CN1163560C - Durably anticorrosion paint and its preparing process - Google Patents
Durably anticorrosion paint and its preparing process Download PDFInfo
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- CN1163560C CN1163560C CNB001361872A CN00136187A CN1163560C CN 1163560 C CN1163560 C CN 1163560C CN B001361872 A CNB001361872 A CN B001361872A CN 00136187 A CN00136187 A CN 00136187A CN 1163560 C CN1163560 C CN 1163560C
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- anticorrosion paint
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Abstract
The present invention belongs to a preparing method of long-acting corrosion-proof paint. An epoxy alloy which is compounded from poly epoxy chloropropane epoxy resin and bisphenol A epoxy resin is used as a film forming substance, and water-resistance solvence-resistant filler with stable size is added in the epoxy alloy to form component A. Polybasic amine, an additional product of epoxypropyl alkyl ethers, liquid polyamide and trialkylamine are mixed to form a composite solidifying agent which is used as component B. The component A and the component B can be proportionally mixed when in use and construction can be carried out by a brush coating method, a roller coating method, a high-pressure spraying method, etc. The effective period of the paint can be more than ten years.
Description
Technical field
The invention belongs to the preparation method of durably anticorrosion paint.
Background technology
Because in seawater, expose to the weather in naval vessel, submarine long period of soaking, salt fog etch, seawater scouring, wave are bounced, not only difference variation is big, but also the influence that sea pressure changes will stand to navigate by water the time, operation condition is very abominable.Therefore particularly naval vessel self is added with the galvanic protection function, and to the performance requriements of impregnating material, key index has three: the one, and anti-cathodic disbonding, the 2nd, coating is to the tack of base material, and the 3rd, the usage period in different media is sex-limited.In product in the past, though the kind of protective system is a lot,, and respectively there is it long as chlorinated rubber, Resins, epoxy, vinyl resins etc., over-all properties is still not ideal enough.Even antiseptic property can satisfy service requirements, but shorter on the valid period of using.Having increased lists and indexes on the naval vessels repaiies number of times, has shortened the period of service.With the bottom anticorrosive paint is example, and the performance index of sticking power are 30kg/cm
2, be 12-30 month work-ing life.Such performance index are not enough for large ship and submarine.
Summary of the invention
The preparation method who the purpose of this invention is to provide a kind of durably anticorrosion paint, the epoxy alloy that selection is made up of Hydrin Resins, epoxy and bisphenol A epoxide resin is main film forming matter, add the filler that some have water tolerance, solvent resistance and dimensional stability, the common base-material of forming is the A component.Affixture by polyamine and epoxypropyl alkyl ether, and with liquid polymeric amide, tertiary amine etc. common to form composite curing agent be the B component, after mixing by a certain percentage during use, can brushing, roller coat, high pressure painting and do not have methods such as the spraying of pressure and hydraulic spraying and construct.
In the A component, the introducing of bisphenol A epoxide resin makes and contains enough characteristic groups in the film forming matter, has given chemical-resistant, tack, obdurability and the reactivity of material excellence.And Hydrin Resins, epoxy has the character of rubber and lower viscosity, its constitutional features is that epoxy group(ing), chloromethyl and ehter bond are arranged in the molecular structure, the good shock-resistance of material, cementability, solvent resistance and heat-resistant aging and good, isostatic mechanical property have been given in its introducing.In the B component, epoxypropyl alkyl oxide amine solidifying agent has been given material curing speed, hardness and lower viscosity faster, and good solvent resistance.Polyamide-based solidifying agent has been given the good tack of material, water tolerance and elasticity.
The epoxy alloy that adopts Hydrin Resins, epoxy and bisphenol A epoxide resin to form among the present invention is main film forming matter, and (the weight percentage %) of film forming matter is 60%-80%.
