CN109135524A - A kind of preparation method of flame retardant type alkyd resin insulated paint - Google Patents
A kind of preparation method of flame retardant type alkyd resin insulated paint Download PDFInfo
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- CN109135524A CN109135524A CN201810931562.6A CN201810931562A CN109135524A CN 109135524 A CN109135524 A CN 109135524A CN 201810931562 A CN201810931562 A CN 201810931562A CN 109135524 A CN109135524 A CN 109135524A
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- alkyd resin
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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
- C09D167/08—Polyesters modified with higher fatty oils or their acids, or with natural resins or resin acids
-
- 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
- C08G63/692—Polyesters containing atoms other than carbon, hydrogen and oxygen containing phosphorus
- C08G63/6924—Polyesters containing atoms other than carbon, hydrogen and oxygen containing phosphorus derived from polycarboxylic acids and polyhydroxy compounds
- C08G63/6928—Polycarboxylic acids and polyhydroxy compounds in which at least one of the two components contains aliphatic unsaturation
-
- 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
- C09D5/00—Coating compositions, e.g. paints, varnishes or lacquers, characterised by their physical nature or the effects produced; Filling pastes
- C09D5/14—Paints containing biocides, e.g. fungicides, insecticides or pesticides
-
- 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
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
- C09D7/00—Features of coating compositions, not provided for in group C09D5/00; Processes for incorporating ingredients in coating compositions
- C09D7/40—Additives
- C09D7/60—Additives non-macromolecular
- C09D7/63—Additives non-macromolecular organic
-
- 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
- C08K2201/014—Additives containing two or more different additives of the same subgroup in C08K
Abstract
The invention discloses the preparation methods of flame retardant type alkyd resin insulated paint, unsaturated alkyd resin, vinyltoluene, peroxide initiator, fat hydrocarbon solvent oil and drier are mixed to get flame retardant type alkyd resin insulated paint, unsaturated alkyd resin is by including that the raw material of binary acid, three phosphazene derivative of polyalcohol, fatty acid and hydroxyl ring is made；Flame retardant type alkyd resin insulated paint produced by the present invention, flame retardant property is stable, insulating properties is high, and effect is best, and meets environmental requirement for three proofings (moisture-proof, mould proof, salt spray proof).
Description
Technical field
The invention belongs to chemical industry macromolecule paint technology fields, and in particular to a kind of system of flame retardant type alkyd resin insulated paint
Preparation Method.
Background technique
Alkyd resin coating be with polyalcohol, polyacid and plant oil modified copolycondensation and manufactured alkyd resin be mainly at
A kind of coating of membrane substance, such paint have good workability, can air drying film forming, film light is plentiful, adhesive force is strong, it is flexible,
It is firm and non-aging；It is assorted at a variety of with their own characteristics also using alkyd resin and the good feature of other resin miscibles
Coating products, to meet all kinds of demands in market；It is widely used to metal surface, consumption electronic product, LED display and various
The fields such as hybrid coil.
However, not fire retardant treated alkyd resin coating flammability is high, dielectric strength is low, in recent years due to all kinds of macromolecules
Material ignite and conduction caused by fire disaster accident be common in report.To reduce fire bring heavy losses, absolutely mostly
Number polymeric material has to pass through fire-retardant and insulation processing when in use, is allowed to that electric leakage can be effectively prevented in use,
Resistance to electric arc can prevent burning or retarded combustion speed in burning.
Patent CN103275604A discloses phosphorous alkyd resin transparent fire-resisting paint and preparation method thereof, by quality percentage
Number meter, phosphorous alkyd resin transparent fire-resisting paint formula are as follows: phosphorous alkyd resin 62% ~ 80%, drier 2% ~ 3%, solvent 18% ~
35%；Its preparation step are as follows: phosphorous alkyd resin is added in formula ratio solvent and disperses 20~40min, drier is added multi-purpose
Disperse after 10~20min in disperse mill up to product.The technical solution has anti-flammability by introducing in alkyd resin
Can element phosphor, improve the fire protecting performance of coating of objects, the additive amount of phosphonium flame retardant it is usually larger (commonly reach 20~
50wt%), it easily will lead to the mechanical degradation of material, rate of drying is slack-off, adhesive force is deteriorated, poor insulativity.
