CN105062296B - A kind of preparation method of flame retardant type alkyd protective paint - Google Patents
A kind of preparation method of flame retardant type alkyd protective paint Download PDFInfo
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Abstract
The invention belongs to technical field of coatings, a kind of preparation method of flame retardant type alkyd protective paint is disclosed, the modified flame-retardant alkyd resin is mixed with organic solvent and drier, flame retardant type alkyd protective paint is obtained；Modified flame-retardant alkyd resin including unsaturated alkyd resin, styrene, phosphorous, nitrogen flame-retardant monomer raw material by preparing.The characteristics of flame retardant type alkyd protective paint of the present invention has good flame retardation effect in the application, colourity is low, salt spray resistance is protruded, can be used for the erosion of protection circuit plate and its relevant device from bad border, improves the safety and reliability used.
Description
Technical field
The present invention relates to technical field of coatings, and in particular to a kind of preparation method of flame retardant type alkyd protective paint.
Background technology
Alkyd resin by raw material of oil and vegetable oil, easy to process, wide in variety, cheap, its composition and property
Characteristic can be in very large range adjusted etc., coating, the film forming matter of paint is mainly used as, the paint film of formation is glossy, tough
Property, adhesive force it is strong, and with good wearability and insulating properties, be widely used to space flight and aviation, military project, consumption electronic product
Deng field.But alkyd resin is inflammable, flame retardant treatment is had to pass through when using.
At present, it is that halogen flame is added in resin or coating or phosphorous is had to improve fire resistance most common method
Machine or inorganic combustion inhibitor, addition halogen containing flame-retardant can obtain obvious flame retardant effect, but can be discharged containing chlorine or bromine in burning
Toxic gas, have seriously polluted to surrounding air；Phosphorous, nitrogen the organic or inorganic fire retardant of addition, its consumption is usual
It is larger, other degradations of material can be caused, such as rate of drying is slack-off, transparency reduction, and pushing away over time
Move, flame retardant molecule can be migrated, is lost in, cause material flame retardant effect to reduce or lose.
The mode that phosphorous or nitrogen combustion inhibitor is participated in into resins synthesis as reactant can avoid additive flame retardant from existing
The problem of, such as CN103275604A discloses phosphorous alkyd resin transparent fire-resisting paint and preparation method thereof, and its scheme is in high score
Anti-flammability P elements are introduced in subchain, the fire protecting performance of paint film is improved, but the color of resin prepared is very deep, colorimeter method test
Its colourity >=12, is unfavorable for its application in the preparation of the materials such as varnish.
The content of the invention
In order to solve the problem of above-mentioned prior art is present, the present invention provides a kind of preparation side of flame retardant type alkyd protective paint
Method, flame retardant type alkyd protective paint prepared by the present invention includes modified Flame-retardant alkyd resin, is passed through by unsaturated alkyd resin
It is modified what is obtained including phosphorous, nitrogen flame-retardant monomer, makes protective paint that there is excellent fire resistance, and colourity is low, salt spray resistance
It is excellent.
The technical solution adopted by the present invention is：
A kind of preparation method of flame retardant type alkyd protective paint, preparing raw material includes modified flame-retardant alkyd resin, organic solvent
And drier, the modified flame-retardant alkyd resin is mixed with organic solvent and drier, flame retardant type alkyd protective paint is obtained；
The modified flame-retardant alkyd resin is by including unsaturated alkyd resin, styrene, phosphorous, nitrogen flame-retardant monomer raw material
It is prepared by the method through comprising the following steps：
Unsaturated alkyd resin, styrene, phosphorous, nitrogen flame-retardant monomer are mixed, 120~140 DEG C are warming up to, with styrene
It is 100 mass parts meters with phosphorous, nitrogen flame-retardant monomer quality sum, adds 0.5-1 mass parts radical initiators, reacts 1-
1.5h, then adds 0.5-1 mass parts radical initiators, reacts 1-1.5h, adds the initiation of 1.5-2.5 mass parts free radical
Agent, reacts 3~8h, reaches 7000mPas~9000mPas to reaction fluid viscosity, cools, obtain modified flame-retardant alkyd tree
Fat；
Phosphorous, nitrogen flame-retardant monomer the structure is as shown in Equation 1：
Formula 1
In formula 1, n is 1-16 natural number.