One, Hydrin Resins, epoxy solventless method is synthetic
1, ring-opening polymerization
Get 1.0 moles dibasic alcohol, specifically: wherein a kind of of ethylene glycol, propylene glycol, butyleneglycol, Diethylene Glycol, dipropylene glycol or hexylene glycol adds the catalyzer of (weight percentage %) 0.5～5% simultaneously; Catalyzer has: phosphorus hexafluoride triethyl oxonium salt, tin tetrachloride, boron trifluoride ethyl ether complex or boron trifluoride tetrahydrofuran complex; Drip the epoxy chloropropane of n mole then, n=10-25; Controlled temperature is at 50-80 ℃ of logical N
2Gas, stirring are incubated 4-8 hour, survey oxirane value=0;
2, ring-closure reaction
With 2.1～2.5 moles NaOH, be made into the solution of 30-40% concentration, be added drop-wise in the above-mentioned reaction, 80-90 ℃ of insulation 4-6 hour;
3, washing
Extremely neutral with 98-100 ℃ of deionized water wash, and the content of mensuration inorganic chlorine stopped washing at 0.05% o'clock;
4, dehydration is purified
The normal pressure distillation is taken off moisture content, continues dehydration then and measure water-content≤0.5% o'clock end under the 10-15mmHg vacuum, measures oxirane value, hydroxyl value and viscosity, promptly obtains Hydrin Resins, epoxy;
Two, the selection commercial goods of bisphenol A epoxide resin, range of choice: molecular weight is 380-1000, oxirane value is 0.51-0.2;
Three, filler selection: wherein one or more of titanium dioxide, carbon black, ferric oxide, kaolin, talcum powder, lime carbonate, ferric sulfate, silica flour or metal powder and pigment;
Four, the epoxypropyl alkyl ether amine is synthetic
Get the polyamine of 1.05-1.2 mole, specifically: wherein a kind of of divinyl propylamine, diethylenetriamine or triethylene tetramine, intensification 40-60 ℃, drip 1.0 moles epoxypropyl alkyl oxide then, specifically: n-butyl glycidyl ether, glycidyl allyl ether, styrene oxide or phenyl glycidyl ether.60-80 ℃ is incubated 4-8 hour;
Five, the preparation technology of coating
The preparation technology of A component
1, get bisphenol A epoxide resin, Hydrin Resins, epoxy, reactive thinner epoxypropyl alkyl oxide, three's weight percent is 40-50: 13-18: 3-10, heats 40-60 ℃ and stirring at low speed;
2,,, stir by the operation instruction input with dispersion agent, defoamer, oxidation inhibitor and stablizer;
3, solid packing and pigment are added in the container successively, fully wetting;
4, disperse with homogenizer, the beginning stirring at low speed, treat each mutually evenly after, carry out high speed dispersion;
5, be cooled to after the room temperature and grind two times with three-roll grinder, detect with Hegman grind gage and reach 20-50um and decide according to specific requirement, barrelling is finished product;
The preparation technology of B component
1, with the epoxypropyl alkyl ether amine, Versamid, three (dimethylamino methyl) phenol, phenylcarbinol drop in the container, and four weight percent is 26-35: 40-60: 4-5: 10-20;
2, intensification 30-40 ℃, stirring makes its thorough mixing even, reduces to room temperature, and barrelling is finished product;
A component: B component (weight ratio)=5.0: 1.0-1.5.
Paint film behind the crosslinking curing has formed the cross-linked state of interpenetrating(polymer)networks, makes it become insoluble infusible material, has showed very strong tack, chemical-resistant and shock resistance, and is nontoxic and have a flame retardant resistance.Be not only applicable to naval vessel, submarine; can also be widely used in the metallic structures of offshore platform, bridge spanning the sea, sea port dock; the inside and outside wall that also can be used for ground bridge, rail vehicle, cargo hold, freight container, oil transportation, gas transmission, water pipe particularly can be applied in the place that is added with galvanic protection or can forms galvanic corrosion naturally.Use valid period can reach more than 10 years.
Embodiment
Embodiment 1: Hydrin Resins, epoxy synthetic
On a 500mL reaction flask, stirring, condenser, thermometer charging opening and ventpipe are housed.Drop into ethylene glycol 12.4g, catalyzer boron trifluoride ethyl ether complex (weight percentage %) 3%, logical N
2, stir, drip epoxy chloropropane 187.6g, temperature is controlled at 50 ℃, is incubated 8 hours, surveys oxirane value=0.With 19.2gNaOH, be made into the solution of 40% concentration, drip in the above-mentioned reaction, and 80 ℃ of insulations 6 hours.To neutral, PH=7 measures content of inorganic chlorine=0.043% and o'clock stops washing with 99 ± 1 ℃ of deionized water wash.Will be above-mentioned product filter the back and drop in the 500ml matrass, first normal pressure dehydration liquid temperature reaches 100 ℃ (or beginning with 90 ℃ of water ring vacuum pump dehydration, liquid temperature), after change decompression dehydration into, the liquid temperature 90 ℃ when absence of liquid distillates, measure water-content=0.5% end.Cooling back discharging gets final product.
Embodiment 2:
In device, drop into butyleneglycol 18.42g, catalyzer boron trifluoride tetrahydrofuran complex (weight percent) 0.5%, logical N with example 1
2, stir.Drip epoxy chloropropane 282g, charge temperature is controlled at 50 ℃, heats up 80 ℃ then, is incubated 4 hours, surveys oxirane value=0.
