CN104194581B - A kind of low-temperature fast-curing aqueous impregnated insulating paint and preparation method thereof - Google Patents
A kind of low-temperature fast-curing aqueous impregnated insulating paint and preparation method thereof Download PDFInfo
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- CN104194581B CN104194581B CN201410381218.6A CN201410381218A CN104194581B CN 104194581 B CN104194581 B CN 104194581B CN 201410381218 A CN201410381218 A CN 201410381218A CN 104194581 B CN104194581 B CN 104194581B
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- 239000003973 paint Substances 0.000 title claims abstract description 27
- 238000002360 preparation method Methods 0.000 title claims abstract description 7
- 229920001568 phenolic resin Polymers 0.000 claims abstract description 59
- 239000005011 phenolic resin Substances 0.000 claims abstract description 54
- 239000002253 acid Substances 0.000 claims abstract description 47
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 31
- 229920002866 paraformaldehyde Polymers 0.000 claims abstract description 15
- 239000004971 Cross linker Substances 0.000 claims abstract description 14
- WSFSSNUMVMOOMR-UHFFFAOYSA-N formaldehyde Chemical compound O=C WSFSSNUMVMOOMR-UHFFFAOYSA-N 0.000 claims abstract description 14
- 125000002924 primary amino group Chemical group [H]N([H])* 0.000 claims abstract description 14
- SRPWOOOHEPICQU-UHFFFAOYSA-N trimellitic anhydride Chemical compound OC(=O)C1=CC=C2C(=O)OC(=O)C2=C1 SRPWOOOHEPICQU-UHFFFAOYSA-N 0.000 claims abstract description 14
- 229920000180 Alkyd Polymers 0.000 claims abstract description 10
- 150000001412 amines Chemical class 0.000 claims abstract description 10
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 10
- 239000003054 catalyst Substances 0.000 claims abstract description 6
- SLGWESQGEUXWJQ-UHFFFAOYSA-N formaldehyde;phenol Chemical compound O=C.OC1=CC=CC=C1 SLGWESQGEUXWJQ-UHFFFAOYSA-N 0.000 claims abstract description 5
- -1 phenol aldehyde Chemical class 0.000 claims abstract description 5
- 238000006243 chemical reaction Methods 0.000 claims description 35
- 238000003756 stirring Methods 0.000 claims description 30
- PEDCQBHIVMGVHV-UHFFFAOYSA-N glycerine Chemical compound OCC(O)CO PEDCQBHIVMGVHV-UHFFFAOYSA-N 0.000 claims description 21
- ZMANZCXQSJIPKH-UHFFFAOYSA-N triethylamine Chemical group CCN(CC)CC ZMANZCXQSJIPKH-UHFFFAOYSA-N 0.000 claims description 20
- 238000010792 warming Methods 0.000 claims description 20
- WNLRTRBMVRJNCN-UHFFFAOYSA-N Adipic acid Chemical compound OC(=O)CCCCC(O)=O WNLRTRBMVRJNCN-UHFFFAOYSA-N 0.000 claims description 16
- ISWSIDIOOBJBQZ-UHFFFAOYSA-N phenol Chemical compound OC1=CC=CC=C1 ISWSIDIOOBJBQZ-UHFFFAOYSA-N 0.000 claims description 14
- 238000006482 condensation reaction Methods 0.000 claims description 13
- 229960002887 Deanol Drugs 0.000 claims description 9
- UEEJHVSXFDXPFK-UHFFFAOYSA-N N-dimethylaminoethanol Chemical compound CN(C)CCO UEEJHVSXFDXPFK-UHFFFAOYSA-N 0.000 claims description 9
- QQVIHTHCMHWDBS-UHFFFAOYSA-N Isophthalic acid Chemical compound OC(=O)C1=CC=CC(C(O)=O)=C1 QQVIHTHCMHWDBS-UHFFFAOYSA-N 0.000 claims description 8
- 239000001361 adipic acid Substances 0.000 claims description 8
- 235000011037 adipic acid Nutrition 0.000 claims description 8
- JDSHMPZPIAZGSV-UHFFFAOYSA-N Melamine Chemical compound NC1=NC(N)=NC(N)=N1 JDSHMPZPIAZGSV-UHFFFAOYSA-N 0.000 claims description 6
- QIGBRXMKCJKVMJ-UHFFFAOYSA-N benzohydroquinone Chemical compound OC1=CC=C(O)C=C1 QIGBRXMKCJKVMJ-UHFFFAOYSA-N 0.000 claims description 6