Preferably, in the formula 1, n is 3-12 natural number.
Preferably, first part of radical initiator is equal with the quality of second part of radical initiator.It is described to add
During radical initiator and reaction, the temperature of reaction system is controlled at 120~140 DEG C.
The viscosity reference《GB/T 7193.1-1987 unsaturated polyester resin viscosity measurements》Determine.
Preferably, the addition 1.5-2.5 mass parts radical initiators are point of 2-4 times additions, adjacent to add twice
Time interval is 0.5~1h.
The radical initiator is peroxide initiator, including but not limited to cumyl peroxide, tert-butyl group mistake
Aoxidize trimethyl-cyclohexane or the perbenzoic acid tert-butyl group.
Preferably, the modified flame-retardant alkyd resin including following raw material by mass percentage by preparing：
Unsaturated alkyd resin 48%~60%
Styrene 32%~46%
Phosphorous, nitrogen flame-retardant monomer 5%~8%.
Preferably, the unsaturated alkyd resin is the reaction product for including following reactant：
The unrighted acid includes 50~70 parts of the aliphatic acid containing conjugated double bond, the aliphatic acid containing conjugated double bond
For dehydrated castor oil fatty acid and/or tung oil fatty acid.
The binary acid can also be dicarboxylic anhydride, selected from phthalic acid, M-phthalic acid, phthalic anhydride, amber
One or more in acid, tetrahydrophthalic acid, pentamethylene -1,2- dioctyl phthalate, hexanedioic acid, azelaic acid.
The polyalcohol is trihydroxylic alcohol and/or tetrahydroxylic alcohol, and the trihydroxylic alcohol is glycerine, trimethylolethane or trihydroxy methyl
Propane, the tetrahydroxylic alcohol includes but is not limited to pentaerythrite or D-sorbite.
The monoacid is saturation monoacid or the monoacid containing aryl, and the saturation monoacid includes but is not limited to new penta
One or more in acid, laurate, stearic acid, the monoacid containing aryl be tetrahydrochysene benzoic acid, 4- p t butylbenzoic acids,
One or more in cyclopentane-carboxylic acid, 2,4- mesitylenic acids, 2- methyl benzoic acids and benzoic acid.
The unrighted acid is the aliphatic acid containing carbon-carbon double bond in molecule, including the aliphatic acid containing conjugated double bond,
Also include the one or more in palmitoleic acid, oleic acid, castor oil acid, linseed oil fatty acid, soy(a)-bean oil fatty acid.
Preferably, the unsaturated alkyd resin is prepared by the method comprised the following steps：
Binary acid, monoacid, polyalcohol, unrighted acid and dehydrating agent are added into reaction vessel, in logical nitrogen bar
180 DEG C~200 DEG C reaction 1-2.5h are warming up under part, then are warming up to 230 DEG C~250 DEG C reactions, 8- is reached to acid number
20mgKOH/g, cooling, obtains unsaturated alkyd resin.
The reaction at 180 DEG C~200 DEG C is reacted for dehydration esterification, is high temperature esterification in 230 DEG C~250 DEG C of reactions
It is required to the water for reacting generation removing reaction system in reaction, course of reaction, such as by way of water knockout drum is condensed.It is described
Cooling is to be down to room temperature to 60 DEG C.
The dehydrating agent includes but is not limited to benzene, toluene and dimethylbenzene, and its consumption is 10~12 parts.
Preferably, the number-average molecular weight of the unsaturated alkyd resin is 1500~3500.
