CN101831061B - Benzoic acid modified waterborne alkyd resin and amino plastic baking varnish prepared by same - Google Patents
Benzoic acid modified waterborne alkyd resin and amino plastic baking varnish prepared by same Download PDFInfo
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- CN101831061B CN101831061B CN2010101688788A CN201010168878A CN101831061B CN 101831061 B CN101831061 B CN 101831061B CN 2010101688788 A CN2010101688788 A CN 2010101688788A CN 201010168878 A CN201010168878 A CN 201010168878A CN 101831061 B CN101831061 B CN 101831061B
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- benzoic acid
- modified waterborne
- acid modified
- resin
- pigment
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- WPYMKLBDIGXBTP-UHFFFAOYSA-N benzoic acid Chemical compound OC(=O)C1=CC=CC=C1 WPYMKLBDIGXBTP-UHFFFAOYSA-N 0.000 title claims abstract description 195
- 239000005711 Benzoic acid Substances 0.000 title claims abstract description 95
- 235000010233 benzoic acid Nutrition 0.000 title claims abstract description 95
- 229920000180 alkyd Polymers 0.000 title claims abstract description 55
- 239000002966 varnish Substances 0.000 title abstract description 7
- 239000004033 plastic Substances 0.000 title description 2
- 125000002924 primary amino group Chemical group [H]N([H])* 0.000 title description 2
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 31
- 229920003180 amino resin Polymers 0.000 claims abstract description 11
- 239000000049 pigment Substances 0.000 claims description 66
- 239000002253 acid Substances 0.000 claims description 53
- 229920005989 resin Polymers 0.000 claims description 47
- 239000011347 resin Substances 0.000 claims description 47
- ZMANZCXQSJIPKH-UHFFFAOYSA-N Triethylamine Chemical compound CCN(CC)CC ZMANZCXQSJIPKH-UHFFFAOYSA-N 0.000 claims description 43
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 42
- 125000003368 amide group Chemical group 0.000 claims description 42
- 239000002002 slurry Substances 0.000 claims description 41
- 239000003795 chemical substances by application Substances 0.000 claims description 35
- 238000003756 stirring Methods 0.000 claims description 32
- POAOYUHQDCAZBD-UHFFFAOYSA-N 2-butoxyethanol Chemical compound CCCCOCCO POAOYUHQDCAZBD-UHFFFAOYSA-N 0.000 claims description 24
- 239000006185 dispersion Substances 0.000 claims description 16
- 230000003472 neutralizing effect Effects 0.000 claims description 16
- 238000005303 weighing Methods 0.000 claims description 16
- 229920000877 Melamine resin Polymers 0.000 claims description 15
- 239000004640 Melamine resin Substances 0.000 claims description 14
- 239000003054 catalyst Substances 0.000 claims description 13
- 239000002318 adhesion promoter Substances 0.000 claims description 12
- 239000007788 liquid Substances 0.000 claims description 12
- 239000004576 sand Substances 0.000 claims description 12
- XGJZQNMUVTZITK-UHFFFAOYSA-N 2-n,2-n,4-n,4-n,6-n,6-n-hexamethoxy-1,3,5-triazine-2,4,6-triamine Chemical compound CON(OC)C1=NC(N(OC)OC)=NC(N(OC)OC)=N1 XGJZQNMUVTZITK-UHFFFAOYSA-N 0.000 claims description 10
- 239000011521 glass Substances 0.000 claims description 9
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 8
- 239000000203 mixture Substances 0.000 claims description 7
- UQSXHKLRYXJYBZ-UHFFFAOYSA-N Iron oxide Chemical compound [Fe]=O UQSXHKLRYXJYBZ-UHFFFAOYSA-N 0.000 claims description 6
- 235000011114 ammonium hydroxide Nutrition 0.000 claims description 6
- 238000009413 insulation Methods 0.000 claims description 6
- 238000003801 milling Methods 0.000 claims description 6
- ARXJGSRGQADJSQ-UHFFFAOYSA-N 1-methoxypropan-2-ol Chemical compound COCC(C)O ARXJGSRGQADJSQ-UHFFFAOYSA-N 0.000 claims description 5
- ZEMPKEQAKRGZGQ-AAKVHIHISA-N 2,3-bis[[(z)-12-hydroxyoctadec-9-enoyl]oxy]propyl (z)-12-hydroxyoctadec-9-enoate Chemical compound CCCCCCC(O)C\C=C/CCCCCCCC(=O)OCC(OC(=O)CCCCCCC\C=C/CC(O)CCCCCC)COC(=O)CCCCCCC\C=C/CC(O)CCCCCC ZEMPKEQAKRGZGQ-AAKVHIHISA-N 0.000 claims description 5
- LNYYKKTXWBNIOO-UHFFFAOYSA-N 3-oxabicyclo[3.3.1]nona-1(9),5,7-triene-2,4-dione Chemical compound C1=CC(C(=O)OC2=O)=CC2=C1 LNYYKKTXWBNIOO-UHFFFAOYSA-N 0.000 claims description 5
- LRHPLDYGYMQRHN-UHFFFAOYSA-N N-Butanol Chemical compound CCCCO LRHPLDYGYMQRHN-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
- SRPWOOOHEPICQU-UHFFFAOYSA-N trimellitic anhydride Chemical compound OC(=O)C1=CC=C2C(=O)OC(=O)C2=C1 SRPWOOOHEPICQU-UHFFFAOYSA-N 0.000 claims description 5
- 239000006229 carbon black Substances 0.000 claims description 4