Patent CN104592814A discloses a kind of insulation coating compositions, wherein the composition includes cellulose nitric acid
Ester, alkyd resin, epoxy resin, organic solvent, curing agent and film forming agent；Wherein, relative to the cellulose nitric acid of 100 parts by weight
Ester, the content of the alkyd resin are 20-50 parts by weight, and the content of the epoxy resin is 20-50 parts by weight, described organic molten
The content of agent is 120-180 parts by weight, and the content of the curing agent is 1-5 parts by weight, and the content of the film forming agent is 1-5 weight
Part；Addition of the technical solution by curing agent and film forming agent, obtained insulated paint excellent insulation performance, fast drying, toughness
It is good, but have no flame retardant property.
Summary of the invention
In order to solve the above technical problems, the present invention provides a kind of preparation method of flame retardant type alkyd resin insulated paint, passes through
The addition of three phosphazene derivative of hydroxyl ring, improves alkyd resin, and obtained alkyd resin coating flame retardant property is stable, exhausted
Edge is high, and effect is best, and meets environmental requirement for three proofings (moisture-proof, mould proof, salt spray proof).
The technical solution adopted in the present invention is as follows:
A kind of preparation method of flame retardant type alkyd resin insulated paint, prepare raw material include unsaturated alkyd resin, vinyltoluene,
Peroxide initiator, fat hydrocarbon solvent oil and drier, the preparation method is as follows:
(1) unsaturated alkyd resin and vinyltoluene is added into reaction kettle in proportion, after being warming up to 100~140 DEG C, to anti-
It answers and at the uniform velocity instills peroxide initiator in kettle, terminate reaction after reacting fluid viscosity qualification；
(2) reaction solution that cooling step (1) obtains, while fat hydrocarbon solvent oil is added, when temperature is down to 60 DEG C or less, add
Enter drier, is mixed and stirred for uniformly to get flame retardant type alkyd resin insulated paint；
Wherein, unsaturated alkyd resin the preparation method is as follows:
(1) binary acid, polyalcohol and fatty acid are added into reaction kettle, is passed through nitrogen, the acid value cooling of esterification to setting；
(2) it is added remaining fatty acid and three phosphazene derivative of hydroxyl ring, after the acid value of high temperature dehydration to setting, terminates anti-
It answers, when reacting liquid temperature is down to 60 DEG C or less, discharges up to unsaturated alkyd resin.
Preferably, when preparing unsaturated alkyd resin, in step (1), high temperature esterification reaction temperature is 180~240 DEG C,
Acid value is set as 50~100mgKOH/g, cooling temperature is 170 ~ 180 DEG C；In step (2), high temperature dehydration temperature is 200~240
DEG C, acid value is set as 5~15mgKOH/g.
The binary acid be phthalic acid, M-phthalic acid, succinic acid, tetrahydrophthalic acid, phthalic anhydride,
One or more of pentamethylene -1,2- dioctyl phthalate, hexanedioic acid, azelaic acid, preferably phthalic anhydride.
Preferably, the polyalcohol is trihydroxylic alcohol and/or tetrahydroxylic alcohol.
It is highly preferred that the tetrahydroxylic alcohol is pentaerythrite or D-sorbite；The trihydroxylic alcohol is glycerol, trimethylolpropane
Diallyl ether, trimethylolethane or trimethylolpropane.
Preferably, fatty acid is tung oil fatty acid, dehydrated castor oil fatty acid, Bristol oleic acid, linseed oil fatty acid, soybean
One or more of fatty acid oil.
Preferably, the fat hydrocarbon solvent oil is low boiling point fat hydrocarbon solvent oil.
Preferably, the structural formula of three phosphazene derivative of hydroxyl ring is as follows:
In formula, group R is the primary alkoxy of phenol oxygroup or 2 ~ 8 carbon atoms, preferably phenol oxygroup；
Group R1 is the hydroxy alkoxy base or ethyl alcohol amido of 2 ~ 4 carbon atoms, preferably ethyl alcohol amido.
Preferably, the drier is metal ethylhexanoate salt, and the metal is one or more of cobalt, manganese, zirconium, zinc.
Preferably, the peroxide initiator is benzoyl peroxide, cumyl peroxide, tert-butyl hydroperoxide three
Hexahydrotoluene or perbenzoic acid tert-butyl.