The organic solvent includes but is not limited to benzene, dimethylbenzene, butyl acetate, 200# solvent naphthas, preferably 200# solvent naphthas,
Its consumption accounts for the 45-55% of the flame retardant type alkyd protective paint gross mass.
The drier can be drier known in the art, and including but not limited to cobalt, zirconium, calcium, zinc and manganese is various
Salt, can be the mixing of a variety of drier, the preferably one or more in cobalt iso-octoate, manganese iso-octoate or zirconium iso-octoate.Institute
The mixture that drier is preferably cobalt iso-octoate, manganese iso-octoate and zirconium iso-octoate is stated, its consumption modified flame-retardant alkyd resin quality
0.18-0.24%.
The colourity of the flame retardant type alkyd protective paint prepared by the present invention is 2-4.The colourity presses Gardner Gardener
Colorimeter method is determined.
By the flame retardant type alkyd protective paint of the present invention and suitable coating additive, such as levelling agent, wetting agent, dispersant,
Thickener, defoamer, stabilizer, pigment etc. are mixed, and can obtain the coating or paint for meeting corresponding construction and performance requirement.
The beneficial effects of the invention are as follows：The present invention carries out grafting processing using radical polymerization to unsaturated alkyd resin,
Introduce phosphorous, nitrogen side chain in the molecule, obtain modified flame-retardant alkyd resin, be remarkably improved resin fire resistance and
Stability, and then the flame retardant type alkyd protective paint of low colourity is obtained, available for protection circuit plate and its relevant device from ring
The erosion in border, improves and increases the service life, it is ensured that the safety and reliability used, and preparation method is simple.
Embodiment
The present invention is further detailed specific embodiment given below.
Phosphorous, nitrogen flame-retardant monomer the structural formula that the embodiment of the present invention 1,2 is used is：
Phosphorous, nitrogen flame-retardant monomer the structural formula used in embodiment 3 is：
The phosphorous of the present invention, nitrogen flame-retardant monomer are prepared with reference to prior art：
By 4- aminostyryls 0.4g, catalyst (for 0.18g sodium hydroxides and the mixture of 0.5g pyridines) and four chlorinations
Carbon 7.5g mixing is added in reactor, and 3-4mmol dialkyl phosphite and 4g carbon tetrachloride, time for adding control is slowly added dropwise
System is in 2-3h, and reaction temperature is maintained at 0-9 DEG C of reaction 35-40h, and solvent and accessory substance is distilled off, and column chromatography is divided in filtering
From purification, phosphorous, nitrogen flame-retardant monomer is obtained, reaction equation is：
In addition, in following examples, the method for testing of acid number is reference《GB/T 2895-2008 plastic polyester resin portions
The measure of acid number and total acid number》, the test reference of viscosity《GB/T 7193.1-1987 unsaturated polyester resins viscosimetric analysis side
Method》Carry out, number-average molecular weight is determined using gel permeation chromatography, and INSTRUMENT MODEL is SW-105, the mobile phase used is tetrahydrochysene furan
Mutter, standard specimen is polystyrene, sample concentration is 10mg/ml, basic parameter setting：Column oven temperature：40℃；Pump discharge：1ml/
min；Using Isocratic clution.
Drier is added by drier solution in following examples, and the preparation method of drier solution is：In 78.4g
1.8g cobalt iso-octoates, 1.8g manganese iso-octoates and 18g zirconium iso-octoates are added in 200# solvent naphthas, under the conditions of 3500r/min at a high speed
Scattered 2h, obtains drier solution.