- IISBACLAFKSPIT-UHFFFAOYSA-N Bisphenol A Chemical compound C=1C=C(O)C=CC=1C(C)(C)C1=CC=C(O)C=C1 IISBACLAFKSPIT-UHFFFAOYSA-N 0.000 claims description 5
- ZJCCRDAZUWHFQH-UHFFFAOYSA-N Trimethylolpropane Chemical compound CCC(CO)(CO)CO ZJCCRDAZUWHFQH-UHFFFAOYSA-N 0.000 claims description 5
- 229940106691 bisphenol A Drugs 0.000 claims description 5
- QWBBPBRQALCEIZ-UHFFFAOYSA-N 2,3-Dimethylphenol Chemical compound CC1=CC=CC(O)=C1C QWBBPBRQALCEIZ-UHFFFAOYSA-N 0.000 claims description 4
- FPYJFEHAWHCUMM-UHFFFAOYSA-N Maleic anhydride Chemical compound O=C1OC(=O)C=C1 FPYJFEHAWHCUMM-UHFFFAOYSA-N 0.000 claims description 4
- QXJQHYBHAIHNGG-UHFFFAOYSA-N Trimethylolethane Chemical compound OCC(C)(CO)CO QXJQHYBHAIHNGG-UHFFFAOYSA-N 0.000 claims description 4
- WMFOQBRAJBCJND-UHFFFAOYSA-M lithium hydroxide Chemical compound [Li+].[OH-] WMFOQBRAJBCJND-UHFFFAOYSA-M 0.000 claims description 4
- 238000000034 method Methods 0.000 claims description 4
- 239000000203 mixture Substances 0.000 claims description 4
- YNAVUWVOSKDBBP-UHFFFAOYSA-N morpholine Chemical compound C1COCCN1 YNAVUWVOSKDBBP-UHFFFAOYSA-N 0.000 claims description 4
- 229940113083 morpholine Drugs 0.000 claims description 4
- 229920003180 amino resin Polymers 0.000 claims description 2
- 239000003795 chemical substances by application Substances 0.000 claims description 2
- 238000004090 dissolution Methods 0.000 claims description 2
- 229940086542 triethylamine Drugs 0.000 claims description 2
- UHOVQNZJYSORNB-UHFFFAOYSA-N benzene Chemical compound C1=CC=CC=C1 UHOVQNZJYSORNB-UHFFFAOYSA-N 0.000 claims 4
- BDAGIHXWWSANSR-UHFFFAOYSA-N formic acid Chemical compound OC=O BDAGIHXWWSANSR-UHFFFAOYSA-N 0.000 claims 3
- 235000019253 formic acid Nutrition 0.000 claims 1
- DKGAVHZHDRPRBM-UHFFFAOYSA-N t-BuOH Chemical compound CC(C)(C)O DKGAVHZHDRPRBM-UHFFFAOYSA-N 0.000 claims 1
- 229920000728 polyester Polymers 0.000 abstract description 14
- 238000007711 solidification Methods 0.000 abstract description 7
- 238000010292 electrical insulation Methods 0.000 abstract 1
- 239000000376 reactant Substances 0.000 abstract 1
- 229920005989 resin Polymers 0.000 description 11
- 239000011347 resin Substances 0.000 description 11
- 238000007792 addition Methods 0.000 description 9
- 238000001816 cooling Methods 0.000 description 9
- 239000008367 deionised water Substances 0.000 description 9
- 239000003960 organic solvent Substances 0.000 description 5
- KKEYFWRCBNTPAC-UHFFFAOYSA-N Terephthalic acid Chemical compound OC(=O)C1=CC=C(C(O)=O)C=C1 KKEYFWRCBNTPAC-UHFFFAOYSA-N 0.000 description 3
- 230000015572 biosynthetic process Effects 0.000 description 3
- QGZKDVFQNNGYKY-UHFFFAOYSA-N ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 description 2
- 239000002585 base Substances 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 238000003786 synthesis reaction Methods 0.000 description 2
- 230000002194 synthesizing Effects 0.000 description 2
- 229920001225 Polyester resin Polymers 0.000 description 1
- 150000008065 acid anhydrides Chemical class 0.000 description 1
- 239000000853 adhesive Substances 0.000 description 1
- 230000001070 adhesive Effects 0.000 description 1
- 239000003513 alkali Substances 0.000 description 1
- 230000005591 charge neutralization Effects 0.000 description 1
- 239000011248 coating agent Substances 0.000 description 1
- 238000000576 coating method Methods 0.000 description 1
- 238000005336 cracking Methods 0.000 description 1
- 239000003431 cross linking reagent Substances 0.000 description 1
- 238000003912 environmental pollution Methods 0.000 description 1
- 235000019197 fats Nutrition 0.000 description 1