Compared with prior art, the present invention has following technical advantage:
(1) present invention makees under the premise of being not introduced into any halogen-containing flame retardant by using three phosphazene derivative of hydroxyl ring
For fire-retardant Material synthesis flame retardant type alkyd resin, make to contain flame retardant property element phosphor and nitrogen in alkyd resin macromolecular chain simultaneously,
And generate synergistic effect, and the additive amount of three phosphazene derivative of hydroxyl ring is low (11~15wt%), obtained insulated paint it is fire-retardant
Performance is stablized, and phenomena such as flame retardant property is reduced, lost will not occurs over time, and meet environmental requirement.
(2) not metal ion, the movement of no positron-electron in paint film made from conventional alkyd resin, therefore paint film itself has
Have faint insulating properties, and in the present invention in the molecular structure of three phosphazene derivative of hydroxyl ring containing multiple active groups (-
OH), the macromolecular that dehydration esterification reaction generates tridimensional network, macromolecular sheet occurs with binary acid and fatty acid at high temperature
Body has extremely strong cohesive force, so that alkyd resin molecule generates electromagnetic adsorption or chemical bond with the interface being in contact, enhances
The cementability and insulating properties of obtained paint film, and fast drying, three proofings (moisture-proof, mould proof, salt spray proof) effect are good.
Specific embodiment
Now in conjunction with specific embodiment, the present invention is further illustrated, and in following embodiment, the test method of acid value is
Referring to " measurement of GB/T 2895-2008 plastic polyester resin portion acid value and total acid number ", the test of viscosity is referring to " GB/T
7193.1-1987 unsaturated polyester resin viscosity measurement " it carries out.
Embodiment 1
A kind of flame retardant type alkyd resin insulated paint, is made of the raw material with following parts by weight:
105 parts of unsaturated alkyd resin, 45 parts of vinyltoluene, 1 part of cumyl peroxide, fat hydrocarbon solvent oil 225 parts,
0.2 part of cobalt iso-octoate, 0.2 part of manganese iso-octoate, 1.6 parts of zirconium iso-octoate；Wherein, unsaturated alkyd resin is by following parts by weight
Raw material is made: 40 parts of phthalic anhydride, 34 parts of pentaerythrite, 50 parts of dehydrated castor oil fatty acid, 90 parts of linseed oil fatty acid,
30 parts of three phosphonitriles of 2,4,6- triphenol oxygroup -2,4,6 three (hydroxyl-oxethyl) ring.
Flame retardant type alkyd resin insulated paint the preparation method is as follows:
(1) 40 parts of phthalic anhydride, 34 parts of pentaerythrite, dehydrated castor oil are added into the first reaction kettle equipped with water segregator
50 parts and 60 parts of linseed oil fatty acid of fatty acid, it is passed through nitrogen, starts stirring, is warming up to 180 DEG C of dehydration esterification reaction 2h, then rise
Temperature to 240 DEG C of high temperature esterifications react, until reaction solution is cooled to 180 DEG C after reaction solution acid value is 80mgKOH/g；
(2) three phosphonitrile of 2,4,6- triphenol oxygroup -2,4,6 three (hydroxyl-oxethyl) ring is added in the reaction solution obtained to step (1)
30 parts and 30 parts of linseed oil fatty acid, 220 DEG C, after high temperature dehydration to acid value is 10mgKOH/g are warming up to, reaction, reaction are terminated
When liquid temperature is down to 60 DEG C or less, discharge up to unsaturated alkyd resin, it is spare.
(3) 105 parts and 45 parts of vinyltoluene of unsaturated alkyd resin are added into the second reaction kettle, is warming up to 140 DEG C
Afterwards, 1 part of cumyl peroxide is taken, average rate instills in reaction kettle, time for adding 3h, isothermal reaction；It extracts reaction solution and uses rouge
Fat hydrocarbon solvent oil is diluted to the resin solution containing 60% admittedly, and whether the viscosity for measuring resin solution as required reaches 8000
The mPa.s of mPa.s~10000 continues the constant temperature reaction for keeping the second reaction kettle, if the resin solution if unqualified
Viscosity test it is qualified after, terminate reaction；
(4) reaction solution that cooling step (3) obtains, while 225 parts of fat hydrocarbon solvent oil is added, 60 DEG C or less are down to temperature
When, be added 0.2 part of cobalt iso-octoate, 0.2 part of manganese iso-octoate, 1.6 parts of zirconium iso-octoate be mixed evenly up to flame retardant type alkyd tree
Rouge insulated paint.
