CN107099221A - A kind of steel surface underloading aqueous rusty self-lubricating coating and preparation method thereof - Google Patents

A kind of steel surface underloading aqueous rusty self-lubricating coating and preparation method thereof Download PDF

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CN107099221A
CN107099221A CN201710351828.5A CN201710351828A CN107099221A CN 107099221 A CN107099221 A CN 107099221A CN 201710351828 A CN201710351828 A CN 201710351828A CN 107099221 A CN107099221 A CN 107099221A
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aqueous
self
water
dispersion
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田雪梅
田闽
乔红斌
李龙娥
吴胜华
古绪鹏
陈国昌
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Anhui University of Technology AHUT
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    • CCHEMISTRY; METALLURGY
    • C09DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09DCOATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
    • C09D163/00Coating compositions based on epoxy resins; Coating compositions based on derivatives of epoxy resins
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08FMACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
    • C08F114/00Homopolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by a halogen
    • C08F114/18Monomers containing fluorine
    • C08F114/26Tetrafluoroethene
    • CCHEMISTRY; METALLURGY
    • C09DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09DCOATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
    • C09D5/00Coating compositions, e.g. paints, varnishes or lacquers, characterised by their physical nature or the effects produced; Filling pastes
    • C09D5/08Anti-corrosive paints
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    • C09DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09DCOATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
    • C09D7/00Features of coating compositions, not provided for in group C09D5/00; Processes for incorporating ingredients in coating compositions
    • C09D7/40Additives
    • C09D7/60Additives non-macromolecular
    • C09D7/61Additives non-macromolecular inorganic
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    • C09DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
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    • C09D7/00Features of coating compositions, not provided for in group C09D5/00; Processes for incorporating ingredients in coating compositions
    • C09D7/40Additives
    • C09D7/60Additives non-macromolecular
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    • C09DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09DCOATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
    • C09D7/00Features of coating compositions, not provided for in group C09D5/00; Processes for incorporating ingredients in coating compositions
    • C09D7/40Additives
    • C09D7/65Additives macromolecular
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08KUse of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K3/00Use of inorganic substances as compounding ingredients
    • C08K3/32Phosphorus-containing compounds
    • C08K2003/321Phosphates
    • C08K2003/328Phosphates of heavy metals

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Abstract

The invention discloses a kind of steel surface underloading aqueous rusty self-lubricating coating and preparation method thereof, belong to technical field of coatings.The aqueous rusty self-lubricating coating is made up of components such as aqueous self-lubricating dispersion, the single-component water-based epoxy of ambient self-crosslinking, composite band rust transforming agent, aluminium triphosphate, trbasic zinc phosphate, sericite, defoamer, wetting agent, levelling agent, deionized water and pH adjusting agents;Wherein:The aqueous self-lubricating dispersion is obtained by Tissuemat E water-borne dispersions and polytetrafluoroethylene (PTFE) wax dispenser compounding.The present invention prepares a kind of aqueous corrosion resisting paint without need of cleaning rust for the steel surface being corroded, while adding the excellent water-borne dispersions of certain proportion greasy property, assigns its specific greasy property.The present invention is coated on steel surface, one layer of fine and close coating can be formed with rust conversion, the coating has good self-lubricating effect after testing.

Description

A kind of steel surface underloading aqueous rusty self-lubricating coating and preparation method thereof
Technical field
The invention belongs to technical field of coatings, and in particular to a kind of steel surface underloading with aqueous rusty self-lubricating coating and Its preparation method.
Background technology
Steel corrosion, brings huge economic loss, in order to prevent steel corrosion, people have invented much to society every year Method is used for the anti-corrosion of steel construction, in numerous anti-corrosion methods, coating process simple possible the most economic, patent CN102838914A and CN104046149A provide it is a kind of can with the aqueous rust transformation primer of application over rust, using tannic acid with The stable complex compound of iron ion generation, strengthens the adhesive force of coating, so as to suppress the growth of rusty scale.Such coating has anti-well Rotten effect, but the coating surface formed is coarse, coefficient of friction is big, therefore such coating be not particularly suited for guide rail, transmission device or The anti-corrosion on tumbler surface.