- 229910052757 nitrogen Inorganic materials 0.000 claims description 4
- 239000001038 titanium pigment Substances 0.000 claims description 4
- QFFVPLLCYGOFPU-UHFFFAOYSA-N barium chromate Chemical compound [Ba+2].[O-][Cr]([O-])(=O)=O QFFVPLLCYGOFPU-UHFFFAOYSA-N 0.000 claims description 3
- KUCOHFSKRZZVRO-UHFFFAOYSA-N terephthalaldehyde Chemical group O=CC1=CC=C(C=O)C=C1 KUCOHFSKRZZVRO-UHFFFAOYSA-N 0.000 claims description 3
- 241001062009 Indigofera Species 0.000 claims description 2
- QQVIHTHCMHWDBS-UHFFFAOYSA-N isophthalic acid Chemical class OC(=O)C1=CC=CC(C(O)=O)=C1 QQVIHTHCMHWDBS-UHFFFAOYSA-N 0.000 claims description 2
- 238000002360 preparation method Methods 0.000 abstract description 19
- 238000000034 method Methods 0.000 abstract description 18
- 239000002904 solvent Substances 0.000 abstract description 10
- 230000008901 benefit Effects 0.000 abstract description 4
- CWYNVVGOOAEACU-UHFFFAOYSA-N Fe2+ Chemical compound [Fe+2] CWYNVVGOOAEACU-UHFFFAOYSA-N 0.000 abstract description 3
- 238000010276 construction Methods 0.000 abstract description 3
- 238000004519 manufacturing process Methods 0.000 abstract description 2
- 238000005201 scrubbing Methods 0.000 abstract description 2
- 231100000331 toxic Toxicity 0.000 abstract description 2
- 230000002588 toxic effect Effects 0.000 abstract description 2
- 239000000853 adhesive Substances 0.000 abstract 1
- 230000001070 adhesive effect Effects 0.000 abstract 1
- 230000007547 defect Effects 0.000 abstract 1
- 239000002994 raw material Substances 0.000 description 11
- 239000003973 paint Substances 0.000 description 10
- 238000000576 coating method Methods 0.000 description 7
- 239000011248 coating agent Substances 0.000 description 6
- FPAFDBFIGPHWGO-UHFFFAOYSA-N dioxosilane;oxomagnesium;hydrate Chemical compound O.[Mg]=O.[Mg]=O.[Mg]=O.O=[Si]=O.O=[Si]=O.O=[Si]=O.O=[Si]=O FPAFDBFIGPHWGO-UHFFFAOYSA-N 0.000 description 6
- 230000007613 environmental effect Effects 0.000 description 4
- 238000005259 measurement Methods 0.000 description 2
- 239000003960 organic solvent Substances 0.000 description 2
- 230000035939 shock Effects 0.000 description 2
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 description 1
- 150000007513 acids Chemical class 0.000 description 1
- 230000001680 brushing effect Effects 0.000 description 1
- 238000001514 detection method Methods 0.000 description 1
- 238000007599 discharging Methods 0.000 description 1
- 239000002612 dispersion medium Substances 0.000 description 1
- 238000001035 drying Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 239000002360 explosive Substances 0.000 description 1
- 238000009434 installation Methods 0.000 description 1
- 239000002932 luster Substances 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 230000001473 noxious effect Effects 0.000 description 1
- 238000007789 sealing Methods 0.000 description 1
- 238000003860 storage Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 230000004083 survival effect Effects 0.000 description 1
- 235000010215 titanium dioxide Nutrition 0.000 description 1
- 239000002699 waste material Substances 0.000 description 1
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Abstract
The invention discloses a benzoic acid modified waterborne alkyd resin and a preparation method thereof and also discloses an application of the benzoic acid modified waterborne alkyd resin in preparing benzoic acid modified waterborne alkyd amino resin baking varnish and an application method thereof. The benzoic acid modified waterborne alkyd amino resin baking varnish as waterborne baking varnish for ferrous products has the advantages of good stability and convenient, safe construction, no toxic solvents releasing, and the like, also has good gloss, weather resistance, water resistance, acid-base resistance, scrubbing resistance, high adhesive force and impact resistance after forming a film and is superior to the traditional solvent-based baking varnish in combination property; and in addition, the invention overcomes the defects of low hardness and poor gloss of the traditional waterborne alkyd resin and has simple and easy manufacturing process, is environmental-friendly and saves the energy by using water as a solvent.
Description
(1) technical field
The present invention relates to a kind of benzoic acid modified waterborne alkyd resin, and use the benzoic acid modified waterborne alcohol acid amido resin baking vanish of said benzoic acid modified waterborne alkyd resin preparation.