Embodiment 2
A kind of flame retardant type alkyd resin insulated paint, is made of the raw material with following parts by weight:
150 parts of unsaturated alkyd resin, 100 parts of vinyltoluene, 2 parts of tert-butyl hydroperoxide trimethyl-cyclohexane, fat hydrocarbon
375 parts of solvent naphtha, 0.2 part of cobalt iso-octoate, 1.6 parts of zirconium iso-octoate；Wherein, unsaturated alkyd resin by following parts by weight original
Material is made: 100 parts of phthalic anhydride, 40 parts of pentaerythrite, 14 parts of trimethylolethane, 50 parts of tung oil fatty acid, soya-bean oil rouge
60 parts, 35 parts of three phosphonitriles of 2,4,6- triphenol oxygroup -2,4,6 three (hydroxyl-oxethyl) ring of fat acid.
Flame retardant type alkyd resin insulated paint the preparation method is as follows:
(1) 100 parts of phthalic anhydride, 40 parts of pentaerythrite, trihydroxy methyl are added into the first reaction kettle equipped with water segregator
14 parts of ethane, 30 parts of tung oil fatty acid, 50 parts of soy(a)-bean oil fatty acid, are passed through nitrogen, start stirring, are warming up to 180 DEG C of dehydration esterifications
2h is reacted, then is warming up to 240 DEG C of high temperature esterification reactions, until being cooled to reaction solution after reaction solution acid value is 100mgKOH/g
180℃；
(2) three phosphonitrile of 2,4,6- triphenol oxygroup -2,4,6 three (hydroxyl-oxethyl) ring is added in the reaction solution obtained to step (1)
35 parts, 20 parts of tung oil fatty acid, 10 parts of soy(a)-bean oil fatty acid are warming up to 220 DEG C, after high temperature dehydration to acid value is 15mgKOH/g, eventually
It only reacts, when reacting liquid temperature is down to 60 DEG C or less, discharges up to unsaturated alkyd resin, it is spare.
(3) 150 parts and 100 parts of vinyltoluene of unsaturated alkyd resin are added into the second reaction kettle, is warming up to 120 DEG C
Afterwards, 2 parts of tert-butyl hydroperoxide trimethyl-cyclohexane are taken, average rate instills in reaction kettle, time for adding 3h, isothermal reaction；It negates
It answers liquid and is diluted to the resin solution containing 60% admittedly with fat hydrocarbon solvent oil, whether the viscosity for measuring resin solution as required reaches
To the mPa.s of 6000 mPa.s~8000, continue the constant temperature reaction for keeping the second reaction kettle if unqualified, if the tree
After the viscosity test of lipoprotein solution is qualified, reaction is terminated；
(4) reaction solution that cooling step (3) obtains, while 375 parts of fat hydrocarbon solvent oil is added, 60 DEG C or less are down to temperature
When, be added 0.2 part of cobalt iso-octoate, 1.6 parts of zirconium iso-octoate be mixed evenly up to flame retardant type alkyd resin insulated paint.
Embodiment 3
A kind of flame retardant type alkyd resin insulated paint, is made of the raw material with following parts by weight:
190 parts of unsaturated alkyd resin, 125 parts of vinyltoluene, 4 parts of tert-butyl hydroperoxide trimethyl-cyclohexane, fat hydrocarbon
400 parts of solvent naphtha, 0.5 part of cobalt iso-octoate, 2 parts of zirconium iso-octoate；Wherein, unsaturated alkyd resin by following parts by weight raw material
It is made: 60 parts of phthalic anhydride, 36 parts of pentaerythrite, 12 parts of trimethylolpropane, 32 parts of tung oil fatty acid, tall oil fatty
20 parts, 20 parts of three phosphonitriles of 2,4,6- tripropoxy -2,4,6 three (ethyl alcohol amido) ring of acid.