- 238000005755 formation reaction Methods 0.000 description 1
- 239000010842 industrial wastewater Substances 0.000 description 1
- 238000009413 insulation Methods 0.000 description 1
- 238000002386 leaching Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000006011 modification reaction Methods 0.000 description 1
- 230000001264 neutralization Effects 0.000 description 1
- 238000006386 neutralization reaction Methods 0.000 description 1
- 229920003986 novolac Polymers 0.000 description 1
- 238000010422 painting Methods 0.000 description 1
- 239000004645 polyester resin Substances 0.000 description 1
- 150000007519 polyprotic acids Polymers 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 230000001988 toxicity Effects 0.000 description 1
- 231100000419 toxicity Toxicity 0.000 description 1
- 235000015112 vegetable and seed oil Nutrition 0.000 description 1
- 235000019871 vegetable fat Nutrition 0.000 description 1
- 239000008158 vegetable oil Substances 0.000 description 1
Abstract
The present invention relates to low-temperature fast-curing impregnated insulating paint of a kind of aqueous and preparation method thereof, it is prepared by method by following component and obtains: prepare phenolic resin by phenol and paraformaldehyde under conditions of base catalyst is catalyzed, again by this phenolic resin and trihydroxylic alcohol, binary acid, trimellitic acid anhydride reactant, neutralize through amine again, add amino crosslinker and water, prepare the water alcohol acid polyester containing high-load phenolic resin.The insullac of the present invention has the performance of phenolic resin and alkyd polyester concurrently, and the more general alkyd resin of curing rate and phenol aldehyde modified alkyd resin are greatly improved, and solidification temperature is also reduced to 120 DEG C, and after solidification, mechanical performance and the electrical insulation properties of paint film are excellent.
Description
Technical field
The present invention relates to a kind of insullac and preparation method thereof, be specifically related to a kind of low-temperature fast-curing aqueous varnished insulation
Paint and preparation method thereof.
Background technology
Along with the consciousness of environmental conservation, production safety is gradually stepped up by society, water paint is being applied to each of society
Individual field.Volatile organic solvent in water consumption substitution coating has absolutely in terms of safety, cost, toxicity and environmental pollution
To advantage.But the resin of water paint must have water solublity or water dispersible.This point determines the resin of water paint
Molecular weight can not be made as the resin of solvent paint big, and water volatilize than organic solvent slow a lot, therefore water
Property paint usually have the shortcoming that the paint film after solidification is dry, intensity is low, weatherability is the best.
Waterborne polyester is a kind of resin relatively conventional in current aqueous impregnated insulating paint, although relatively with vegetable oil or fat
The standby alkyd resin of fat processed with acid has more preferable outdoor stability, hardness, elasticity and adhesive force, but it still has cured paint film to do
Dry slow shortcoming, especially toasts at middle low temperature 130 DEG C, is dried slow, therefore typically requires at about 150 DEG C baking 2-3 little
Time, the paint film of formation can be only achieved certain mechanical performance and weatherability.