(2) background technology
Along with the progress in social development and epoch, people's environmental consciousness is more and more stronger, and industry environmental protection requires also increasingly high; At present, domestic ferrous products all uses solvent based coating, although solvent based coating has many good qualities; But the discharging of VOC all the time can't be up to standard, and the volatilization of organic solvent has caused great threat to the environment of human survival, not only in production, storage, transportation and construction process, is prone to cause inflammable, explosive and the toxic and harmful effusion; There is very big potential safety hazard; And along with the high speed development of industry, this pollution will be on the rise.In addition, the raw material of solvent based coating has 75% to come from petrochemical complex, and along with the growing tension of international energy, with an organic solvent not only cost rises, and causes great waste.
The coating that with water is solvent or dispersion medium is called water base (property) coating.Water resource price is cheap, the source is abundant, not only environmental protection, and also safe in utilization, have significant social and economic benefit.Water-base resin is the water-borne coatings most important component; Aqueous alkide resin is the maximum resin of present usage quantity; It has low price; Advantages such as good brushing property and wettability, its paint film of coating that the aqueous alkide resin of the non-modified of using always on the market at present makes often exist shortcomings such as difference of hardness, gloss are low, have limited its use range.
(3) summary of the invention
The objective of the invention is to prepare the high firmness modified waterborne alkyd amino-stoving varnish that various aspects of performance specifications such as hardness is big, gloss is high, sticking power all meet or exceed solvent-borne type baking vanish technical indicator.
The technical scheme that the present invention adopts is:
A kind of benzoic acid modified waterborne alkyd resin, described benzoic acid modified waterborne alkyd resin prepares as follows: Viscotrol C and TriMethylolPropane(TMP) under nitrogen protection, are heated to 180 ℃ of reaction 1.5h; Add isophthalic anhydride, phenylformic acid and esterifying catalyst then, and water trap is installed, continue to be heated to 220～230 ℃; Insulation reaction, tracking monitor reaction system acid number is low to moderate 10mgKOH/g to the system acid number; Cool to 140～150 ℃; Adding trimellitic anhydride, is 50～55mgKOH/g at 170～180 ℃ of following insulation reaction to acid numbers, is cooled to 100 ℃; Add solubility promoter 1, neutralizing agent 1, reaction 0.5～1h makes said benzoic acid modified waterborne alkyd resin; The mass ratio of said Viscotrol C, TriMethylolPropane(TMP), isophthalic anhydride, phenylformic acid, esterifying catalyst, trimellitic anhydride, solubility promoter 1, neutralizing agent 1 is 16～25: 17～27: 17～28: 3～6: 0.005～0.01: 4～7: 17～26: 5～9; Said esterifying catalyst is terephthaldehyde's acids esterifying catalyst or m-phthalic acid class esterifying catalyst (esterifying catalyst 4100 that preferred Guangzhou will one is produced); Said solubility promoter 1 is for being propyl carbinol, ethylene glycol monobutyl ether or propylene glycol monomethyl ether, preferred ethylene glycol monobutyl ether; Described neutralizing agent 1 is ammoniacal liquor, triethylamine or di-alcohol, preferred triethylamine.
Described benzoic acid modified waterborne alkyd resin can be applicable to prepare benzoic acid modified waterborne alcohol acid amido resin baking vanish.
Comparatively concrete, described benzoic acid modified waterborne alcohol acid amido resin baking vanish mainly is made up of the component of following mass parts:
2 12～28 parts of benzoic acid modified waterborne alkyd resins
4～8 parts in aminoresin
2 2～4 parts of neutralizing agents
1～3 part of adhesion promoter
2 6～18 parts of solubility promoters
17～40 parts of pigment slurrys
0.1～0.4 part of flow agent
0.1～0.4 part of skimmer
25～35 parts in water
Said pigment slurry is made up of the component of following mass parts:
118～50 parts of benzoic acid modified waterborne alkyd resins
10～60 parts of pigment
0.5～2.5 part of dispersion agent
3 17～37 parts of solubility promoters
Said aminoresin is melamine resin, methyl-etherified melamine resin or hexa methoxy melamine resin, preferred hexa methoxy melamine resin.
Said pigment is the combination of a kind of or any several kinds of arbitrary proportions in white titanium pigment, iron oxide red, organic indigo plant, carbon black or the permanent yellow.
Described solubility promoter 2 or solubility promoter 3 are independent separately to be propyl carbinol, ethylene glycol monobutyl ether or propylene glycol monomethyl ether, preferred ethylene glycol monobutyl ether.
Described neutralizing agent 2 is ammoniacal liquor, triethylamine or di-alcohol, preferred triethylamine.
Said adhesion promoter is the W-100 that HP-520 water-based adhesion promoter or BSK produce, the W-100 that preferred BSK produces.
Described dispersion agent is BYK-190 or BYK-191, preferred BYK-190.
Said skimmer is BYK-024 or Tego-830, preferred BYK-024.
