vacuum oven at 90 DEG C, obtain sulfonic group benzophenone tetrazine class condensation polymer.
Preferably, 2,2'- dihydroxy -4,4'- dimethoxy-benzophenone -5,5'- sodium disulfonate, clofentezine, alkali
Property catalyst, high boiling solvent, toluene, hydrochloric acid mass ratio be 1.58:1:(0.5-1): (8-12): (3-5): 0.4.
Preferably, the high boiling solvent is selected from butyl, dimethyl sulfoxide, n,N-Dimethylformamide, N- first
One or more of base pyrrolidones.
Preferably, the basic catalyst is selected from one or more of cesium carbonate, potassium carbonate, sodium carbonate.
Preferably, the inert gas is selected from one or more of helium, neon, argon gas.
Further, the preparation method of the cyano acrylate containing fluorine copolymer includes the following steps: 4- propylene
Oxygroup -2- dihydroxy benaophenonel, cyanacrylate, hexafluoro-isobutene, (2- acryloyl-oxyethyl) trimethyl ammonium chloride,
Initiator is added in dimethyl sulfoxide, is stirred to react at 70-80 DEG C of nitrogen atmosphere 4-6 hours, after settle out in water, and will analysis
Polymer out is washed 3-5 times with ethyl alcohol, is placed at 70-80 DEG C of vacuum oven and is dried 12-18 hours, obtains cyano fluorine-containing propene
Acid esters analog copolymer.
Preferably, the 4- propenyloxy group -2- dihydroxy benaophenonel, cyanacrylate, hexafluoro-isobutene, (2- third
Alkene trimethylammonium) trimethyl ammonium chloride, initiator, dimethyl sulfoxide mass ratio be 1:1:1:(1-2): (0.03-0.05):
(15-20)。
Preferably, the initiator is selected from least one of azodiisobutyronitrile, azobisisoheptonitrile.
Further, the preparation method of the surface modification Ti-O-B-F, includes the following steps:
By titanium tetrachloride, ttraethylammonium tetrafluoroborate is dissolved in the aqueous citric acid solution that mass fraction is 10-20% to be formed S1
Solution, the hydro-thermal reaction 15-18h at 165-185 DEG C, it is small that rear taking-up is placed in 110-120 DEG C of baking 10-14 in air dry oven
When, after product is ground, cross 200-400 mesh obtain, obtain Ti-O-B-F；
S2 disperses the Ti-O-B-F being prepared by step S1 in ethyl alcohol, then silane coupling agent is added thereto
KH560 is stirred to react 3-5 hours at 50-60 DEG C, rear to be centrifuged, then is placed at 80-90 DEG C of vacuum oven and is dried 12-18 hours,
Obtain surface modification Ti-O-B-F.
Preferably, titanium tetrachloride described in step S1, ttraethylammonium tetrafluoroborate, aqueous citric acid solution mass ratio be 2:
0.03:(6-10)。
Preferably, Ti-O-B-F described in step S2, ethyl alcohol, silane coupling agent KH560 mass ratio be 1:(5-10):
0.2。
Preferably, the preparation method of the new-energy automobile anti-flaming dope, includes the following steps: to mix each component,
With 70-80 DEG C of temperature, 1000-1200 revs/min of speed is stirred 40-60 minutes, is then ground, and crosses 200-400 mesh,
Obtain new-energy automobile anti-flaming dope.
Preferably, the application method of the new-energy automobile anti-flaming dope includes the following steps: the new energy vapour
Automobile-used anti-flaming dope even application is printed in substrate, is solidified at a temperature of 120-150 DEG C, forms new-energy automobile with fire-retardant
Coating.
Due to the application of the above technical scheme, the invention has the following advantages:
(1) a kind of new-energy automobile anti-flaming dope disclosed by the invention and preparation method thereof, the preparation method is simply easy
Row, not high to device dependence, raw material is easy to get, cheap, is suitble to industrialized production.
(2) new-energy automobile anti-flaming dope disclosed by the invention overcomes traditional anti-flaming dope system in the prior art
Standby higher cost, poor flame retardant properties, heat conductive insulating performance need to be further increased, and in the long-term use, these functions are filled out
Material will appear exosmose, so that the technical issues of shortening service life, has preparation cost cheap, fire retardant insulating heat-conducting effect
Well, the advantages of stability is good, high mechanical strength.