Phenolic resin has good weatherability and hardness, but after pure phenolic resin curing, fragility is bigger, easily
Cracking, therefore should not be used alone.
The method that phenolic resin modified aqueous alkide resin is conventional is first to synthesize aqueous alkide resin, synthesizes at waterborne polyester
Latter stage, add organic solvent miscible with water and reduce viscosity, add phenolic resin and be modified at 120 ~ 150 DEG C instead
Should, after reaction terminates, cooling adds amine neutralization, and dilute dissolves.This way is simple to operate, but modified phenolic resin
Amount the most limited, consumption is many, can have a strong impact on the water solublity of resin, and the condition of modified-reaction is not easily controlled.If
Modification temperature is high, and time length can make the molecular weight of resin be significantly increased, thus affect water solublity, even gel.If changed
Degree warm in nature is low, and the time is short, and phenolic resin is not connected with polyester resin completely, when dilute, and free phenolic aldehyde
Resin will separate out, and causes painting dulling, the stability of paint is caused significant impact.The most this way must also add necessarily
The organic solvent of amount, otherwise during modified-reaction, viscosity can be very big, causes gel.
Summary of the invention
It is an object of the present invention to provide the leaching that a kind of aqueous containing high phenolic resin content is low-temperature fast-curing
Stain insullac.
The technical solution used in the present invention is:
A kind of low-temperature fast-curing aqueous impregnated insulating paint, described insullac is made up of the component of following percentage by weight:
Phenolic resin 14.0 ~ 22.0%；
Trihydroxylic alcohol 7.8 ~ 12.8%；
Binary acid 7.8 ~ 13.4%；
Trimellitic anhydride 3.4 ~ 4.6%；
Amine nertralizer 2.2 ~ 4.8%；
Amino crosslinker 8.2 ~ 12.0%；
Water 41.7 ~ 47.1%.
Wherein said water is preferably used deionized water.
Preferably, described phenolic resin by phenol, paraformaldehyde and base catalyst according to weight ratio 100:(15-40): (1-
3), make through phenol formaldehyde condensation reaction.
Preferably, described phenol is any one or a few in phenol, xylenol, hydroquinone, bisphenol-A, and described alkali is urged
Agent is any one in triethylamine, dimethylethanolamine, Lithium hydrate.
Preferably, one or more during described trihydroxylic alcohol is glycerol, trimethylolethane, trimethylolpropane；Described
Binary acid is one or more in M-phthalic acid, p-phthalic acid, adipic acid, maleic anhydride；Described amine nertralizer
It is one or more in triethylamine, dimethylethanolamine, morpholine.
Preferably, described amino crosslinker be the trade mark be Resimene747, Resimene717, Cymel 350,
One or more in the water soluble amino resin of Cymel327.
Preferably, described insullac is according to above-mentioned weight hundred by phenolic resin, trihydroxylic alcohol, binary acid and trimellitic anhydride
After proportion by subtraction reaction obtains alkyd resin, add amine nertralizer and neutralize, add amino crosslinker and water mixed dissolution forms.
Further object is that a kind of method that low-temperature fast-curing aqueous impregnated insulating paint is provided, the method
Comprise the following steps:
1) phenolic resin, trihydroxylic alcohol and binary acid are mixed, be warming up to 220 DEG C-240 DEG C；
2) testing procedure 1) the acid number of mixture, when acid number is 1-10mgKOH/g, cool the temperature to 150 DEG C-170
DEG C, add trimellitic anhydride, and maintain temperature, until acid number reaches 50 ~ 55mgKOH/g, be cooled to 80 DEG C-90 DEG C；
3) amine nertralizer is added, stirring, temperature is reduced to 50 DEG C-70 DEG C, adds amino crosslinker, after stirring,
Add water.
Preferably, the preparation method of described phenolic resin comprises the following steps:
A) phenol, paraformaldehyde and base catalyst are mixed, be warming up to 120 DEG C-140 DEG C and carry out phenol formaldehyde condensation reaction；
B) viscosity of the mixture of testing procedure a), when viscosity reaches 1200 ~ 1500cps@80 DEG C, cools the temperature to room
Temperature, obtains phenolic resin.