Flame retardant type alkyd resin insulated paint the preparation method is as follows:
(1) 60 parts of phthalic anhydride, 36 parts of pentaerythrite, trihydroxy methyl third are added into the first reaction kettle equipped with water segregator
12 parts of alkane, 32 parts of tung oil fatty acid, 10 parts of ready denier oil acid, are passed through nitrogen, start stirring, are warming up to 180 DEG C of dehydration esterifications
2h is reacted, then is warming up to 240 DEG C of high temperature esterification reactions, until being cooled to reaction solution after reaction solution acid value is 60mgKOH/g
180℃；
(2) three phosphonitrile 20 of 2,4,6- tripropoxy -2,4,6 three (ethyl alcohol amido) ring is added in the reaction solution obtained to step (1)
Part, 10 parts of ready denier oil acid are warming up to 220 DEG C, after high temperature dehydration to acid value is 8mgKOH/g, terminate reaction, reaction solution temperature
When degree is down to 60 DEG C or less, discharge up to unsaturated alkyd resin, it is spare.
(3) 190 parts and 125 parts of vinyltoluene of unsaturated alkyd resin are added into the second reaction kettle, is warming up to 120 DEG C
Afterwards, 4 parts of tert-butyl hydroperoxide trimethyl-cyclohexane are taken, average rate instills in reaction kettle, time for adding 3h, isothermal reaction；It negates
It answers liquid and is diluted to the resin solution containing 60% admittedly with fat hydrocarbon solvent oil, whether the viscosity for measuring resin solution as required reaches
To the mPa.s of 16000 mPa.s~20000, continue the constant temperature reaction for keeping the second reaction kettle if unqualified, if described
After the viscosity test of resin solution is qualified, reaction is terminated；
(4) reaction solution that cooling step (3) obtains, while 400 parts of fat hydrocarbon solvent oil is added, 60 DEG C or less are down to temperature
When, be added 0.5 part of cobalt iso-octoate, 2 parts of zirconium iso-octoate be mixed evenly up to flame retardant type alkyd resin insulated paint.
Comparative example 1
Patent CN103275604A discloses a kind of preparation method of phosphorous alkyd resin transparent fire-resisting paint, and steps are as follows:
(1) 28 parts of behenic acid, 7.6 parts of pentaerythrite, 4.8 parts and 3 parts of phthalic anhydride are added in the four-hole boiling flask of 100ml
Dimethylbenzene.Logical nitrogen, opens stirring, slowly heats up.(180 DEG C are heated in 30-40min).The sound that oil splashes is begun at 160 DEG C
Sound, and there is backflow phenomenon.System is turbid solution.20min system is reacted after 170 DEG C of temperature becomes micro- glistening yellow clear liquid.Work as body
It is to start to keep the temperature 40min when temperature reaches 180 DEG C.4.9 parts of DOPOMA being added portionwise in 10min after heat preservation.It has fed
200 DEG C of insulation reaction 30min are to slowly warm up to after finishing, then are to slowly warm up to 210 DEG C, final 5 reaction temperature of heat preservation is 210-
220 DEG C (can not be rapidly heated to 220 DEG C, to avoid boiling explosion phenomenon).With the progress of reaction, system color is gradually deepened,
It eventually becomes orange red.Acid value is measured every half an hour after insulation reaction 2 hours, when acid value is 10mgKOH/g or so
Phosphorous alkyd resin can be obtained in stopping heating, cooling, discharging；
(2) in 50g 200# solvent naphtha, 3g cobalt iso-octoate, 10g manganese iso-octoate, 10g zirconium iso-octoate is added, in 3500r/min
Under the conditions of high speed dispersion 2h phosphorous alkyd resin transparent fire-resisting paint drier can be obtained；
(3) preparation of phosphorous alkyd resin transparent fire-resisting paint is by 7g200# solvent naphtha, 7g200# cyclohexanone, the phosphorous alkyd of 30g
20~40min of resin dispersion is added 1g drier and disperses after 10~20min up to product.
Comparative example 2
Patent CN104592814A discloses a kind of preparation method of coating compositions that insulate, specific as follows: by 100g cellulose nitre
Acid esters, 30g alkyd resin, 30g epoxy resin and 140g toluene are heated to 50 DEG C and stir to being completely dissolved, and obtain mixture
M1；It is double that 2g diethylenetriamine, 2g acrylic resin, 0.5g dimethyl silicone polymer, 0.5g vinyl are added into mixture M 1
Stearmide simultaneously stirs evenly, and obtains insulated paint A1.