Said flow agent is BYK-346, BYK-333 or BYK-381, preferred BYK-346.
Benzoic acid modified waterborne alkyd resin of the present invention 1 and benzoic acid modified waterborne alkyd resin 2 are meant the same benzoic acid modified waterborne alkyd resin that is provided by the present invention program; 1 and 2 is to be used for distinguishing benzoic acid modified waterborne alkyd resin to be in the different raw materials prescription, explains especially here.
Benzoic acid modified waterborne alcohol acid amido resin baking vanish of the present invention can also add sanitas, and described benzoic acid modified waterborne alcohol acid amido resin baking vanish preferably is made up of the component of following mass parts:
2 12～28 parts of benzoic acid modified waterborne alkyd resins
4～8 parts in aminoresin
2 2～4 parts of neutralizing agents
1～3 part of adhesion promoter
2 6～18 parts of solubility promoters
17～40 parts of pigment slurrys
1～15 part of talcum powder
0.1～0.4 part of flow agent
0.1～0.4 part of skimmer
25～35 parts in water.
Described benzoic acid modified waterborne alcohol acid amido resin baking vanish can also contain sanitas, and described benzoic acid modified waterborne alcohol acid amido resin baking vanish preferably is made up of the component of following mass parts:
2 12～28 parts of benzoic acid modified waterborne alkyd resins
4～8 parts in aminoresin
2 2～4 parts of neutralizing agents
1～3 part of adhesion promoter
2 6～18 parts of solubility promoters
17～40 parts of pigment slurrys
0.1～0.5 part of sanitas
0.1～0.4 part of flow agent
0.1～0.4 part of skimmer
25～35 parts in water
Described sanitas is KIL-200.
Preferred, described benzoic acid modified waterborne alcohol acid amido resin baking vanish preferably is made up of the component of following mass parts:
2 13.6 parts of benzoic acid modified waterborne alkyd resins
4.2 parts of hexa methoxy melamine resins
2 parts of triethylamines
2 parts of adhesion promoters
10.5 parts of ethylene glycol monobutyl ethers
37 parts of pigment slurrys
0.4 part of sanitas
0.2 part of BYK-346
0.1 part of BYK-024
30 parts in water
Said pigment slurry is made up of the component of following mass parts:
1 20.1 parts of benzoic acid modified waterborne alkyd resins
Pigment yellow 155 part
1 part of dispersion agent
23.9 parts of ethylene glycol monobutyl ethers
Further; Described benzoic acid modified waterborne alcohol acid amido resin baking vanish makes as follows: pigment slurry is produced in (1): take by weighing solubility promoter 3 and dispersion agent, benzoic acid modified waterborne alkyd resin 1, pigment by pigment slurry prescription amount; After mixing; Being ground to gained pigment fineness is (to measure the pigment fineness with Hegman grind gage usually) below the 15 μ m, obtains pigment slurry; (2) take by weighing all components beyond dewatering in the benzoic acid modified waterborne alcohol acid amido resin baking vanish prescription by the prescription amount, after stirring, add the water of prescription amount, obtain said benzoic acid modified waterborne alcohol acid amido resin baking vanish with filtered through gauze.
Concrete, described benzoic acid modified waterborne alcohol acid amido resin baking vanish can prepare by following method (A), method (B) or method (C):
Method (A); When not containing sanitas and talcum powder in the component: pigment slurry is produced in (1): take by weighing solubility promoter 3 by the prescription amount of pigment slurry and dissolve each other with the dispersion agent blend; Add then in the benzoic acid modified waterborne alkyd resin 1 of prescription amount, in the sand mill dispersion tank, under the rotating speed of 600～800r/min (preferred 700r/min), stirred 20～30 minutes; The pigment that adds the prescription amount then; Under the rotating speed of 2000～3000r/min (preferred 2500r/min), stir and pulverized 20～40 minutes, add granulated glass sphere (selecting diameter usually is the granulated glass sphere of 1.5mm and 2.5mm) again, under the rotating speed of 2500～3000r/min (preferred 2700r/min); Sand milling to pigment fineness is below the 15um, to obtain pigment slurry; (2) take by weighing benzoic acid modified waterborne alkyd resin 2, neutralizing agent 2 by the prescription amount, the back that stirs adds aminoresin, obtains mixed liquor A; Solubility promoter 2, skimmer, flow agent, adhesion promoter stir and obtain mixed liquid B; Mixed liquid B is added in the mixed liquor A; 2000～3000/min (preferred 2500r/min) rotating speed stirs 20～30min down; Add the pigment slurry that step (1) makes again; 600～800r/min (preferred 700r/min) rotating speed stirs 20～30min down, adds the water of prescription amount, filters with gauze (using 3400 purpose gauzes usually) and obtains said benzoic acid modified waterborne alcohol acid amido resin baking vanish.