Occasion for much requiring low-friction coefficient, such as guide rail, transmission device, tumbler.The most frequently used is anti- Rotten and antifriction method is to coat lubricating oil or lubricating grease on its surface.But lubricating oil, lubricating grease can cause environmental pollution, and should With being limited in scope.It can hardly be used under high/low temperature, below-G conditions.Although the preparation of related lubricant has very big in recent years Development, can effectively reduce coefficient of friction and comparatively safe environmental protection, it is sub- that such as patent CN103602362A introduces a kind of curing The preparation method of iron-graphene composite Nano lubricant, patent CN101914409A introduces a kind of preparation of fire-resistant lubricants Method.But can useful effect in the lubricant in equipment and few of easily getting rusty or got rusty.
Self-lubricating coating has the vapour bushing in application, such as self-lubricating bearing, piston-mode motor in many fields, very Lubricating oil, lubricating grease are solved in big degree can not solve or non-serviceable occasion at all.In the prior art, self-lubricating coating Generally it is made up of, coating is coated on metal substrate anti-wear additive, bonding agent, kollag and color stuffing when it is used Special lubricant coating is formed after sintering curing.Patent CN102277082A provides a kind of self-lubricating sintering coating and painting Coating method.Although it has good wearability, its application field is narrow, and construction method is complicated.
Easily it is corroded and gets rusty in some transmission portions or rotary part, cause frictional force to increase, for example lockhole, bearing etc., Traditional lubricant grease can not solve this problem at all, and can also cause environmental pollution.
The content of the invention
For above-mentioned the deficiencies in the prior art, the present invention devises a kind of steel surface underloading aqueous rusty self-lubricating and applied Material, it is therefore an objective to while solve the hydrophobic antirust and antifriction noise reduction of steel surface, in the working interface got rusty without many Remaining pre-treatment, fine and close coating is formed with rust conversion, and coating has good self-lubricating and antiseptic property.
To achieve these goals, present invention employs following technical scheme.
A kind of steel surface underloading aqueous rusty self-lubricating coating, the coating is made up of following parts by weight of component:
Described aqueous self-lubricating dispersion is 36~43 parts of Tissuemat E aqueous liquid dispersions and 57~64 parts of polytetrafluoroethyl-nes The compound of alkene aqueous liquid dispersion.
The composite band rust transforming agent is that 4.5~5.5 parts of tannic acid and 1.5~0.5 parts of pyrogallic acid are dissolved in 10 In~15 parts of water, then it is added dropwise thereto obtained in 0.5~1 part of ethanol solution.
The defoamer is tributyl phosphate or polyether-modified silicon.
The wetting agent is Tego Wet KL 245 or BYK-346.
The levelling agent is isophorone and DAA in mass ratio 1:1 mixed liquor.
The pH adjusting agent formic acid and one kind or mixed liquor in salicylic acid.
Tissuemat E aqueous liquid dispersion in the aqueous self-lubricating dispersion is through the following steps that prepared:
A. 61~69 parts of water are weighed in the four-hole boiling flask with agitating device;
B. 0.01~0.05 part of N is weighed, N- diethylanilines and 0.1~0.2 part of benzoyl peroxide dissolve in 4~6 part two In toluene;
C. the product in step b is put into the four-hole boiling flask in step a, then is separately added into 3~4 parts of propylene thereto Acid and 18~24 parts of Tissuemat E powder, are warming up to 50~55 DEG C, lead to N280~100min is swelled, then is warming up to predetermined reaction After 85~87 DEG C of temperature, 1.5~2h of reaction, then 1.8~2.4 parts of lauryl sodium sulfate and 0.3~0.6 part are added thereto tell Temperature 80, is warming up to 98~102 DEG C, emulsifies 35~40min, naturally cools to 45 DEG C of dischargings, that is, Tissuemat E aqueous dispersion is made Liquid.