Performance measurement
Modified alkyd resin composition made from embodiment 1 ~ 3 and comparison column 1 ~ 2 is tested for the property, including when drying
Between, flame retardant property, insulation performance and application performance, wherein；
Drying time, test was referring to national standard " GB/T1728-79 paint film, putty lacquer drying time measuring method "
The test of flame retardant property is referring to U.S.'s fire proofing standard ANSI/UL-94-1985
The test of electrical insulation capability is referring to " QJ 2220.3-1992 paint film electrical insulation capability test method "
The test method of application performance are as follows: modified alkyd resin composition is used as varnish, referring to national standard " GB/T1727-1992
Paint film is typically prepared method " preparing paint film, (insulation performance tests paint film preparation referring to " HG/T 3855-2006 insulated paint paint film system
Standby method " preparation), after film curing 7 days, the sample to be tested for the paint film for being about 15 μm with transparent thickness is obtained, according to " GB/
T6739-2006 paint and varnish pencil method measure hardness of paint film " measurement paint film hardness, according to " GB/T 1733-1993
Paint film water resistance measuring method " measure the water resistance of paint film, according to " GB/T 2423.17-2008 electric and electronic product environmental test
Second part: test method tests Ka: salt fog " salt fog resistance of measurement paint film, according to " GB/T 9216-1998 colored paint and clear
Paint the cross cut test of paint film " adhesive force of measurement paint film, measurement result is shown in Table 1；
Table 1
By table 1, it can be seen that, compared with comparative example 1 and comparison column 2, the flame retardant type alkyd resin insulated paint in the present invention has simultaneously
Better flame retardant effect and higher dielectric strength；And preparation method is simple, exempts from for protection circuit plate and its relevant device
By the erosion of environment, prolong the service life, it is ensured that the safety and reliability used.
Claims (10)
1. a kind of preparation method of flame retardant type alkyd resin insulated paint, it is characterised in that: preparing raw material includes unsaturated alkyd tree
Rouge, vinyltoluene, peroxide initiator, fat hydrocarbon solvent oil and drier, the preparation method is as follows:
(1) unsaturated alkyd resin and vinyltoluene is added into reaction kettle in proportion, after being warming up to 100~140 DEG C, to anti-
It answers and at the uniform velocity instills peroxide initiator in kettle, terminate reaction after reacting fluid viscosity qualification；
(2) reaction solution that cooling step (1) obtains, while fat hydrocarbon solvent oil is added, when temperature is down to 60 DEG C or less, add
Enter drier, is mixed and stirred for uniformly to get flame retardant type alkyd resin insulated paint；
Wherein, unsaturated alkyd resin the preparation method is as follows:
(1) binary acid, polyalcohol and fatty acid are added into reaction kettle, is passed through nitrogen, the acid value cooling of esterification to setting；
(2) it is added remaining fatty acid and three phosphazene derivative of hydroxyl ring, after the acid value of high temperature dehydration to setting, terminates anti-
It answers, when reacting liquid temperature is down to 60 DEG C or less, discharges up to unsaturated alkyd resin.
2. a kind of preparation method of flame retardant type alkyd resin insulated paint according to claim 1, it is characterised in that: preparing
When unsaturated alkyd resin, in step (1), high temperature esterification reaction temperature is 180~240 DEG C, set acid value as 50~
100mgKOH/g, cooling temperature are 170 ~ 180 DEG C；In step (2), high temperature dehydration temperature is 200~240 DEG C, sets acid value as 5
~15mgKOH/g.
3. a kind of preparation method of flame retardant type alkyd resin insulated paint according to claim 1, it is characterised in that: described two
First acid is phthalic acid, M-phthalic acid, succinic acid, tetrahydrophthalic acid, phthalic anhydride, pentamethylene -1,2- bis-
One or more of formic acid, hexanedioic acid, azelaic acid, preferably phthalic anhydride.
4. a kind of preparation method of flame retardant type alkyd resin insulated paint according to claim 1, it is characterised in that: described more
First alcohol is trihydroxylic alcohol and/or tetrahydroxylic alcohol.
5. a kind of preparation method of flame retardant type alkyd resin insulated paint according to claim 4, it is characterised in that: described four
First alcohol is pentaerythrite or D-sorbite；The trihydroxylic alcohol is glycerol, trimethylolpropane allyl ether, trimethylolethane
Or trimethylolpropane.