Selecting paraformaldehyde in step a), and the formalin that need not commonly use is raw material, can avoid producing substantial amounts of
Industrial wastewater；In addition polyformaldehyde reaction activity is high, and the production time is short.And it is one that viscosity reaches 1200 ~ 1500cps@80 DEG C
The most moderate reaction controlling parameter, viscosity controls low, easily has more unreacted free phenol, affects product quality,
The most not environmentally；Viscosity controls high, then prepare viscosity in the step of impregnated insulating paint below and be easily made too high, affect finished product
, even there is gel in the manufacturability of paint and water solublity.
The invention has the beneficial effects as follows:
The present invention by first novolak resin, then by phenolic resin with the polyprotic acid of other synthesis waterborne polyester and
Polyhydric alcohol carries out condensation reaction, synthesizes the waterborne polyester of a kind of high phenolic resin content based on phenolic resin.Same
As waterborne polyester and phenol aldehyde modified waterborne polyester compare, it can more fast low temperature cure, solidification temperature as little as 120
DEG C, hardening time is 90 minutes, and the mechanical strength after solidification is also greatly improved, and weatherability is obviously improved.
The present invention is by based on phenolic resin, and synthesis aqueous alkyd polyester on this basis, after making product solidification
Paint film has both the performance that environment resistant, the fast setting of the toughness of alkyd polyester, cementability and phenolic resin are dried；Simultaneously because
This system is in the synthetic reaction that phenolic resin participates directly in alkyd polyester, and it is one that phenolic resin and alkyd polyester melt completely
Body, it is to avoid some common faults of conventional phenolic resin modified aqueous alkide resin, such as: unstable, easy dulling, modified-reaction
Easily gel, phenolic resin consumption is limited, have to add part organic solvent etc..
Detailed description of the invention
Below in conjunction with specific embodiment, the present invention is expanded on further.
Embodiment 1
A: prepare phenolic resin:
By weight, take in phenol 100 parts, paraformaldehyde 30 parts, triethylamine 1.2 parts addition the first reactor, start
Stirring, is warming up to 130 DEG C and carries out condensation reaction；The viscosity of test reaction thing, until viscosity reaches 1200 ~ 1500cps@80 DEG C,
Cooling, terminates.Take on from the first reactor, standby.
B: the phenolic resin prepared by step A synthesizes product of the present invention
Take 100 parts of above-mentioned phenolic resin, glycerol 58 parts, M-phthalic acid 40 parts, adipic acid 10 parts addition the second reactor
In, start stirring, be warming up to 230 DEG C, the acid number of test reaction thing, until acid number is less than 10mgKOH/g, cool the temperature to 160
DEG C, adding trimellitic anhydride 18 parts, maintain still temperature 160 DEG C, the acid number of test reaction thing, until acid number is reduced to 50-
55mgKOH/g, cools the temperature to 85 DEG C, adds triethylamine 16 parts, stirs 30 minutes, and reduction still temperature, to 60 DEG C, adds 45 parts of ammonia
Based cross-linker Resimene 747, after stirring, adds deionized water 234 parts, obtains product of the present invention.
Embodiment 2
A: prepare phenolic resin:
By weight, take in xylenol 100 parts, paraformaldehyde 20 parts, triethylamine 1.5 parts addition the first reactor, open
Dynamic stirring, is warming up to 130 DEG C and carries out condensation reaction；The viscosity of test reaction thing, until viscosity reaches 1200 ~ 1500cps@80
DEG C, cooling, terminates.Take on from the first reactor, standby.