(3) new-energy automobile anti-flaming dope disclosed by the invention, while condensation polymer is added and two kinds of addition polymers film forming are poly-
Object is closed, they can have complementary advantages, and improve filming performance, weatherability and stability；The two is keyed by ion, so that
Coating structure is more compact, and comprehensive performance is more preferably；Benzophenone, sulfonate, phenyl ring, tetrazine knot are introduced on condensation polymer strand
Structure, each structure synergistic effect, so that coating has excellent anti-flammability, and these flame retarding constructions are directly in film forming matter strand
On, it avoids and is mutually separated caused by addition inorganic fire retardants, exosmose effectively increases coating performance stability, improves
Its processing fluidity；Contain fluorine, cyano, benzophenone structural in addition polymers, improves the weatherability and insulating properties of coating.
(4) new-energy automobile anti-flaming dope disclosed by the invention, each ingredient synergistic effect are conducive to improve coating synthesis
Performance, so that coating heat conductive insulating flame retardant effect is more preferable；The introducing of sulfonic group, phenolic hydroxyl group, ionic group, improves coating and base
The adhesion strength of material；By the way that surface modification Ti-O-B-F is added, heat conductive insulating ability can be effectively improved.
Specific embodiment
It is described below for disclosing the present invention so that those skilled in the art can be realized the present invention.It is excellent in being described below
Embodiment is selected to be only used as illustrating, it may occur to persons skilled in the art that other obvious modifications.
Raw material used in the embodiment of the present invention is purchased from Mo Bei (Shanghai) Biotechnology Co., Ltd.
Embodiment 1
A kind of new-energy automobile anti-flaming dope, the raw material components including following parts by weight: sulfonic group benzophenone tetrazine
40 parts of class condensation polymer, 20 parts of cyano acrylate containing fluorine copolymer, Ti-O-B-F15 parts of surface modification, 1 part of tributyl phosphate,
1 part of calgon, 15 parts of ethyl alcohol.
The sulfonic group benzophenone tetrazine class condensation polymer is by 2,2' dihydroxy 4,4' dimethoxy benzophenone-
5,5'- sodium disulfonate and clofentezine are prepared by polycondensation reaction.
The preparation method of the sulfonic group benzophenone tetrazine class condensation polymer, includes the following steps: 2,2'- dihydroxy-
4,4'- dimethoxy-benzophenone -5,5'- sodium disulfonate 15.8g, clofentezine 10g, cesium carbonate 5g are added to and are connected to the three of water segregator
In mouthful bottle, then plus butyl 80g and toluene 30g, reaction system is heated to 135 DEG C, stirred under nitrogen atmosphere reaction 8
Hour, the water and toluene that generate in reaction process are removed by water segregator, water is eliminated and reaction temperature is slowly increased to 155 later
DEG C, continue to be stirred to react 8 hours, be after reaction cooled to room temperature reaction system, then mass fraction is added thereto and is
Reaction 4 hours is stirred at room temperature in 36% hydrochloric acid 4g, and revolving removes unreacted hydrochloric acid, after be filtered to remove reaction generate it is inorganic
Salt, then be precipitated in acetone, by the polymer of precipitation with ethanol washing 3 times, it is placed in the vacuum oven at 80 DEG C dry
20 hours, obtain sulfonic group benzophenone tetrazine class condensation polymer.
The preparation method of the cyano acrylate containing fluorine copolymer includes the following steps: 4- propenyloxy group -2- hydroxyl
Base benzophenone 10g, cyanacrylate 10g, hexafluoro-isobutene 10g, (2- acryloyl-oxyethyl) trimethyl ammonium chloride
10g, azodiisobutyronitrile 0.3g are added in dimethyl sulfoxide 150g, are stirred to react at 70 DEG C of nitrogen atmosphere 4 hours, after in water
In settle out, and the polymer of precipitation is washed 3 times with ethyl alcohol, is placed at 70 DEG C of vacuum oven and dries 12 hours, obtain cyano and contain
Perfluoroalkyl acrylate lipin polymer.