Aqueous dispersion of polytetrafluoroethyland in the aqueous self-lubricating dispersion is through the following steps that prepared:
Added into polymeric kettle 72~77 parts high purity water, 0.5~0.75 part of dispersant perfluorooctanoic acid and 0.015~ 0.03 part of initiator benzoyl peroxide, closes polymeric kettle, opens stirring, and rotating speed is adjusted to 80~100rpm, is 1.5 in pressure ~1.6MPa, temperature control be 17~21 DEG C at carry out vacuum experiment and pressurize experiment, it is qualified after be passed through high pure nitrogen thereto, 21~25 parts of tetrafluoroethene is added in the way of continuously adding in the course of the polymerization process, maintains after the constant 6~7h of polymerization pressure, stops Only feed and stir, use N2Unreacted monomer is excluded, that is, obtains aqueous dispersion of polytetrafluoroethyland.
Invention also provides the preparation method of above-mentioned steel surface underloading aqueous rusty self-lubricating coating, specific bag Include following steps:
(1) preparation of aqueous epoxy curing agent:
A, the aromatic multi-amine for weighing 37~42 parts and 33~38 parts of butanediol ether, are added into three-necked flask, water Bath is heated to 58~62 DEG C, is stirred with 150~200rpm speed after 1~1.5h, then 0.5~0.7 part of grass is added dropwise thereto Acid, obtains solution A standby;
B, weigh 73~78 parts of novolac epoxy resins and 4~7 parts of butanediol ether are put into another three-necked flasks, water-bath adds Heat is stirred to 85 DEG C with 150~200rpm rotating speed, after novolac epoxy resin is completely dissolved, and adds 14.6~19.5 part three Monoethanolamine, reacts 2~3h, plus 0.6~0.9 part of oxalic acid, obtains solution B standby;
C, obtained solution A is weighed in 2~3 parts of lauryl glycidol ethers, 50~55 parts of step a in 250ml's In three-necked flask, then solution B obtained in 22~27 parts of step b is added thereto, with 200~400rpm rotating speed stirring simultaneously Heating water bath obtains aromatic multi-amine novolac epoxy resin to 85 DEG C of 3~4h of reaction;
D, obtained aromatic multi-amine novolac epoxy resin is weighed in 81~87 parts of step c in 1500~1800rpm of rotating speed Lower stirring, plus 13~17 parts of water carry out that aqueous epoxy curing agent is made after 3~5h of phase reversal.
(2) preparation of ambient self-crosslinking water-base epoxy:0.5~0.8 part of formic acid is weighed in three mouthfuls with agitating device In flask, rotating speed is adjusted to 50~75rpm, and aqueous ring made from 16~21 parts of above-mentioned steps (1) is added in the state of being stirred on side Oxygen curing agent, adds 75~83 parts of aqueous epoxy resins thereto after 10 minutes, continue to stir 30min, obtained normal temperature selfing Join water-base epoxy standby.
(3) preparation of aqueous self-lubricating dispersion:Weigh 36~43 parts of Tissuemat E aqueous liquid dispersions and 57~64 parts poly- Tetrafluoroethene aqueous liquid dispersion, stirs 1.5h in magnetic stirring apparatus, obtains aqueous self-lubricating dispersion standby.
(4) preparation of composite band rust transforming agent:4.5~5.5 parts of tannic acid are weighed to be dissolved in 2~4 parts of ethanol solution, then The pyrogallic acid of 1.5~0.5 parts of addition, magnetic agitation 0.5h, obtain composite band rust transforming agent standby thereto.
(5) 25~35 parts of deionized waters are weighed, magnetic agitation is separately added into 4~6 parts of aluminium triphosphates, 3~5 thereto Part trbasic zinc phosphate, the composite band rust transforming agent obtained by 3~4 parts of sericites and 11~15 parts of above-mentioned steps (4), then be placed on In the planetary ball mill of XQM~6, revolution speed is adjusted to 140rpm, and rotational velocity is adjusted to 460rpm, and grinding 6h obtains raw material for standby.