B: the phenolic resin prepared by step A synthesizes product of the present invention
Take 100 parts of above-mentioned phenolic resin, trimethylolpropane 42 parts, glycerol 20 parts, M-phthalic acid 40 parts, adipic acid 22
Part adds in the second reactor, starts stirring, is warming up to 230 DEG C, the acid number of test reaction thing, until acid number is less than 10mgKOH/
G, cools the temperature to 160 DEG C, addition trimellitic anhydride 24 parts, maintenance still temperature 160 DEG C, the acid number of test reaction thing, until acid number
It is reduced to 50-55mgKOH/g, cools the temperature to 85 DEG C, add dimethylethanolamine 27.5 parts, stir 30 minutes, reduce still temperature
To 60 DEG C, add 18 parts of amino crosslinker Resimene 717 and 40 parts of Cymel 350, after stirring, add deionized water
238.5 parts, obtain product of the present invention.
Embodiment 3
A: prepare phenolic resin:
By weight, phenol 100 parts, paraformaldehyde 40 parts, dimethylethanolamine 3.0 parts addition the first reactor are taken
In, start stirring, be warming up to 130 DEG C and carry out condensation reaction；The viscosity of test reaction thing, until viscosity reach 1200 ~
1500cps@80 DEG C, cooling, terminates.Take on from the first reactor, standby.
B: the phenolic resin prepared by step A synthesizes product of the present invention
Take 100 parts of above-mentioned phenolic resin, trimethylolethane 80 parts, M-phthalic acid 50 parts, adipic acid 20 parts add the
In two reactors, starting stirring, be warming up to 230 DEG C, the acid number of test reaction thing, until acid number is less than 10mgKOH/g, by temperature
Being down to 160 DEG C, add trimellitic anhydride 28 parts, maintain still temperature 160 DEG C, the acid number of test reaction thing, until acid number is reduced to 50-
55mgKOH/g, cools the temperature to 85 DEG C, adds morpholine 30 parts, stirs 30 minutes, and reduction still temperature, to 60 DEG C, adds 36 parts of amino
Cross-linking agent Cymel 350 and 20 parts of Cymel 327, after stirring, adds deionized water 260 parts, obtains product of the present invention.
Embodiment 4
A: prepare phenolic resin:
By weight, take in hydroquinone 100 parts, paraformaldehyde 38 parts, triethylamine 2.0 parts addition the first reactor,
Start stirring, be warming up to 130 DEG C and carry out condensation reaction；The viscosity of test reaction thing, until viscosity reaches 1200 ~ 1500cps@80
DEG C, cooling, terminates.Take on from the first reactor, standby.
B: the phenolic resin prepared by step A synthesizes product of the present invention
Take 100 parts of above-mentioned phenolic resin, trimethylolethane 72 parts, M-phthalic acid 30 parts, adipic acid 30 parts add the
In two reactors, starting stirring, be warming up to 230 DEG C, the acid number of test reaction thing, until acid number is less than 10mgKOH/g, by temperature
Being down to 160 DEG C, add trimellitic anhydride 23 parts, maintain still temperature 160 DEG C, the acid number of test reaction thing, until acid number is reduced to 50-
55mgKOH/g, cools the temperature to 85 DEG C, adds dimethylethanolamine 32 parts, stirs 30 minutes, and reduction still temperature, to 60 DEG C, adds
76.5 parts of amino crosslinker Cymel327, after stirring, add deionized water 300 parts, obtain product of the present invention.
Embodiment 5
A: prepare phenolic resin:
By weight, take bisphenol-A 20 parts, phenol 80 parts, paraformaldehyde 17 parts, Lithium hydrate 1.0 parts add first anti-
Answer in still, start stirring, be warming up to 130 DEG C and carry out condensation reaction；The viscosity of test reaction thing, until viscosity reach 1200 ~
1500cps@80 DEG C, cooling, terminates.Take on from the first reactor, standby.
B: the phenolic resin prepared by step A synthesizes product of the present invention
Take 100 parts of above-mentioned phenolic resin, glycerol 80 parts, M-phthalic acid 46.6 parts, adipic acid 20 parts addition the second reaction
In still, start stirring, be warming up to 230 DEG C, the acid number of test reaction thing, until acid number is less than 10mgKOH/g, cool the temperature to
160 DEG C, adding trimellitic anhydride 24.7 parts, maintain still temperature 160 DEG C, the acid number of test reaction thing, until acid number is reduced to 50-
55mgKOH/g, cools the temperature to 85 DEG C, adds morpholine 20 parts, stirs 30 minutes, and reduction still temperature, to 60 DEG C, adds 85.0 parts of ammonia
Based cross-linker Cymel327, after stirring, adds deionized water 335.0 parts, obtains product of the present invention.