The preparation method of the surface modification Ti-O-B-F, includes the following steps:
Titanium tetrachloride 20g, ttraethylammonium tetrafluoroborate 0.3g are dissolved in the aqueous citric acid solution 60g that mass fraction is 10% by S1
Middle formation solution, the hydro-thermal reaction 15h at 165 DEG C, it is rear take out to be placed in air dry oven dry 10 hours for 110 DEG C, after will produce
Object grinding is crossed 200 meshes and is obtained, obtains Ti-O-B-F；
S2 disperses the Ti-O-B-F10g being prepared by step S1 in ethyl alcohol 50g, then silane idol is added thereto
Join agent KH5602g, is stirred to react at 50 DEG C 3 hours, it is rear to be centrifuged, then be placed at 80 DEG C of vacuum oven and dry 12 hours, it obtains
Surface modification Ti-O-B-F.
The preparation method of the new-energy automobile anti-flaming dope, includes the following steps: to mix each component, with 70 DEG C
Temperature, 1000 revs/min of speed are stirred 40 minutes, are then ground, cross 200 meshes to get to new-energy automobile with fire-retardant
Coating.
The application method of the new-energy automobile anti-flaming dope includes the following steps: to hinder the new-energy automobile
Burning coating material even application solidifies at a temperature of 120 DEG C in substrate, forms new-energy automobile flame retardant coating.
Embodiment 2
A kind of new-energy automobile anti-flaming dope, the raw material components including following parts by weight: sulfonic group benzophenone tetrazine
43 parts of class condensation polymer, 23 parts of cyano acrylate containing fluorine copolymer, Ti-O-B-F17 parts of surface modification, defoaming agent moral are modest
31002 parts, 2 parts of polycarboxylate sodium, 16 parts of isopropanol.
The sulfonic group benzophenone tetrazine class condensation polymer is by 2,2' dihydroxy 4,4' dimethoxy benzophenone-
5,5'- sodium disulfonate and clofentezine are prepared by polycondensation reaction.
The preparation method of the sulfonic group benzophenone tetrazine class condensation polymer, includes the following steps: 2,2'- dihydroxy-
4,4'- dimethoxy-benzophenone -5,5'- sodium disulfonate 15.8g, clofentezine 10g, potassium carbonate 6.5g are added to and are connected to water segregator
In there-necked flask, then plus dimethyl sulfoxide 95g and toluene 35g, reaction system is heated to 139 DEG C, the lower stirring of helium atmosphere protection is anti-
It answers 8.5 hours, the water and toluene that generate in reaction process is removed by water segregator, eliminate water and be later slowly increased to reaction temperature
158 DEG C, continues to be stirred to react 8.5 hours, after reaction be cooled to room temperature reaction system, then mass fraction is added thereto
For 37% hydrochloric acid 4g, reaction 4.5 hours is stirred at room temperature, revolving removes unreacted hydrochloric acid, after be filtered to remove what reaction generated
Inorganic salts, then be precipitated in acetone, by the polymer of precipitation with ethanol washing 4 times, it is placed in the vacuum oven at 83 DEG C
It is 21 hours dry, obtain sulfonic group benzophenone tetrazine class condensation polymer.
The preparation method of the cyano acrylate containing fluorine copolymer includes the following steps: 4- propenyloxy group -2- hydroxyl
Base benzophenone 10g, cyanacrylate 10g, hexafluoro-isobutene 10g, (2- acryloyl-oxyethyl) trimethyl ammonium chloride
12g, azobisisoheptonitrile 0.35g are added in dimethyl sulfoxide 165g, are stirred to react at 72 DEG C of nitrogen atmosphere 4.5 hours, after
It settles out in water, and the polymer of precipitation is washed 4 times with ethyl alcohol, be placed at 73 DEG C of vacuum oven and dry 13.5 hours, obtain
Cyano acrylate containing fluorine copolymer.
The preparation method of the surface modification Ti-O-B-F, includes the following steps:
Titanium tetrachloride 20g, ttraethylammonium tetrafluoroborate 0.3g are dissolved in the aqueous citric acid solution 75g that mass fraction is 12% by S1
Middle formation solution, the hydro-thermal reaction 16h at 170 DEG C, it is rear take out to be placed in air dry oven dry 11.5 hours for 113 DEG C, after will
Product grinding is crossed 250 meshes and is obtained, obtains Ti-O-B-F；
S2 disperses the Ti-O-B-F10g being prepared by step S1 in ethyl alcohol 65g, then silane idol is added thereto
Join agent KH5602g, is stirred to react at 53 DEG C 3.5 hours, it is rear to be centrifuged, then be placed at 83 DEG C of vacuum oven and dry 13.5 hours,
Obtain surface modification Ti-O-B-F.