(6) 46~65 parts of raw material obtained in above-mentioned steps (5) is weighed in the three-necked flask with agitating device, is turned Velocity modulation is slow respectively to add 1~1.5 part of defoamer, 0.1~0.2 part of wetting agent, 0.1~0.3 part of levelling thereto to 50rpm Aqueous self-lubricating dispersion obtained by agent and 20~25 parts of above-mentioned steps (3), rotating speed is adjusted to after 150rpm, stirring 30min Add ambient self-crosslinking water-base epoxy made from 20~29 parts of steps (2) thereto again;Continue to stir after 1.5h, then add thereto Enter 1~4 part of pH adjusting agent, the pH of coating is adjusted to 3~5, target product is produced.
The principles of science of the present invention:
The present invention be by raw material of Tissuemat E powder, N, N- diethylanilines be emulsifying agent, using heating N2Isolation is empty The method of gas prepares aqueous polyethylene wax aqueous liquid dispersion;Using tetrafluoroethene as raw material, perfluorooctanoic acid dispersant, benzoyl peroxide Formyl is initiator, is 1.5~1.6MPa in pressure, temperature leads to N to take dispersin polymerization under conditions of 17~21 DEG C2Prepare Aqueous dispersion of polytetrafluoroethyland.By compounding Tissuemat E aqueous liquid dispersion and aqueous dispersion of polytetrafluoroethyland system in proportion Standby aqueous self-lubricating dispersion assigns coating excellent self-lubricating property, make band rust convert formed coating have it is relatively low Coefficient of friction.The mass ratio of novolac epoxy resin and triethanolamine is controlled in addition, so as to control the open loop rate of novolac epoxy resin It is modified 30% or so, then by aromatic multi-amine, normal temperature aqueous epoxy curing agent is made, so as to prepare a kind of ambient self-crosslinking Water-base epoxy.The present invention plays band rust transforming agent and aqueous by adjusting dispersion liquid, the characteristic with rust transforming agent and epoxy resin The cooperative effect of self-lubricating dispersion, to assign the excellent band rust conversion performance of coating and self-lubricating property.
Compared with prior art, the present invention has following technique effect:
(1) the invention provides a kind of underloading aqueous rusty self-lubricating coating, not oil-containing, without fat, be practically free of Machine solvent, environmental sound.
(2) present invention is by adding water-borne dispersions compound in hydrotropism's on rust paint so that the coating with rust conversion With excellent self-lubricating property.
(3) application prospect of the present invention extensively, can be widely applied to the steel surface that gets rusty, and easy construction, without polishing (or Polished slightly according to steel situation of getting rusty) directly coating.Converting obtained coating has the double grading of anti-corrosion and lubrication.
Embodiment
The present invention is described in detail below in conjunction with specific embodiment, but the present invention is not limited to following embodiments.
First, the preparation of underloading of the present invention aqueous rusty self-lubricating coating
Embodiment 1
(1) preparation of aqueous epoxy curing agent:
1. 37g aromatic multi-amine and 33g butanediol ether are weighed, is added into 250ml three-necked flask, water-bath adds Heat after 150rpm speed stirring 1h, then is added dropwise 0.5g oxalic acid, obtains 68.3g solution As standby thereto to 58 DEG C.
2. 73g novolac epoxy resins are weighed and 4g butanediols ether is put into another 250ml there-necked flask, heating water bath is arrived 85 DEG C, stirred with 150rpm rotating speed, after novolac epoxy resin is completely dissolved, add 14.6g triethanolamines, react 2h, plus 0.6g oxalic acid, obtains 79.6g solution Bs standby.
3. the step of weighing 2g lauryls glycidol ether, 50g 2. in obtained solution B in new tri- mouthfuls of burnings of 250ml In bottle, then obtained solution A in adding 22g steps thereto 1., the rotating speed stirring and heating water bath with 200rpm are to 85 DEG C 3h is reacted, 71.1g aromatic multi-amine novolac epoxy resins are obtained.