Embodiment 6
A: prepare phenolic resin:
By weight, take in bisphenol-A 100 parts, paraformaldehyde 40 parts, triethylamine 1.0 parts addition the first reactor, open
Dynamic stirring, is warming up to 130 DEG C and carries out condensation reaction；The viscosity of test reaction thing, until viscosity reaches 1200 ~ 1500cps@80
DEG C, cooling, terminates.Take on from the first reactor, standby.
B: the phenolic resin prepared by step A synthesizes product of the present invention
Take 100 parts of above-mentioned phenolic resin, trimethylolpropane 36 parts, M-phthalic acid 30 parts, maleic anhydride 6 parts add
Enter in the second reactor, start stirring, be warming up to 230 DEG C, the acid number of test reaction thing, until acid number is less than 10mgKOH/g, will
Temperature is down to 160 DEG C, adds trimellitic anhydride 19 parts, maintains still temperature 160 DEG C, the acid number of test reaction thing, until acid number reduces
To 50-55mgKOH/g, cool the temperature to 85 DEG C, add dimethylethanolamine 18 parts, stir 30 minutes, reduction still temperature to 60 DEG C,
Add 45.3 parts of amino crosslinker Resimene 717, after stirring, add deionized water 208.3 parts, obtain the present invention and produce
Product.
Embodiment 7
A: prepare phenolic resin:
By weight, take 85 parts, 15 parts bisphenol-A paraformaldehydes of xylenol 25 parts, dimethylethanolamine 1.5 parts adds the
In one reactor, start stirring, be warming up to 130 DEG C and carry out condensation reaction；The viscosity of test reaction thing, until viscosity reaches 1200
~ 1500cps@80 DEG C, cooling, terminates.Take on from the first reactor, standby.
B: the phenolic resin prepared by step A synthesizes product of the present invention
Take 100 parts of above-mentioned phenolic resin, glycerol 56 parts, p-phthalic acid 40 parts, maleic anhydride 8 parts add second anti-
Answer in still, start stirring, be warming up to 230 DEG C, the acid number of test reaction thing, until acid number is less than 10mgKOH/g, cool the temperature to
160 DEG C, adding trimellitic anhydride 20.4 parts, maintain still temperature 160 DEG C, the acid number of test reaction thing, until acid number is reduced to 50-
55mgKOH/g, cools the temperature to 85 DEG C, adds triethylamine 24 parts, stirs 30 minutes, and reduction still temperature, to 60 DEG C, adds 64.3 parts
Amino crosslinker Cymel 350, after stirring, adds deionized water 278.7 parts, obtains product of the present invention.
Embodiment 8
A: prepare phenolic resin:
By weight, take in phenol 100 parts, paraformaldehyde 22.0 parts, Lithium hydrate 2.5 parts addition the first reactor,
Start stirring, be warming up to 130 DEG C and carry out condensation reaction；The viscosity of test reaction thing, until viscosity reaches 1200 ~ 1500cps@80
DEG C, cooling, terminates.Take on from the first reactor, standby.
B: the phenolic resin prepared by step A synthesizes product of the present invention
Take 100 parts of above-mentioned phenolic resin, trimethylolpropane 47.1 parts, glycerol 10 parts, p-phthalic acid 50 parts, adipic acid
35.7 parts add in the second reactor, start stirring, be warming up to 230 DEG C, and the acid number of test reaction thing, until acid number is less than
10mgKOH/g, cools the temperature to 160 DEG C, adds trimellitic anhydride 29.1 parts, maintains still temperature 160 DEG C, the acid of test reaction thing
Value, until acid number is reduced to 50-55mgKOH/g, cools the temperature to 85 DEG C, adds dimethylethanolamine 14.3 parts, stirs 30 points
Clock, reduction still temperature, to 60 DEG C, adds 52.4 parts of amino crosslinker Cymel327, after stirring, adds deionized water 300 parts,
Obtain product of the present invention.