Method (B); When containing sanitas in the component: pigment slurry is produced in (1): take by weighing solubility promoter 3 by the prescription amount of pigment slurry and dissolve each other with the dispersion agent blend; Add then in the benzoic acid modified waterborne alkyd resin 1 of prescription amount, in the sand mill dispersion tank, under the rotating speed of 600～800r/min (preferred 700r/min), stirred 20～30 minutes; The pigment that adds the prescription amount then; Under the rotating speed of 2000～3000r/min (preferred 2500r/min), stir and pulverized 20～40 minutes, add granulated glass sphere (selecting diameter usually is the granulated glass sphere of 1.5mm and 2.5mm) again, under the rotating speed of 2500～3000r/min (preferred 2700r/min); Sand milling to pigment fineness is below the 15um, to obtain pigment slurry; (2) take by weighing benzoic acid modified waterborne alkyd resin 2, neutralizing agent 2 by the prescription amount, the back that stirs adds aminoresin, obtains mixed liquor A; Solubility promoter 2, skimmer, flow agent, adhesion promoter, sanitas stir and obtain mixed liquid B; Mixed liquid B is added in the mixed liquor A; 2000～3000/min (preferred 2500r/min) rotating speed stirs 20～30min down; Add the pigment slurry that step (1) makes again; 600～800r/min (preferred 700r/min) rotating speed stirs 20～30min down, adds the water of prescription amount, filters with gauze (using 3400 purpose gauzes usually) and obtains said benzoic acid modified waterborne alcohol acid amido resin baking vanish;
Method (C); When containing talcum powder in the component: pigment slurry is produced in (1): take by weighing solubility promoter 3 by the prescription amount of pigment slurry and dissolve each other with the dispersion agent blend; Add then in the benzoic acid modified waterborne alkyd resin 1 of prescription amount, in the sand mill dispersion tank, under the rotating speed of 600～800r/min (preferred 700r/min), stirred 20～30 minutes; The pigment that adds the prescription amount then; Under the rotating speed of 2000～3000r/min (preferred 2500r/min), stir and pulverized 20～40 minutes, add granulated glass sphere (selecting diameter usually is the granulated glass sphere of 1.5mm and 2.5mm) again, under the rotating speed of 2500～3000r/min (preferred 2700r/min); Sand milling to pigment fineness is below the 15um, to obtain pigment slurry; (2) take by weighing benzoic acid modified waterborne alkyd resin 2, talcum powder, neutralizing agent 2 by the prescription amount, the back that stirs adds aminoresin, obtains mixed liquor A; Solubility promoter 2, skimmer, flow agent, adhesion promoter stir and obtain mixed liquid B; Mixed liquid B is added in the mixed liquor A; 2000～3000/min (preferred 2500r/min) rotating speed stirs 20～30min down; Add the pigment slurry that step (1) makes again; 600～800r/min (preferred 700r/min) rotating speed stirs 20～30min down, adds the water of prescription amount, filters with gauze (using 3400 purpose gauzes usually) and obtains said benzoic acid modified waterborne alcohol acid amido resin baking vanish.
Benzoic acid modified waterborne alcohol acid amido resin baking vanish provided by the invention is as ferrous products use baking vanish; Has good stability; Advantages such as easy construction, safety, no noxious solvent release have characteristics such as good luster, weather-proof, water-fast, acid and alkali-resistance, scrubbing resistance, sticking power be high, shock-resistant after the film forming, over-all properties is superior to conventional solvent type baking vanish; And overcome that traditional aqueous alkide resin hardness is low, the shortcoming of gloss difference; The preparation process is simple, is solvent with water, environmental protection, the saving energy.
(4) description of drawings
The preparation process schema of accompanying drawing 1 benzoic acid modified waterborne alcohol acid amido resin baking vanish
(5) embodiment
With specific embodiment technical scheme of the present invention is further described below, but protection scope of the present invention is not limited thereto:
Embodiment 1
A, preparation benzoic acid modified waterborne alkyd resin:
26g Viscotrol C and 30.1g TriMethylolPropane(TMP) under nitrogen protection, are heated to 180 ℃ of reaction 1.5h, add 24.5g isophthalic anhydride, 6g phenylformic acid and 0.007g terephthaldehyde acids esterifying catalyst (esterifying catalyst 4100 that will one trade Co., Ltd in Guangzhou produces) then; And the installation water trap, continue to be heated to 220 ℃, insulation reaction; Tracking monitor reaction system acid number is low to moderate 10mgKOH/g to the system acid number, cools to 150 ℃; Adding the 8g trimellitic anhydride, is 55mgKOH/g at 170 ℃ of following insulation reaction to acid numbers, is cooled to 100 ℃; Remove water trap and nitrogen; Add 28g ethylene glycol monobutyl ether, 11g triethylamine, reaction 0.5h makes benzoic acid modified waterborne alkyd resin 120g, and sealing is preserved for use.