4. obtained aromatic multi-amine novolac epoxy resin is stirred under rotating speed 1500rpm in weighing 40.5g steps 3., plus 6.5g water is carried out after phase reversal 3h, and 45.5g aqueous epoxy curing agents are made.
(2) preparation of ambient self-crosslinking water-base epoxy:1.0g formic acid is weighed in three mouthfuls of burnings of the 250ml with agitating device In bottle, rotating speed is adjusted to 60rpm, adds 32.0g aqueous epoxy curing agents in the state of being stirred on side, is added thereto after 10 minutes 150g aqueous epoxy resins, continue to stir 30min, obtained ambient self-crosslinking water-base epoxy 179.3g is standby.
(3) preparation of aqueous self-lubricating dispersion:
1. the preparation of Tissuemat E aqueous liquid dispersion:
A. 61g water is weighed in the four-hole boiling flask with agitating device 250ml;
B. 0.01gN is weighed, N- diethylanilines and 0.1g benzoyl peroxides are dissolved in 4g dimethylbenzene;
C. the product in step b is put into the four-hole boiling flask in step a, then be separately added into thereto 3g acrylic acid and 18g Tissuemat E powder, is warming up to 50 DEG C, leads to N280min is swelled, then is warming up to predetermined 85 DEG C of reaction temperature, 1.5h is reacted Afterwards, then thereto 1.8g lauryl sodium sulfate and 0.3g Tween 80s are added, 98 DEG C are warming up to, 35min is emulsified, naturally cools to 45 DEG C of dischargings, obtain 81.9g Tissuemat E aqueous liquid dispersions.
2. the preparation of aqueous dispersion of polytetrafluoroethyland:72g high purity water, 0.5g perfluorooctanoic acids is added into polymeric kettle With 0.015g benzoyl peroxides, polymeric kettle is closed, stirring is opened, rotating speed is adjusted to 80rpm, is 1.5MPa in pressure, temperature is Carry out vacuum experiment and pressurize experiment at 17 DEG C, it is qualified after be passed through high pure nitrogen thereto, in the course of the polymerization process continuously to add Mode add 21g tetrafluoroethene, maintain after the constant 6h of polymerization pressure, stop charging and stir, use N2Exclude unreacted list Body, obtains 89.5g to aqueous dispersion of polytetrafluoroethyland.
3. 36g Tissuemat Es aqueous liquid dispersion and 57g aqueous dispersion of polytetrafluoroethyland are weighed, is stirred in magnetic stirring apparatus 1.5h is mixed, the aqueous self-lubricating dispersions of 90.1g are obtained standby.
(4) preparation of composite band rust transforming agent:Weigh 4.5g tannic acid to be dissolved in 10g water, then add thereto 0.5g pyrogallic acids, finally instill 0.5g ethanol solution thereto, and magnetic agitation 0.5h obtains 14.3g composite bands rust and turned Agent is standby.
(5) 25g deionized waters are weighed in the three-necked flask with agitating device, magnetic agitation is separately added into thereto 4g aluminium triphosphates, 3g trbasic zinc phosphates and 3g sericites and 11g composite bands rust transforming agent, then it is placed on XQM-6 planetary ball mills In, revolution speed is adjusted to 140rpm, and rotational velocity is adjusted to 460rpm, and grinding 6h obtains raw material for standby.
(6) raw material 46g obtained in above-mentioned steps (5) is weighed in the three-necked flask with agitating device, and rotating speed is adjusted It is slow respectively to add 1g defoamers tributyl phosphate, 0.1g wetting agent TegoWet KL 245,0.1g streams thereto to 50rpm Obtained aqueous self-lubricating dispersion in flat agent and 20g above-mentioned steps (3), rotating speed is adjusted to after 150rpm, stirring 30min again Ambient self-crosslinking water-base epoxy made from 20g above-mentioned steps (2) is added thereto.Stir after 1.5h, then add 1g first thereto After acid, stirring 20min, that is, a kind of underloading aqueous rusty self-lubricating coat in use is made.