With 20gNaOH, be made into the solution of 30% concentration, drip in above-mentioned reaction, and 90 ℃ of insulations 4 hours.To neutral, PH=7 measures content of inorganic chlorine=0.05% and o'clock stops washing with 99 ± 1 ℃ of deionized water wash.The purification of dewatering then, method is with embodiment 1.
Embodiment 3:
In device, drop into propylene glycol 15.2g, catalyzer boron trifluoride tetrahydrofuran complex (weight percentage %) 5%, logical N with example 1
2, stir.Drip epoxy chloropropane 384.8g, charge temperature is controlled at 50 ℃, is incubated 5 hours, surveys oxirane value=0.With 16.8gNaOH, be made into the solution of 40% concentration, drip in above-mentioned reaction, and 80 ℃ of insulations 6 hours.To neutral, PH=7 measures content of inorganic chlorine=0.048% and o'clock stops washing with 99 ± 1 ℃ of deionized water wash.The purification of dewatering then, method is with embodiment 1.
Embodiment 4: epoxypropyl alkyl ether amine synthetic
On a 500ml reaction flask, stirring, condenser, thermometer and charging opening are housed, drop into diethylenetriamine 108.2g, be warming up to 40 ℃, begin to drip glycidyl allyl ether 114g, 60 ℃ of insulations 8 hours heat up in the reinforced back that is over.Reduce to discharging after the room temperature.
Embodiment 5:
In device with example 3, drop into divinyl propylamine 109.2g, heat up 60 ℃, begin to drip n-butyl glycidyl ether 91g, heating up 80 ℃ in the reinforced back that is over, is incubated 4 hours.Reduce to discharging after the room temperature.
Embodiment 6: the preparation of coating
With bisphenol A epoxide resin E
44Shrink sweet 50g barite, 30g talcum powder of 560g, Hydrin Resins, epoxy 140g normal-butyl adds in the container, makes it fully wetting.Stirring at low speed makes each mutually even, carries out high-speed stirring after 30 minutes, disperses 30 minutes.After reducing to room temperature, grind twice, get final product when detecting fineness to 20um with three-roll grinder.
Embodiment 7:
With bisphenol A epoxide resin E
20165g, glycidyl allyl ether 50g, phenylcarbinol 45g drops in the container, heats up 60 ℃ to stir 30 minutes.And then input E
44236.5g Hydrin Resins, epoxy 148.5g stirs.With 2.5g defoamer EFKA2720,1.5g oxidation inhibitor JH1010, with the molten oxidation inhibitor of 7g toluene, 6g stabilizer T inuvin292, the 6g dispersion agent adds EFKA5065, adds in the said vesse to stir 10 minutes.Stop to stir, 120g titanium dioxide, 12g carbon black, 100g kaolin, 50g barite, 50g lime carbonate are added in the container, make it fully wetting.Stirring at low speed makes each mutually even, carries out high-speed stirring after 30 minutes, disperses 30 minutes.After reducing to room temperature, grind twice, get final product when detecting fineness=30um with three-roll grinder.
Embodiment 8:
With bisphenol A epoxide resin E
51504g, Hydrin Resins, epoxy 126g, n-butyl glycidyl ether 30g drops in the container, heats up 40 ℃, stirs 10 minutes.With 2.5g defoamer EFKA2720,3g oxidation inhibitor 900B, the molten oxidation inhibitor of 8g toluene; 6.5g stabilizer T inuvin292,6g dispersion agent EFKA5065 adds in the said vesse, stirs 10 minutes.Stop to stir, with the 150g red iron oxide, 94g kaolin, the 50g barite, 20g lime carbonate adds in the container, makes it fully wetting.Stirring at low speed makes each mutually even, carries out high-speed stirring after 30 minutes, disperses 30 minutes.After reducing to room temperature, grind twice, get final product when detecting fineness=50um with three-roll grinder.
Embodiment 9:
With bisphenol A epoxide resin E
20420g, n-butyl glycidyl ether 95g drops in the container, heats up 60 ℃ to stir 40 minutes.Then Hydrin Resins, epoxy 180g is dropped in the container, stir.With 2.5g defoamer EFKA2722,2.0g oxidation inhibitor 900B is with the molten oxidation inhibitor of 9g toluene; 6.5g stablizer UV-326 adds in the said vesse, stirs 10 minutes.Stop to stir, with the 200g red iron oxide, 50g kaolin, the 30g talcum powder, 5g lime carbonate adds in the container, makes it fully wetting.Stirring at low speed makes that each is mutually even, carries out high-speed stirring after 30 minutes, disperses to reduce in 30 minutes room temperature, grinds twice with three-roll grinder, gets final product during detection fineness=50um.