The preparation method of the new-energy automobile anti-flaming dope, includes the following steps: to mix each component, with 74 DEG C
Temperature, 1050 revs/min of speed are stirred 45 minutes, are then ground, cross 250 meshes to get to new-energy automobile with fire-retardant
Coating.
The application method of the new-energy automobile anti-flaming dope includes the following steps: to hinder the new-energy automobile
Burning coating material even print solidifies at a temperature of 130 DEG C in substrate, forms new-energy automobile flame retardant coating.
Embodiment 3
A kind of new-energy automobile anti-flaming dope, the raw material components including following parts by weight: sulfonic group benzophenone tetrazine
45 parts of class condensation polymer, 25 parts of cyano acrylate containing fluorine copolymer, Ti-O-B-F20 parts of surface modification, defoaming agent BYK0883
Part, 2 parts of calgon, 17.5 parts of propylene glycol monomethyl ether.
The sulfonic group benzophenone tetrazine class condensation polymer is by 2,2' dihydroxy 4,4' dimethoxy benzophenone-
5,5'- sodium disulfonate and clofentezine are prepared by polycondensation reaction.
The preparation method of the sulfonic group benzophenone tetrazine class condensation polymer, includes the following steps: 2,2'- dihydroxy-
4,4'- dimethoxy-benzophenone -5,5'- sodium disulfonate 15.8g, clofentezine 10g, sodium carbonate 8g are added to and are connected to the three of water segregator
In mouthful bottle, then plus n,N-Dimethylformamide 100g and toluene 40g, reaction system is heated to 140 DEG C, the lower stirring of neon protection
Reaction 9 hours removes the water and toluene that generate in reaction process by water segregator, eliminates water and is later slowly increased to reaction temperature
160 DEG C, continue to be stirred to react 9 hours, be after reaction cooled to room temperature reaction system, then mass fraction is added thereto and is
Reaction 5 hours is stirred at room temperature in 38% hydrochloric acid 4g, and revolving removes unreacted hydrochloric acid, after be filtered to remove reaction generate it is inorganic
Salt, then be precipitated in acetone, by the polymer of precipitation with ethanol washing 5 times, it is placed in the vacuum oven at 86 DEG C dry
23 hours, obtain sulfonic group benzophenone tetrazine class condensation polymer.
The preparation method of the cyano acrylate containing fluorine copolymer includes the following steps: 4- propenyloxy group -2- hydroxyl
Base benzophenone 10g, cyanacrylate 10g, hexafluoro-isobutene 10g, (2- acryloyl-oxyethyl) trimethyl ammonium chloride
16g, azodiisobutyronitrile 0.4g are added in dimethyl sulfoxide 180g, are stirred to react at 76 DEG C of nitrogen atmosphere 5.1 hours, after
It settles out in water, and the polymer of precipitation is washed 4 times with ethyl alcohol, be placed at 77 DEG C of vacuum oven and dry 16 hours, obtain cyano
Acrylate containing fluorine copolymer.
The preparation method of the surface modification Ti-O-B-F, includes the following steps:
Titanium tetrachloride 20g, ttraethylammonium tetrafluoroborate 0.3g are dissolved in the aqueous citric acid solution 85g that mass fraction is 17% by S1
Middle formation solution, the hydro-thermal reaction 17h at 175 DEG C, it is rear take out to be placed in air dry oven dry 13 hours for 117 DEG C, after will produce
Object grinding is crossed 300 meshes and is obtained, obtains Ti-O-B-F；
S2 disperses the Ti-O-B-F10g being prepared by step S1 in ethyl alcohol 85g, then silane idol is added thereto
Join agent KH5602g, is stirred to react at 57 DEG C 4 hours, it is rear to be centrifuged, then be placed at 87 DEG C of vacuum oven and dry 16 hours, it obtains
Surface modification Ti-O-B-F.
The preparation method of the new-energy automobile anti-flaming dope, includes the following steps: to mix each component, with 77 DEG C
Temperature, 1100 revs/min of speed are stirred 52 minutes, are then ground, cross 320 meshes to get to new-energy automobile with fire-retardant
Coating.