Embodiment 1
The preparation method of flame retardant type alkyd protective paint is：
To equipped with addition phthalic anhydride 40g, trimethylolpropane in water knockout drum, condenser, the reaction bulb of agitator
45g, dehydrated castor oil fatty acid 60g, linseed oil fatty acid 62g, benzoic acid 5g and dimethylbenzene 11g, in the bar of maintaining nitrogen purge
Under part, 180 DEG C of dehydration esterification reaction 2h are warming up to, then are warming up to 240 DEG C of progress high temperature esterification reactions, 10mg is reached to acid number
KOH/g, stops reaction, is cooled to 60 DEG C, obtains unsaturated alkyd resin, and its number-average molecular weight is 1780；
Take unsaturated alkyd resin 150g, styrene 135g, phosphorous, nitrogen flame-retardant monomer 15g to add in reaction bulb, be warming up to
140 DEG C, 0.75g cumyl peroxides are added, 1h is reacted, 0.75g cumyl peroxides are then added, 1h is reacted, then will
3g cumyl peroxides are divided into 4 parts of additions, and the time interval of adjacent two parts of additions is 1h, and last portion reacts after adding
4h, 8400mPas~8600mPas is reached to viscosity, obtains modified flame-retardant alkyd resin, adds 200# solvent naphtha 250g,
60 DEG C are cooled to, drier solution 3.3g is added, stirs, obtain flame retardant type alkyd protective paint.
Embodiment 2
The preparation method of flame retardant type alkyd protective paint is：
To equipped with added in water knockout drum, condenser, the reaction bulb of agitator phthalic anhydride 45g, pentaerythrite 26g,
Trimethylolpropane 20g, dehydrated castor oil fatty acid 50g, soy(a)-bean oil fatty acid 65g, benzoic acid 7g and dimethylbenzene 12g, in normal temperature
Under logical condition of nitrogen gas, 180 DEG C of dehydration esterification reaction 1h are warming up to, 240 DEG C of progress high temperature esterification reactions are warming up to again afterwards, to acid
Value reaches 10mgKOH/g, is cooled to 60 DEG C, obtains unsaturated alkyd resin, and it is 2250 to test its number-average molecular weight；
Take unsaturated alkyd resin 144g, styrene 138g, phosphorous, nitrogen flame-retardant monomer 18g to be added in reaction bulb, heat up
To 140 DEG C, cumyl peroxide 0.78g is added, 1h is reacted, cumyl peroxide 0.78g is then added, 1h is reacted, then
3.9g cumyl peroxides are divided into 3 parts of additions, the time interval of adjacent two parts of additions is 1h, and last portion is anti-after adding
5h is answered, 8400mPas~8600mPas is reached to viscosity, modified flame-retardant alkyd resin is obtained, 200# solvent 250g, drop is added
Temperature adds drier solution 3g, stirs, obtain flame retardant type alkyd protective paint to 60 DEG C.
Embodiment 3
The preparation method of flame retardant type alkyd protective paint is：
To equipped with added in water knockout drum, condenser, the reaction bulb of agitator phthalic anhydride 35g, pentaerythrite 29g,
Dehydrated castor oil fatty acid 66g, linseed oil fatty acid 84g and dimethylbenzene 12g, under conditions of maintaining nitrogen purge, are warming up to 200
DEG C dehydration esterification reaction 1h, is warming up to 250 DEG C of progress high temperature esterification reactions, reaches 8mgKOH/g to acid number, stop reaction afterwards,
60 DEG C are cooled to, unsaturated alkyd resin is obtained, it is 2920 to test its number-average molecular weight.
Take unsaturated alkyd resin 180g, styrene 96g, phosphorous, nitrogen flame-retardant monomer 24g to add in reaction bulb, be warming up to
120 DEG C, tert-butyl hydroperoxide trimethyl-cyclohexane 0.73g is added, 1.5h is reacted, tert-butyl hydroperoxide front three basic ring is then added
Hexane 0.73g, reacts 1.5h, adds tert-butyl hydroperoxide trimethyl-cyclohexane 2.94g, reacts 7.5h, is reached to viscosity
7000mPas~7500mPas, obtains modified flame-retardant alkyd resin, adds 200# solvent oil solvent 250g, is cooled to 60
DEG C, drier solution 2.6g is added, stirs, obtains flame retardant type alkyd protective paint.