Embodiment 10: the preparation of solidifying agent
With 80g Versamid (amine value=400), 70g epoxypropyl alkyl ether amine, 10g three (dimethylamino methyl) phenol, the 40g phenylcarbinol drops in the 500mL container, heats up 40 ℃ to stir 30 minutes.Reducing to room temperature gets final product.
Embodiment 11:
With 120g Versamid (amine value=400), 52g epoxypropyl alkyl ether amine, 8.0g three (dimethylamino methyl) phenol, the 20g phenylcarbinol drops in the 500ml container, heats up 40 ℃, stirs 30 minutes mixed getting final product in the chamber of reducing to.
Claims (9)
1. the preparation method of a durably anticorrosion paint is characterized in that the epoxy alloy that adopts Hydrin Resins, epoxy and bisphenol A epoxide resin to form is main film forming matter, and the percentage composition of film forming matter is 60%-80%;
One, Hydrin Resins, epoxy solventless method is synthetic
1), ring-opening polymerization
Get 1.0 moles dibasic alcohol, specifically: wherein a kind of of ethylene glycol, propylene glycol, butyleneglycol, Diethylene Glycol, dipropylene glycol or hexylene glycol adds the catalyzer of (weight percentage %) 0.5～5% simultaneously; Catalyzer has: phosphorus hexafluoride triethyl oxonium salt, tin tetrachloride, boron trifluoride ethyl ether complex or boron trifluoride tetrahydrofuran complex; Drip the epoxy chloropropane n=10-25 of n mole then, controlled temperature is at 50-80 ℃ of logical N
2Gas, stirring are incubated 4-8 hour, survey oxirane value=0;
2), ring-closure reaction
With 2.1～2.5 moles NaOH, be made into the solution of 30-40% concentration, be added drop-wise in the above-mentioned reaction, 80-90 ℃ of insulation 4-6 hour;
3), washing
Extremely neutral with 98-100 ℃ of deionized water wash, and the content of mensuration inorganic chlorine stopped washing at 0.05% o'clock;
4), dehydration is purified
The normal pressure distillation is taken off moisture content, continues dehydration then and measure water-content≤0.5% o'clock end under the 10-15mmHg vacuum, measures oxirane value, hydroxyl value and viscosity, promptly obtains Hydrin Resins, epoxy;
Two, bisphenol A epoxide resin is selected the commercial goods, and range of choice: molecular weight is 380-1000, and oxirane value is 0.51-0.2;
Three, filler selection: wherein one or more of titanium dioxide, carbon black, ferric oxide, kaolin, talcum powder, lime carbonate, ferric sulfate, silica flour or metal powder and pigment;
Four, the epoxypropyl alkyl ether amine is synthetic
Get the polyamine of 1.05-1.2 mole, specifically: wherein a kind of of divinyl propylamine, diethylenetriamine or triethylene tetramine, intensification 40-60 ℃, drip 1.0 moles epoxypropyl alkyl oxide then, specifically: n-butyl glycidyl ether, glycidyl allyl ether, styrene oxide or phenyl glycidyl ether, 60-80 ℃ is incubated 4-8 hour;
Five, the preparation technology of coating
The preparation technology of A component
1), get bisphenol A epoxide resin, Hydrin Resins, epoxy and reactive thinner epoxypropyl alkyl oxide, three's weight percent is 40-50: 13-18: 3-10, heats 40-60 ℃ and stirring at low speed;
2), with dispersion agent, defoamer, oxidation inhibitor and stablizer, by the operation instruction input, stir;
3), solid packing and pigment are added in the container successively, fully wetting;
4), disperse with homogenizer, the beginning stirring at low speed, treat each mutually evenly after, carry out high speed dispersion;
5), be cooled to after the room temperature and grind two times with three-roll grinder, detect with Hegman grind gage and reach 20-50um and decide according to specific requirement, barrelling is finished product;
The preparation technology of B component
1), with the epoxypropyl alkyl ether amine, Versamid, three (dimethylamino methyl) phenol and phenylcarbinol drop in the container, four weight percent is 26-35: 40-60: 4-5: 10-20;
2), intensification 30-40 ℃, stir and make its thorough mixing even, reduce to room temperature, barrelling is finished product;
A component: B component (weight ratio)=5.0: 1.0-1.5.