The application method of the new-energy automobile anti-flaming dope includes the following steps: to hinder the new-energy automobile
Burning coating material even application solidifies at a temperature of 135 DEG C in substrate, forms new-energy automobile flame retardant coating.
Embodiment 4
A kind of new-energy automobile anti-flaming dope, the raw material components including following parts by weight: sulfonic group benzophenone tetrazine
48 parts of class condensation polymer, 28 parts of cyano acrylate containing fluorine copolymer, Ti-O-B-F23 parts of surface modification, 2 parts of defoaming agent, dispersion
3 parts of agent, 19 parts of cosolvent.
The sulfonic group benzophenone tetrazine class condensation polymer is by 2,2' dihydroxy 4,4' dimethoxy benzophenone-
5,5'- sodium disulfonate and clofentezine are prepared by polycondensation reaction.
The defoaming agent is selected from that tributyl phosphate, defoaming agent moral be modest 3100, defoaming agent BYK088 2:1:1 in mass ratio mixing
Made of mixture；The dispersing agent is the mixture that calgon, polycarboxylate sodium 3:5 in mass ratio are mixed；Institute
Stating cosolvent is isopropanol, isobutanol, propylene glycol monomethyl ether, ethylene glycol ethyl ether, butyl 1:2:1:3:1 in mass ratio mixed
Mixture made of conjunction.
The preparation method of the sulfonic group benzophenone tetrazine class condensation polymer, includes the following steps: 2,2'- dihydroxy-
4,4'- dimethoxy-benzophenone -5,5'- sodium disulfonate 15.8g, clofentezine 10g, basic catalyst 9g are added to and are connected to water segregator
There-necked flask in, then increase boiling point solvent 115g and toluene 45g, reaction system be heated to 143 DEG C, the lower stirring of argon gas protection is anti-
It answers 9.5 hours, the water and toluene that generate in reaction process is removed by water segregator, eliminate water and be later slowly increased to reaction temperature
163 DEG C, continues to be stirred to react 9.5 hours, after reaction be cooled to room temperature reaction system, then mass fraction is added thereto
For 37% hydrochloric acid, reaction 5.5 hours is stirred at room temperature, revolving removes unreacted hydrochloric acid, after be filtered to remove the nothing that reaction generates
Machine salt, then be precipitated in acetone, by the polymer of precipitation with ethanol washing 5 times, it is placed in the vacuum oven at 88 DEG C and does
Dry 24 hours, obtain sulfonic group benzophenone tetrazine class condensation polymer；The high boiling solvent is butyl, diformazan Asia
The mixture that sulfone, N,N-dimethylformamide, N-Methyl pyrrolidone 1:1:2:1 in mass ratio are mixed；The alkalinity is urged
Agent is the mixture that cesium carbonate, potassium carbonate, sodium carbonate 2:3:1 in mass ratio are mixed.
The preparation method of the cyano acrylate containing fluorine copolymer includes the following steps: 4- propenyloxy group -2- hydroxyl
Base benzophenone 10g, cyanacrylate 10g, hexafluoro-isobutene 10g, (2- acryloyl-oxyethyl) trimethyl ammonium chloride
18g, initiator 0.45g are added in dimethyl sulfoxide 190g, are stirred to react at 78 DEG C of nitrogen atmosphere 6 hours, after sink in water
Out, and by the polymer of precipitation with ethyl alcohol it washes 5 times, is placed at 78 DEG C of vacuum oven and dries 17.5 hours, it is fluorine-containing to obtain cyano
Acrylic acid esters co-polymer；It is mixed that the initiator is that azodiisobutyronitrile, azobisisoheptonitrile 3:5 in mass ratio are mixed
Close object.
The preparation method of the surface modification Ti-O-B-F, includes the following steps:
Titanium tetrachloride 20g, ttraethylammonium tetrafluoroborate 0.3g are dissolved in the aqueous citric acid solution 93g that mass fraction is 18% by S1
Middle formation solution, the hydro-thermal reaction 17.5h at 180 DEG C, rear take out are placed in 118 DEG C baking 13.5 hours in air dry oven, after
Product is ground, 350 meshes is crossed and obtains, obtain Ti-O-B-F；
S2 disperses the Ti-O-B-F10g being prepared by step S1 in alcohol 95 g, then silane idol is added thereto
Join agent KH5602g, is stirred to react at 58 DEG C 4.5 hours, it is rear to be centrifuged, then be placed at 89 DEG C of vacuum oven and dry 17.5 hours,
Obtain surface modification Ti-O-B-F.