Testing example
Performance test is carried out to flame retardant type alkyd protective paint prepared by embodiment 1~3, it is specific as follows：
Drying time：With reference to national standard《GB/T1728-79 paint films, putty lacquer drying time determination method》；
Fire resistance：In long 12.7cm, wide 1.27cm pours into flame retardant type alkyd protective paint in thick 1.5mm model, dried
Sample is obtained after 7 days, with reference to U.S.'s fire proofing standard ANSI/UL-94-1985 fire resistances；
Colourity：Determined by Gardner Gardener colorimeter methods；
By flame retardant type alkyd protective paint with reference to national standard《GB/T1727-1992 paint films are typically prepared method》Prepare paint film, solidification 7
After it, obtain carrying the testing sample that transparent thickness is about 15 μm of paint film, according to《GB/T6739-2006 paint and varnish
Pencil method determines hardness of paint film》The hardness of paint film is determined, according to《GB/T 1733-1993 paint film water resistance determination methods》Determine paint
The water resistance of film, according to《GB/T 2423.17-2008 electric and electronic product environmental test Part II：Test method tests Ka：
Salt fog》Determine the salt fog resistance of paint film；
Adhesive force：According to《The cross cut test of GB/T 9216-1998 paint and varnish paint films》Determine adhesive force；
Insulating properties：Reference《HG/T 3855-2006 insulated paint paint film prepares method》Sample is prepared, according to《QJ 2220.3-
1992 paint film electrical insulation capability method of testings》Determine the electrical insulation capability of paint film.
Data are shown in Table 1.
Table 1
From the data in table 1, it can be seen that flame retardant type alkyd protective paint prepared by the present invention includes unsaturated alkyd resin through fire-retardant list
Modifies obtained resin, makes protective paint have salt spray resistance, good water resistance, good flame retardation effect, colourity low in the application
The characteristics of, and preparation method is simple, for protection circuit plate and its relevant device from the erosion of environment, increases the service life,
Ensure the safety and reliability used.
Above content is to combine specific preferred embodiment further description made for the present invention, it is impossible to assert
The specific implementation of the present invention is confined to these explanations.For general technical staff of the technical field of the invention,
On the premise of not departing from present inventive concept, some simple deduction or replace can also be made, should all be considered as belonging to the present invention's
Protection domain.
Claims (6)
1. a kind of preparation method of flame retardant type alkyd protective paint, preparing raw material include modified flame-retardant alkyd resin, organic solvent and
Drier, the modified flame-retardant alkyd resin is mixed with organic solvent and drier, obtains flame retardant type alkyd protective paint；
The modified flame-retardant alkyd resin is by including unsaturated alkyd resin, styrene, and phosphorous, nitrogen flame-retardant monomer raw material is through bag
It is prepared by the method for including following steps：
By unsaturated alkyd resin, styrene, phosphorous, nitrogen flame-retardant monomer mixing is warming up to 120~140 DEG C, with styrene with containing
Phosphorus, the quality sum of nitrogen flame-retardant monomer are 100 mass parts meters, add 0.5-1 mass parts radical initiators, react 1-1.5h,
Then 0.5-1 mass parts radical initiators are added, 1-1.5h is reacted, adds 1.5-2.5 mass parts radical initiators, instead
3~8h is answered, 7000mPas~9000mPas is reached to reaction fluid viscosity, cools, obtain modified flame-retardant alkyd resin；
Phosphorous, nitrogen flame-retardant monomer the structure is as shown in Equation 1：
In formula 1, n is 1-16 natural number,
The unsaturated alkyd resin is the reaction product comprising following reactant according to the mass fraction：
The unrighted acid includes 50~70 parts of the aliphatic acid containing conjugated double bond, and the aliphatic acid containing conjugated double bond is de-
Water Castor Oil Fatty Acid and/or tung oil fatty acid,
The colourity of the flame retardant type alkyd protective paint is 2-4,
The modified flame-retardant alkyd resin including following raw material by mass percentage by preparing：
Unsaturated alkyd resin 48%~60%
Styrene 32%~46%
Phosphorous, nitrogen flame-retardant monomer 5%~8%.