2. the preparation method of durably anticorrosion paint as claimed in claim 1 is characterized in that the dibasic alcohol of ring-opening polymerization being ethylene glycol, propylene glycol or butyleneglycol.
3. the preparation method of durably anticorrosion paint as claimed in claim 1 is characterized in that catalyzer is boron trifluoride ethyl ether complex or boron trifluoride tetrahydrofuran complex.
4. the preparation method of durably anticorrosion paint as claimed in claim 1, the synthetic polyamine that it is characterized in that the epoxypropyl alkyl ether amine is divinyl propylamine or diethylenetriamine.
5. the preparation method of durably anticorrosion paint as claimed in claim 1 is characterized in that the epoxypropyl alkyl oxide is n-butyl glycidyl ether or glycidyl allyl ether.
6. the preparation method of durably anticorrosion paint as claimed in claim 1, the preparation dispersion agent that it is characterized in that the A component is EFKA5065.
7. the preparation method of durably anticorrosion paint as claimed in claim 1, the preparation defoamer that it is characterized in that the A component is EFKA2720 or EFKA2722.
8. the preparation method of durably anticorrosion paint as claimed in claim 1, the preparation oxidation inhibitor that it is characterized in that the A component is JH1010 or 900B.
9. the preparation method of durably anticorrosion paint as claimed in claim 1, the preparation stablizer that it is characterized in that the A component is Tinuvin292 or UV-326.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB001361872A CN1163560C (en) | 2000-12-27 | 2000-12-27 | Durably anticorrosion paint and its preparing process |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB001361872A CN1163560C (en) | 2000-12-27 | 2000-12-27 | Durably anticorrosion paint and its preparing process |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN1306052A CN1306052A (en) | 2001-08-01 |
| CN1163560C true CN1163560C (en) | 2004-08-25 |
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| Application Number | Title | Priority Date | Filing Date |
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| CNB001361872A Expired - Fee Related CN1163560C (en) | 2000-12-27 | 2000-12-27 | Durably anticorrosion paint and its preparing process |
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Families Citing this family (13)
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| CN101096465B (en) * | 2006-06-29 | 2010-06-09 | 彭文表 | Aqueous long-acting anticorrosion paint and preparation method thereof |
| CN100469812C (en) * | 2006-09-26 | 2009-03-18 | 蓝星化工新材料股份有限公司无锡树脂厂 | Preparing method for epoxy resin active diluent of low organic chlorine content |
| CN101724331B (en) * | 2008-10-29 | 2012-01-25 | 中国科学院金属研究所 | Anticorrosion epoxy powder paint used outside marine steel pipe pile |
| CN101503607B (en) * | 2009-01-14 | 2012-07-25 | 宋洪涛 | High strength glass fibre reinforced plastic adhesive and preparation |
| CN102442800A (en) * | 2010-10-09 | 2012-05-09 | 苏州工业园区鑫丰林塑料科技有限公司 | Solvent-free epoxy self-leveling floor coating process |
| CN102702927A (en) * | 2012-06-22 | 2012-10-03 | 山东乐化漆业股份有限公司 | Nano modified epoxy antiseptic paint |
| CN103682462B (en) * | 2013-12-31 | 2015-11-18 | 深圳市格瑞普电池有限公司 | Pour into integrated Li-ion batteries piles and preparation method |
| CN103788830A (en) * | 2014-01-20 | 2014-05-14 | 南通华新环保设备工程有限公司 | Acid and alkali resistant coating for stirring equipment and preparation method thereof |
| CN108129956A (en) * | 2018-01-18 | 2018-06-08 | 合肥威希特汽车配件加工有限公司 | A kind of preparation method of durably anticorrosion paint |
| CN109206574A (en) * | 2018-06-25 | 2019-01-15 | 青岛海尔股份有限公司 | Glycol composition and its polyurethane rigid foam plastic of preparation |
| CN109880526A (en) * | 2019-03-06 | 2019-06-14 | 乐清市华尊电气有限公司 | A kind of quick-drying raw lacquer liquid and preparation method thereof with bacteriostasis property |
| CN110079188A (en) * | 2019-04-11 | 2019-08-02 | 江南大学 | A kind of water-based anticorrosive paint and preparation method thereof of sustainable cathodic protection |
| CN113249012A (en) * | 2021-05-25 | 2021-08-13 | 成都扬华源动新材料科技有限公司 | Hydrophobic resin coating, preparation method thereof and drainage pipeline |
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2000
- 2000-12-27 CN CNB001361872A patent/CN1163560C/en not_active Expired - Fee Related
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