The preparation method of the new-energy automobile anti-flaming dope, includes the following steps: to mix each component, with 79 DEG C
Temperature, 1150 revs/min of speed are stirred 55 minutes, are then ground, cross 350 meshes to get to new-energy automobile with fire-retardant
Coating.
The application method of the new-energy automobile anti-flaming dope includes the following steps: to hinder the new-energy automobile
Burning coating material even print solidifies at a temperature of 145 DEG C in substrate, forms new-energy automobile flame retardant coating.
Embodiment 5
A kind of new-energy automobile anti-flaming dope, the raw material components including following parts by weight: sulfonic group benzophenone tetrazine
50 parts of class condensation polymer, 30 parts of cyano acrylate containing fluorine copolymer, Ti-O-B-F25 parts of surface modification, 3 parts of tributyl phosphate,
3 parts of polycarboxylate sodium, 20 parts of ethylene glycol ethyl ether.
The sulfonic group benzophenone tetrazine class condensation polymer is by 2,2' dihydroxy 4,4' dimethoxy benzophenone-
5,5'- sodium disulfonate and clofentezine are prepared by polycondensation reaction.
The preparation method of the sulfonic group benzophenone tetrazine class condensation polymer, includes the following steps: 2,2'- dihydroxy-
4,4'- dimethoxy-benzophenone -5,5'- sodium disulfonate 15.8g, clofentezine 10g, cesium carbonate 10g are added to and are connected to water segregator
In there-necked flask, then plus N-Methyl pyrrolidone 120g and toluene 50g, reaction system is heated to 145 DEG C, stirred under nitrogen atmosphere
Reaction 10 hours removes the water and toluene that generate in reaction process by water segregator, eliminates water and later slowly rises reaction temperature
To 165 DEG C, continue to be stirred to react 10 hours, be after reaction cooled to room temperature reaction system, then quality point is added thereto
Reaction 6 hours is stirred at room temperature in the hydrochloric acid 4g that number is 38%, and revolving removes unreacted hydrochloric acid, after be filtered to remove what reaction generated
Inorganic salts, then be precipitated in acetone, by the polymer of precipitation with ethanol washing 5 times, it is placed in the vacuum oven at 90 DEG C
It is 25 hours dry, obtain sulfonic group benzophenone tetrazine class condensation polymer.
The preparation method of the cyano acrylate containing fluorine copolymer includes the following steps: 4- propenyloxy group -2- hydroxyl
Base benzophenone 10g, cyanacrylate 10g, hexafluoro-isobutene 10g, (2- acryloyl-oxyethyl) trimethyl ammonium chloride
20g, azobisisoheptonitrile 0.5g are added in dimethyl sulfoxide 200g, are stirred to react at 80 DEG C of nitrogen atmosphere 6 hours, after in water
In settle out, and the polymer of precipitation is washed 5 times with ethyl alcohol, is placed at 80 DEG C of vacuum oven and dries 18 hours, obtain cyano and contain
Perfluoroalkyl acrylate lipin polymer.
The preparation method of the surface modification Ti-O-B-F, includes the following steps:
Titanium tetrachloride 20g, ttraethylammonium tetrafluoroborate 0.3g are dissolved in the aqueous citric acid solution that mass fraction is 20% by S1
Solution is formed in 100g, the hydro-thermal reaction 18h at 185 DEG C, rear take out is placed in 120 DEG C baking 14 hours in air dry oven, after
Product is ground, 400 meshes is crossed and obtains, obtain Ti-O-B-F；
S2 disperses the Ti-O-B-F10g being prepared by step S1 in ethyl alcohol 100g, then silane is added thereto
Coupling agent KH5602g is stirred to react 5 hours at 60 DEG C, rear to be centrifuged, then is placed at 90 DEG C of vacuum oven and is dried 18 hours, is obtained
To surface modification Ti-O-B-F.
The preparation method of the new-energy automobile anti-flaming dope, includes the following steps: to mix each component, with 80 DEG C
Temperature, 1200 revs/min of speed are stirred 60 minutes, are then ground, cross 400 meshes to get to new-energy automobile with fire-retardant
Coating.