Embodiment 9
Being tested by insullac product of the present invention for embodiment 1-8 gained, solidification temperature is reduced to 120 DEG C, hardening time
It is as short as 90min.And general waterborne polyester and phenol aldehyde modified waterborne polyester need to toast 2-3 hour at about 150 DEG C.Cause
This, the insullac of the present invention can more fast low temperature cure.
The related performance indicators of insullac of the present invention is listed in the table below.
From table 1, insullac various aspects of performance of the present invention is excellent.
Claims (7)
1. a low-temperature fast-curing aqueous impregnated insulating paint, it is characterised in that: described insullac is by following percentage by weight
Component is made:
Described insullac is the phenolic resin by above percentage ratio, trihydroxylic alcohol, binary acid hybrid reaction, adds trimellitic anhydride
After reaction obtains alkyd resin, add amine nertralizer and neutralize, add amino crosslinker and water mixed dissolution forms.
One the most according to claim 1 low-temperature fast-curing aqueous impregnated insulating paint, it is characterised in that: described phenolic aldehyde tree
Fat by phenol, paraformaldehyde and base catalyst according to weight ratio 100:(15-40): (1-3), make through phenol formaldehyde condensation reaction.
One the most according to claim 2 low-temperature fast-curing aqueous impregnated insulating paint, it is characterised in that: described phenol is benzene
Any one or a few in phenol, xylenol, hydroquinone, bisphenol-A, described base catalyst is triethylamine, dimethyl ethanol
Any one in amine, Lithium hydrate.
One the most according to claim 1 low-temperature fast-curing aqueous impregnated insulating paint, it is characterised in that: described trihydroxylic alcohol
It is one or more in glycerol, trimethylolethane, trimethylolpropane；Described binary acid is M-phthalic acid, to benzene two
One or more in formic acid, adipic acid, maleic anhydride；Described amine nertralizer is triethylamine, dimethylethanolamine, morpholine
In one or more.
One the most according to claim 1 low-temperature fast-curing aqueous impregnated insulating paint, it is characterised in that: described amino is handed over
Connection agent be the trade mark be in the water soluble amino resin of Resimene747, Resimene717, Cymel 350, Cymel327
Plant or several.
6. the method for a kind of low-temperature fast-curing aqueous impregnated insulating paint prepared described in claim 1, it is characterised in that:
Comprise the following steps:
1) phenolic resin, trihydroxylic alcohol and binary acid are mixed, be warming up to 220 DEG C-240 DEG C；
2) testing procedure 1) the acid number of mixture, when acid number is 1-10mgKOH/g, cools the temperature to 150 DEG C-170 DEG C, add
Enter trimellitic anhydride, and maintain temperature, until acid number reaches 50～55mgKOH/g, be cooled to 80 DEG C-90 DEG C；
3) amine nertralizer is added, stirring, temperature is reduced to 50 DEG C-70 DEG C, adds amino crosslinker, after stirring, add
Water.
A kind of method preparing low-temperature fast-curing aqueous impregnated insulating paint the most according to claim 6, it is characterised in that: institute
The preparation method stating phenolic resin comprises the following steps:
A) phenol, paraformaldehyde and base catalyst are mixed, be warming up to 120 DEG C-140 DEG C and carry out phenol formaldehyde condensation reaction；
B) viscosity of the mixture of testing procedure a), when viscosity reaches 1200～1500cps@80 DEG C, cools the temperature to room temperature,
Obtain phenolic resin.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201410381218.6A CN104194581B (en) | 2014-08-05 | A kind of low-temperature fast-curing aqueous impregnated insulating paint and preparation method thereof |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201410381218.6A CN104194581B (en) | 2014-08-05 | A kind of low-temperature fast-curing aqueous impregnated insulating paint and preparation method thereof |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN104194581A CN104194581A (en) | 2014-12-10 |
| CN104194581B true CN104194581B (en) | 2017-01-04 |
Family
ID=
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