6. a kind of preparation method of flame retardant type alkyd resin insulated paint according to claim 1, it is characterised in that: fatty acid
For one of tung oil fatty acid, dehydrated castor oil fatty acid, Bristol oleic acid, linseed oil fatty acid, soya fatty acid or several
Kind.
7. a kind of preparation method of flame retardant type alkyd resin insulated paint according to claim 1, it is characterised in that: the rouge
Fat hydrocarbon solvent oil is low boiling point fat hydrocarbon solvent oil.
8. a kind of preparation method of flame retardant type alkyd resin insulated paint according to claim 1, it is characterised in that: described to contain
The structural formula of three phosphazene derivative of hydroxyl ring is as follows:
In formula, group R is the primary alkoxy of phenol oxygroup or 2 ~ 8 carbon atoms, preferably phenol oxygroup；
Group R1 is the hydroxy alkoxy base or ethyl alcohol amido of 2 ~ 4 carbon atoms, preferably ethyl alcohol amido.
9. a kind of preparation method of flame retardant type alkyd resin insulated paint according to claim 1, it is characterised in that: described to urge
Dry agent is metal ethylhexanoate salt, and the metal is one or more of cobalt, manganese, zirconium, zinc.
10. a kind of preparation method of flame retardant type alkyd resin insulated paint according to claim 1, it is characterised in that: described
Peroxide initiator is benzoyl peroxide, cumyl peroxide, tert-butyl hydroperoxide trimethyl-cyclohexane or peroxidating
Benzoic acid tert-butyl.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112480624A (en) * | 2019-09-11 | 2021-03-12 | 广东广山新材料股份有限公司 | Alkyd resin composition and preparation method and application thereof |
Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103102655A (en) * | 2012-12-31 | 2013-05-15 | 杭州福斯特光伏材料股份有限公司 | Inflaming retarding polyester film and preparation method thereof |
| CN103665358A (en) * | 2013-10-16 | 2014-03-26 | 上海大学 | Phosphorus-nitrogen copolyester material containing cyclotriphosphonitrile group and preparation method thereof |
| CN103992353A (en) * | 2014-05-04 | 2014-08-20 | 常州大学 | Flame retardant hexabutanol cyclotriphosphazene, and preparation method and application thereof |
| CN105062296A (en) * | 2015-08-06 | 2015-11-18 | 惠州市安品新材料有限公司 | Preparation method of flame retardation hydroxyacid protection paint |
| CN107250267A (en) * | 2015-06-24 | 2017-10-13 | 科莱恩塑料和涂料有限公司 | Anticorrosive fire-retardant preparaton for thermoplastic polymer |
-
2018
- 2018-08-16 CN CN201810931562.6A patent/CN109135524A/en active Pending
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103102655A (en) * | 2012-12-31 | 2013-05-15 | 杭州福斯特光伏材料股份有限公司 | Inflaming retarding polyester film and preparation method thereof |
| CN103665358A (en) * | 2013-10-16 | 2014-03-26 | 上海大学 | Phosphorus-nitrogen copolyester material containing cyclotriphosphonitrile group and preparation method thereof |
| CN103992353A (en) * | 2014-05-04 | 2014-08-20 | 常州大学 | Flame retardant hexabutanol cyclotriphosphazene, and preparation method and application thereof |
| CN107250267A (en) * | 2015-06-24 | 2017-10-13 | 科莱恩塑料和涂料有限公司 | Anticorrosive fire-retardant preparaton for thermoplastic polymer |
| CN105062296A (en) * | 2015-08-06 | 2015-11-18 | 惠州市安品新材料有限公司 | Preparation method of flame retardation hydroxyacid protection paint |
Non-Patent Citations (1)
| Title |
|---|
| 游歌云等: "环三磷腈类阻燃剂的合成及应用研究进展", 《应用化学》 * |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112480624A (en) * | 2019-09-11 | 2021-03-12 | 广东广山新材料股份有限公司 | Alkyd resin composition and preparation method and application thereof |
| CN112480624B (en) * | 2019-09-11 | 2023-01-13 | 广东广山新材料股份有限公司 | Alkyd resin composition and preparation method and application thereof |
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