The application method of the new-energy automobile anti-flaming dope includes the following steps: to hinder the new-energy automobile
Burning coating material even print solidifies at a temperature of 150 DEG C in substrate, forms new-energy automobile flame retardant coating.
Comparative example
This example provides a kind of anti-flaming dope for new-energy automobile, preparation method and the same Chinese invention patent of formula
CN108329798A embodiment 1.
Above embodiments 1-5 and the comparative example new-energy automobile prepared are tested for the property with anti-flaming dope, test side
Method and test result are shown in Table 1.
Table 1
| Test item | Thermal conductivity | Shock strength | Volume resistivity | Adhesive force | Limit oxygen index |
| Unit | W/m.K | Kg.cm | Ω.cm | MPa | % |
| Testing standard | GB/T10295-88 | GB1732-79 | GB/T1410-2006 | GB/T5210-2006 | GB/T2406 |
| Embodiment 1 | 5.5 | 226 | 5.9×1016 | 8.9 | 33.5 |
| Embodiment 2 | 5.7 | 229 | 6.5×1016 | 9.5 | 34.2 |
| Embodiment 3 | 5.9 | 234 | 7.0×1016 | 9.9 | 34.5 |
| Embodiment 4 | 6.2 | 238 | 7.4×1016 | 10.3 | 35.0 |
| Embodiment 5 | 6.5 | 244 | 7.8×1016 | 10.8 | 35.4 |
| Comparative example | 3.0 | 190 | 1.5×1015 | 5.9 | 15.2 |
As seen from Table 1, new-energy automobile anti-flaming dope disclosed by the embodiments of the present invention, with fire-retardant painting in the prior art
Material is compared, and has more excellent insulating heat-conductive flame retardant effect, and shock resistance and adhesive force are bigger.
The basic principles, main features and advantages of the present invention have been shown and described above.The technology of the industry
Personnel are it should be appreciated that the present invention is not limited to the above embodiments, and what is described in the above embodiment and the description is only the present invention
Principle, various changes and improvements may be made to the invention without departing from the spirit and scope of the present invention, these variation and
Improvement is both fallen in the range of claimed invention.The present invention claims protection scope by appended claims and its
Equivalent defines.
Claims (10)
1. a kind of new-energy automobile anti-flaming dope, which is characterized in that the raw material components including following parts by weight: sulfonic group hexichol
40-50 parts of ketone tetrazine class condensation polymer, 20-30 parts of cyano acrylate containing fluorine copolymer, surface modification Ti-O-B-F15-25
Part, 1-3 parts of defoaming agent, 1-3 parts of dispersing agent, 15-20 parts of cosolvent；The sulfonic group benzophenone tetrazine class condensation polymer be by 2,
2'- dihydroxy -4,4'- dimethoxy-benzophenone -5,5'- sodium disulfonate and clofentezine are prepared by polycondensation reaction.
2. new-energy automobile anti-flaming dope according to claim 1, which is characterized in that the defoaming agent is selected from tricresyl phosphate
Butyl ester, defoaming agent moral be modest 3100, one or more of defoaming agent BYK088；The dispersing agent is selected from calgon, poly- carboxylic
At least one of acid sodium-salt；The cosolvent is selected from ethyl alcohol, isopropanol, isobutanol, n-butanol, propylene glycol monomethyl ether, ethylene glycol
One or more of ether, butyl.
3. new-energy automobile anti-flaming dope according to claim 1, which is characterized in that the sulfonic group benzophenone four
The preparation method of piperazine class condensation polymer includes the following steps: 2,2'- dihydroxy -4,4'- dimethoxy-benzophenone -5,5'- bis-
Sodium sulfonate, clofentezine, basic catalyst are added in the there-necked flask for being connected to water segregator, then increase boiling point solvent and toluene, will be reacted
System is heated to 135-145 DEG C, is stirred to react under nitrogen or inert gas shielding 8-10 hours, removes dereaction mistake by water segregator
The water and toluene generated in journey eliminates and reaction temperature is slowly increased to 155-165 DEG C after water, continues to be stirred to react 8-10 small
When, reaction system is cooled to room temperature after reaction, then the hydrochloric acid that mass fraction is 36-38% is added thereto, room temperature is stirred
Mix reaction 4-6 hour, revolving removes unreacted hydrochloric acid, after be filtered to remove the inorganic salts of reaction generation, then be precipitated in acetone,
By the polymer of precipitation with ethanol washing 3-5 times, drying 20-25 hours in the vacuum oven at 80-90 DEG C are placed on, are obtained
Sulfonic group benzophenone tetrazine class condensation polymer.