B, preparation benzoic acid modified waterborne alcohol acid amido resin baking vanish, the raw material consumption is following:
Pigment slurry:
Benzoic acid modified waterborne alkyd resin 20.1g
White titanium pigment 55g
BYK-190 1g
Ethylene glycol monobutyl ether 23.9g
Benzoic acid modified waterborne alcohol acid amido resin baking vanish:
Benzoic acid modified waterborne alkyd resin 13.6g
Hexa methoxy melamine resin (Shunchang, Zhangjiagang 4.2g
Chemical industry ltd, down together)
Triethylamine 2g
The W-100 2g that BSK produces
Ethylene glycol monobutyl ether 10.5g
Pigment slurry 37g
KIL-200 0.4g
BYK-346 0.2g
BYK-024 0.1g
Water 30g
The preparation method is following: pigment slurry is produced in (1): take by weighing ethylene glycol monobutyl ether and the BYK-190 blend is dissolved each other by the raw material consumption; Add then in the 20.1g benzoic acid modified waterborne alkyd resin of steps A preparation, in the sand mill dispersion tank, under the rotating speed of 700r/min, stirred 20 minutes; Add pigment titanium white then; Under the rotating speed of 2500r/min, stir and pulverized 30 minutes, add the granulated glass sphere that diameter is 1.5mm and 2.5mm again, improve rotating speed to 2700r/min; Sand milling to pigment fineness is 14～15um (Hegman grind gage measurement), obtains pigment slurry; (2) take by weighing 13.6g benzoic acid modified waterborne alkyd resin, the triethylamine that steps A prepares by the raw material consumption, the back that stirs adds the hexa methoxy melamine resin, obtains mixed liquor A; Ethylene glycol monobutyl ether, BYK-024, BYK-346, BSK-w100, KIL-200 stir and obtain mixed liquid B; Mixed liquid B is added in the mixed liquor A; The 2500r/min rotating speed stirs 20min down, adds the pigment slurry that step (1) makes again, and the 700r/min rotating speed stirs 25min down; Add the water of prescription amount, obtain benzoic acid modified waterborne alcohol acid amido resin baking vanish 100g with 3400 purpose filtered through gauze.
Embodiment 2
Preparing method and step are with embodiment 1, and different is that the raw material consumption of preparation benzoic acid modified waterborne alcohol acid amido resin baking vanish is following among the step B:
Pigment slurry:
Benzoic acid modified waterborne alkyd resin 50g
Iron oxide red 30g
BYK-190 1.5g
Ethylene glycol monobutyl ether 18.5g
Benzoic acid modified waterborne alcohol acid amido resin baking vanish:
Benzoic acid modified waterborne alkyd resin 24.5g
Pigment slurry 18.8g
Hexa methoxy melamine resin 7.4g
Triethylamine 2g
The W-100 1.8g that BSK produces
Ethylene glycol monobutyl ether 15.2g
BYK-346 0.2g
BYK-024 0.1g
Water 30g
Other operations and condition make benzoic acid modified waterborne alcohol acid amido resin baking vanish 100g with embodiment 1.
Embodiment 3
Preparing method and step are with embodiment 1, and different is that the raw material consumption of preparation benzoic acid modified waterborne alcohol acid amido resin baking vanish is following among the step B:
Pigment slurry:
Benzoic acid modified waterborne alkyd resin 50g
Permanent yellow 20g
Ethylene glycol monobutyl ether 29.2g
BYK-190 0.8g
Benzoic acid modified waterborne alcohol acid amido resin baking vanish:
Benzoic acid modified waterborne alkyd resin 14.4g
Pigment slurry 31.5g
Hexa methoxy melamine resin 6.7g
Triethylamine 2g
The W-100 2.6g that BSK produces
Ethylene glycol monobutyl ether 12.5g
BYK-346 0.2g
BYK-024 0.1g
Water 30g
Other operations and condition make benzoic acid modified waterborne alcohol acid amido resin baking vanish 100g with embodiment 1.
Embodiment 4
The raw material consumption of preparation benzoic acid modified waterborne alcohol acid amido resin baking vanish is following among the step B:
Pigment slurry:
Benzoic acid modified waterborne alkyd resin 50g
Carbon black 11g
BYK-190 4g
Ethylene glycol monobutyl ether 35g
Benzoic acid modified waterborne alcohol acid amido resin baking vanish:
Benzoic acid modified waterborne alkyd resin 14.7g
Hexa methoxy melamine resin 7g
Triethylamine 2g
The W-100 1.5g that BSK produces
Ethylene glycol monobutyl ether 7g
Pigment slurry 24.5g
BYK-346 0.2g
BYK-024 0.1g
Talcum powder (Dongguan City three Feng Huagong ltds) 13g
Water 30g
A, preparation benzoic acid modified waterborne alkyd resin, the preparation method is with embodiment 1;
B, preparation benzoic acid modified waterborne alcohol acid amido resin baking vanish, the preparation method is following: pigment slurry is produced in (1): take by weighing ethylene glycol monobutyl ether with the BYK-190 blend is dissolved each other by the raw material consumption, add then in the 50g benzoic acid modified waterborne alkyd resin that steps A prepares; In the sand mill dispersion tank; Under the rotating speed of 700r/min, stirred 20 minutes, add the pigment carbon black then, under the rotating speed of 2500r/min, stir and pulverized 30 minutes; Add the granulated glass sphere that diameter is 1.5mm and 2.5mm again; Improve rotating speed to 2700r/min, sand milling to pigment fineness is 14～15um (Hegman grind gage measurement), obtains pigment slurry; (2) take by weighing 14.7g benzoic acid modified waterborne alkyd resin, talcum powder, the triethylamine that steps A prepares by the raw material consumption, the back that stirs adds the hexa methoxy melamine resin, obtains mixed liquor A; Ethylene glycol monobutyl ether, BYK-024, BYK-346, BSK-w100 stir and obtain mixed liquid B; Mixed liquid B is added in the mixed liquor A; The 2500r/min rotating speed stirs 20min down, adds the pigment slurry that step (1) makes again, and the 700r/min rotating speed stirs 25min down; Add the water of prescription amount, obtain benzoic acid modified waterborne alcohol acid amido resin baking vanish 100g with 3400 purpose filtered through gauze.