2. the preparation method of flame retardant type alkyd protective paint as claimed in claim 1, it is characterised in that the binary acid is adjacent benzene
One in dioctyl phthalate, M-phthalic acid, butanedioic acid, tetrahydrophthalic acid, pentamethylene -1,2- dioctyl phthalate, hexanedioic acid, azelaic acid
Plant or several, or be phthalic anhydride.
3. the preparation method of flame retardant type alkyd protective paint as claimed in claim 1, it is characterised in that the polyalcohol is ternary
Alcohol and/or tetrahydroxylic alcohol, the trihydroxylic alcohol are glycerine, trimethylolethane or trimethylolpropane, and the tetrahydroxylic alcohol is Ji Wusi
Alcohol.
4. the preparation method of flame retardant type alkyd protective paint as claimed in claim 1, it is characterised in that the unrighted acid
For the one or more in palmitoleic acid, oleic acid, castor oil acid, linseed oil fatty acid, soy(a)-bean oil fatty acid.
5. the preparation method of flame retardant type alkyd protective paint as claimed in claim 1, it is characterised in that the unsaturated alkyd tree
Fat is prepared by the method comprised the following steps：
Binary acid, monoacid, polyalcohol, unrighted acid and dehydrating agent are added into reaction vessel, under logical condition of nitrogen gas
180 DEG C~200 DEG C reaction 1-2.5h are warming up to, then are warming up to 230 DEG C~250 DEG C reaction to acid numbers and reach 8-20mgKOH/g, are dropped
Temperature, obtains unsaturated alkyd resin.
6. the preparation method of flame retardant type alkyd protective paint as claimed in claim 1, it is characterised in that the unsaturated alkyd tree
The number-average molecular weight of fat is 1500~3500.
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| CN109880068B (en) * | 2018-04-09 | 2021-06-04 | 鹤山市肇能新材料有限公司 | Autocatalytic alkyd resin and preparation method thereof |
| CN109135524A (en) * | 2018-08-16 | 2019-01-04 | 东莞市万维电子科技有限公司 | A kind of preparation method of flame retardant type alkyd resin insulated paint |
| CN109082232A (en) * | 2018-08-16 | 2018-12-25 | 东莞市万维电子科技有限公司 | A kind of flame retardant type alkyd resin insulated paint |
| CN111349379A (en) * | 2018-12-20 | 2020-06-30 | 艾伦塔斯电气绝缘材料(珠海)有限公司 | Tri-proof paint with reactive fluorescence and preparation method thereof |
| CN110894285A (en) * | 2019-12-07 | 2020-03-20 | 合众（佛山）化工有限公司 | Oleyl polyether-2 phosphate modified waterborne alkyd flame-retardant resin and preparation method thereof |
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| EP1749071B1 (en) * | 2004-05-25 | 2016-07-06 | Akzo Nobel Coatings International BV | Coating composition comprising a vinyl modified alkyd resin |
| CN103275604B (en) * | 2013-06-26 | 2015-05-20 | 兰州理工大学 | Phosphorous alkyd resin transparent fire retardant coating and preparation method thereof |
| CN103539814A (en) * | 2013-09-12 | 2014-01-29 | 江苏雅克科技股份有限公司 | Fire retardant containing styrene structure and phosphorus and nitrogen elements and synthetic method thereof |
| CN104804626A (en) * | 2014-01-24 | 2015-07-29 | 程威军 | Fire retardation three-proofing lacquer and preparation method thereof |
| CN104130660A (en) * | 2014-07-25 | 2014-11-05 | 惠州市强达电子工业有限公司 | Three-proofing covering paint and preparation method thereof |
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