4. new-energy automobile anti-flaming dope according to claim 3, which is characterized in that dihydroxy -4 2,2'-,
The matter of 4'- dimethoxy-benzophenone -5,5'- sodium disulfonate, clofentezine, basic catalyst, high boiling solvent, toluene, hydrochloric acid
Amount is than being 1.58:1:(0.5-1): (8-12): (3-5): 0.4；It is sub- that the high boiling solvent is selected from butyl, diformazan
One or more of sulfone, N,N-dimethylformamide, N-Methyl pyrrolidone；The basic catalyst is selected from cesium carbonate, carbon
One or more of sour potassium, sodium carbonate；The inert gas is selected from one or more of helium, neon, argon gas.
5. new-energy automobile anti-flaming dope according to claim 1, which is characterized in that the cyano fluorinated acrylate
The preparation method of analog copolymer includes the following steps: 4- propenyloxy group -2- dihydroxy benaophenonel, cyanacrylate, six
Fluorine isobutene, (2- acryloyl-oxyethyl) trimethyl ammonium chloride, initiator are added in dimethyl sulfoxide, in nitrogen atmosphere 70-
Be stirred to react at 80 DEG C 4-6 hours, after settle out in water, and the polymer of precipitation is washed 3-5 times with ethyl alcohol, it is dry to be placed on vacuum
It is dried 12-18 hours at 70-80 DEG C of dry case, obtains cyano acrylate containing fluorine copolymer.
6. new-energy automobile anti-flaming dope according to claim 5, which is characterized in that the 4- propenyloxy group -2- hydroxyl
Base benzophenone, cyanacrylate, hexafluoro-isobutene, (2- acryloyl-oxyethyl) trimethyl ammonium chloride, initiator, two
The mass ratio of first sulfoxide is 1:1:1:(1-2): (0.03-0.05): (15-20)；The initiator is selected from azodiisobutyronitrile, idol
At least one of different heptonitrile of nitrogen two.
7. new-energy automobile anti-flaming dope according to claim 1, which is characterized in that the surface modification Ti-O-B-F
Preparation method, include the following steps:
For S1 by titanium tetrachloride, ttraethylammonium tetrafluoroborate, which is dissolved in the aqueous citric acid solution that mass fraction is 10-20%, forms solution,
The hydro-thermal reaction 15-18h at 165-185 DEG C, rear take out are placed in 110-120 DEG C bakings 10-14 hours in air dry oven, after general
Product grinding is crossed 200-400 mesh and is obtained, obtains Ti-O-B-F；
S2 disperses the Ti-O-B-F being prepared by step S1 in ethyl alcohol, then silane coupling agent KH560 is added thereto,
It is stirred to react at 50-60 DEG C 3-5 hours, it is rear to be centrifuged, then be placed at 80-90 DEG C of vacuum oven and dry 12-18 hours, obtain table
Ti-O-B-F is modified in face.
8. new-energy automobile anti-flaming dope according to claim 7, which is characterized in that four chlorinations described in step S1
Titanium, ttraethylammonium tetrafluoroborate, aqueous citric acid solution mass ratio be 2:0.03:(6-10)；Ti-O-B-F described in step S2, second
Alcohol, silane coupling agent KH560 mass ratio be 1:(5-10): 0.2.
9. new-energy automobile anti-flaming dope according to claim 1-8, which is characterized in that the new energy vapour
The preparation method of automobile-used anti-flaming dope includes the following steps: to mix each component, with 70-80 DEG C of temperature, 1000-1200 turns/
Point speed stir 40-60 minute, then ground, mistake 200-400 mesh is to get to new-energy automobile anti-flaming dope.
10. new-energy automobile anti-flaming dope according to claim 1-8, which is characterized in that the new energy
The application method of automobile anti-flaming dope includes the following steps: the new-energy automobile anti-flaming dope even application or print
Brush solidifies at a temperature of 120-150 DEG C in substrate, forms new-energy automobile flame retardant coating.
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