Embodiment 5
Preparing method and step are with embodiment 1, and different is that the raw material consumption of preparation benzoic acid modified waterborne alcohol acid amido resin baking vanish is following among the step B:
Pigment slurry:
Benzoic acid modified waterborne alkyd resin 20.1g
White titanium pigment 55g
BYK-190 1g
Ethylene glycol monobutyl ether 23.9g
Benzoic acid modified waterborne alcohol acid amido resin baking vanish:
Benzoic acid modified waterborne alkyd resin 13.6g
Melamine resin (Zhangjiagang Shunchang Chemical Co., Ltd) 4.2g
Ammoniacal liquor 2g
The W-100 2g that BSK produces
Ethylene glycol monobutyl ether 10.5g
Pigment slurry 37g
BYK-346 0.2g
BYK-024 0.1g
Water 30g
The benzoic acid modified waterborne alcohol acid amido resin baking vanish of getting embodiment 1～5 preparation detects, and detection method is following:
The paint film preparation is undertaken by the method for GB1727-92 regulation; Paint film appearance is tested by the method for GB1727-92 regulation; The paint film water resistance test carries out according to the method for GB/T1733-93 regulation; The paint film adhesion test is carried out according to the method for GB/T9286-1998 regulation; The test of paint film impact resistance is carried out according to the regulation of GB/T1732-93; The paint film pencil hardness test is undertaken by the method for GB/T6739-2006 regulation; Paint film weatherability (UV-light) test is carried out according to the method for GB/T1865-1997 regulation; The paint film flexibility test is undertaken by the method for GB/T1732-93 regulation.
Detected result such as following table 1:
Table 1: the technical indicator of benzoic acid modified waterborne alcohol acid amido resin baking vanish
| Title | Embodiment 1 | Embodiment 2 | Embodiment 3 | Embodiment 4 | Embodiment 5 |
| Paint film appearance | Smooth, smooth | Smooth, smooth | Smooth, smooth | Smooth, smooth | Smooth, smooth |
| Weathering resistance (UV-light) | ≥220h | ≤220h | ≤220h | ≤220h | ≤220h |
| Water tolerance (40 ℃ ± 2) | No change | No change | No change | No change | No change |
| Resistance to acids and bases 24h | No change | No change | No change | No change | No change |
| Gloss | 95 | 89 | 92 | 60 | 80 |
| Shock-resistant (kg.cm) | 50 | 50 | 50 | 50 | 50 |
| Snappiness (mm) | ≤2 | ≤2 | ≤2 | ≤2 | ≤2 |
| Pencil hardness (H) | 3 | 3 | 3 | 3 | 3 |
| Sticking power | 1 | 1 | 1 | 1 | 1 |
| Drying conditions | 140-150 ℃/30min | 140-150 ℃/30min | 140-150 ℃/30min | 140-150 ℃/30min | 140-150 ℃/30min |
Claims (9)
1. benzoic acid modified waterborne alkyd resin is characterized in that described benzoic acid modified waterborne alkyd resin prepares as follows: Viscotrol C and TriMethylolPropane(TMP) under nitrogen protection, are heated to 170～200 ℃ of reaction 1～3h; Add isophthalic anhydride, phenylformic acid and esterifying catalyst then, and water trap is installed, continue to be heated to 220～230 ℃; Insulation reaction, tracking monitor reaction system acid number is low to moderate 10mgKOH/g to the system acid number; Cool to 140～150 ℃; Adding trimellitic anhydride, is 50～55mgKOH/g at 170～180 ℃ of following insulation reaction to acid numbers, is cooled to 90～100 ℃; Add solubility promoter 1, neutralizing agent 1, reaction 0.5～1h makes said benzoic acid modified waterborne alkyd resin; The mass ratio of said Viscotrol C, TriMethylolPropane(TMP), isophthalic anhydride, phenylformic acid, esterifying catalyst, trimellitic anhydride, solubility promoter 1, neutralizing agent 1 is 16～25: 17～27: 17～28: 3～6: 0.005～0.01: 4～7: 17～26: 5～9; Said esterifying catalyst is terephthaldehyde's acids esterifying catalyst or m-phthalic acid class esterifying catalyst, and said solubility promoter 1 is propyl carbinol, ethylene glycol monobutyl ether or propylene glycol monomethyl ether; Described neutralizing agent 1 is ammoniacal liquor, triethylamine or di-alcohol.
2. benzoic acid modified waterborne alkyd resin as claimed in claim 1 is applied to prepare benzoic acid modified waterborne alcohol acid amido resin baking vanish.
3. application as claimed in claim 2 is characterized in that described benzoic acid modified waterborne alcohol acid amido resin baking vanish mainly is made up of the component of following mass parts:
Said pigment slurry is made up of the component of following mass parts:
Said aminoresin is melamine resin, methyl-etherified melamine resin or hexa methoxy melamine resin;
Said pigment is the combination of a kind of or any several kinds of arbitrary proportions in white titanium pigment, iron oxide red, organic indigo plant, carbon black or the permanent yellow;
Described solubility promoter 2 or solubility promoter 3 are independent separately to be propyl carbinol, ethylene glycol monobutyl ether or propylene glycol monomethyl ether;
Described neutralizing agent 2 is ammoniacal liquor, triethylamine or di-alcohol;
Said adhesion promoter is the W-100 that HP-520 water-based adhesion promoter or BSK produce.
4. application as claimed in claim 2 is characterized in that described benzoic acid modified waterborne alcohol acid amido resin baking vanish is made up of the component of following mass parts:
Described solubility promoter 2 is propyl carbinol, ethylene glycol monobutyl ether or propylene glycol monomethyl ether;
Described neutralizing agent 2 is ammoniacal liquor, triethylamine or di-alcohol.
5. application as claimed in claim 3 is characterized in that described dispersion agent is BYK-190 or BYK-191.
6. like the described application of one of claim 3～4, it is characterized in that said skimmer is BYK-024 or Tego-830.
7. like the described application of one of claim 3～4, it is characterized in that said flow agent is BYK-346, BYK-333 or BYK-381.
8. application as claimed in claim 3; It is characterized in that described benzoic acid modified waterborne alcohol acid amido resin baking vanish makes as follows: pigment slurry is produced in (1): by pigment slurry prescription amount take by weighing solubility promoter 3 with dispersion agent, benzoic acid modified waterborne alkyd resin 1, pigment, mix after; Being ground to gained pigment fineness is below the 15 μ m, obtains pigment slurry; (2) take by weighing all components beyond dewatering in the benzoic acid modified waterborne alcohol acid amido resin baking vanish prescription by the prescription amount, after stirring, add the water of prescription amount, obtain said benzoic acid modified waterborne alcohol acid amido resin baking vanish with filtered through gauze.
9. application as claimed in claim 3, it is characterized in that described benzoic acid modified waterborne alcohol acid amido resin baking vanish makes as follows: pigment slurry is produced in (1): take by weighing solubility promoter 3 by the prescription amount of pigment slurry and dissolve each other with the dispersion agent blend, add then in the benzoic acid modified waterborne alkyd resin 1 of prescription amount; In the sand mill dispersion tank; Under the rotating speed of 600～800r/min, stirred 20～30 minutes, add the pigment of prescription amount then, under the rotating speed of 2000～3000r/min, stir and pulverized 20～40 minutes; Add granulated glass sphere again; Under the rotating speed of 2500～3000r/min, sand milling to pigment fineness is below the 15 μ m, obtains pigment slurry; (2) take by weighing benzoic acid modified waterborne alkyd resin 2, neutralizing agent 2 by the prescription amount, the back that stirs adds aminoresin, obtains mixed liquor A; Solubility promoter 2, skimmer, flow agent, adhesion promoter stir and obtain mixed liquid B; Mixed liquid B is added in the mixed liquor A; 2000～3000r/min rotating speed stirs 20～30min down; Add the pigment slurry that step (1) makes again; 600～800r/min rotating speed stirs 20～30min down, adds the water of prescription amount, obtains said benzoic acid modified waterborne alcohol acid amido resin baking vanish with filtered through gauze.
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| CN2010101688788A CN101831061B (en) | 2010-05-11 | 2010-05-11 | Benzoic acid modified waterborne alkyd resin and amino plastic baking varnish prepared by same |
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|---|---|---|---|---|
| EP3728396B1 (en) * | 2017-12-20 | 2022-06-22 | Akzo Nobel Coatings International B.V. | Alkyd for pigment paste |
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| CN104513385A (en) * | 2014-12-04 | 2015-04-15 | 北京金汇利应用化工制品有限公司 | Preparation method for waterborne alkyd resin and aqueous dispersion thereof |
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| CN108912318B (en) * | 2018-07-13 | 2020-10-16 | 浙江启墨新材料科技有限公司 | Modified waterborne alkyd resin and baking varnish prepared from same |
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| CN110229537B (en) * | 2019-07-01 | 2021-05-11 | 黄山美森新材料科技股份有限公司 | Flame-retardant plastic-wood composite material with excellent water boiling resistance and preparation method thereof |
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