Embodiment 2
(1) preparation of aqueous epoxy curing agent:
1. 37g aromatic multi-amine and 33g butanediol ether are weighed, is added into 250ml three-necked flask, water-bath adds Heat after 150rpm speed stirring 1h, then is added dropwise 0.5g oxalic acid, obtains 68.2g solution As standby thereto to 58 DEG C.
2. 73g novolac epoxy resins are weighed and 4g butanediols ether is put into another 250ml there-necked flask, heating water bath is arrived 85 DEG C, stirred with 150rpm rotating speed, after novolac epoxy resin is completely dissolved, add 14.6g triethanolamines, react 2h, plus 0.6g oxalic acid, obtains 79.1g solution Bs standby.
3. the step of weighing 2g lauryls glycidol ether, 50g 2. in obtained solution B in new tri- mouthfuls of burnings of 250ml In bottle, then obtained solution A in adding 22g steps thereto 1., the rotating speed stirring and heating water bath with 200rpm are to 85 DEG C 3h is reacted, 70.3g aromatic multi-amine novolac epoxy resins are obtained.
4. obtained aromatic multi-amine novolac epoxy resin is stirred under rotating speed 1500rpm in weighing 40.5g steps 3., plus 6.5g water is carried out after phase reversal 3h, and 45.7g aqueous epoxy curing agents are made.
(2) preparation of ambient self-crosslinking water-base epoxy:1.0g formic acid is weighed in three mouthfuls of burnings of the 250ml with agitating device In bottle, rotating speed is adjusted to 60rpm, adds 32.0g aqueous epoxy curing agents in the state of being stirred on side, is added thereto after 10 minutes 150g aqueous epoxy resins, continue to stir 30min, obtained ambient self-crosslinking water-base epoxy 179.6g is standby.
(3) preparation of aqueous self-lubricating dispersion:
1. the preparation of Tissuemat E aqueous liquid dispersion:
A. 61g water is weighed in the four-hole boiling flask with agitating device 250ml;
B. 0.01gN is weighed, N- diethylanilines and 0.1g benzoyl peroxides are dissolved in 4g dimethylbenzene;
C. the product in step b is put into the four-hole boiling flask in step a, then be separately added into thereto 3g acrylic acid and 18g Tissuemat E powder, is warming up to 50 DEG C, leads to N280min is swelled, then is warming up to predetermined 85 DEG C of reaction temperature, 1.5h is reacted Afterwards, then thereto 1.8g lauryl sodium sulfate and 0.3g Tween 80s are added, 98 DEG C are warming up to, 35min is emulsified, naturally cools to 45 DEG C of dischargings, obtain 82.3g Tissuemat E aqueous liquid dispersions.
2. the preparation of aqueous dispersion of polytetrafluoroethyland:72g high purity water, 0.5g perfluorooctanoic acids is added into polymeric kettle With 0.015g benzoyl peroxides, polymeric kettle is closed, stirring is opened, rotating speed is adjusted to 80rpm, is 1.5MPa in pressure, temperature is Carry out vacuum experiment and pressurize experiment at 17 DEG C, it is qualified after be passed through high pure nitrogen thereto, in the course of the polymerization process continuously to add Mode add 21g tetrafluoroethene, maintain after the constant 6h of polymerization pressure, stop charging and stir, use N2Exclude unreacted list Body, obtains 89.4g to aqueous dispersion of polytetrafluoroethyland.
3. 36g Tissuemat Es aqueous liquid dispersion and 57g aqueous dispersion of polytetrafluoroethyland are weighed, is stirred in magnetic stirring apparatus 1.5h is mixed, the aqueous self-lubricating dispersions of 90.3g are obtained standby.
(4) preparation of composite band rust transforming agent:Weigh 4.5g tannic acid to be dissolved in 10g water, then add thereto 0.5g pyrogallic acids, finally instill 0.5g ethanol solution thereto, and magnetic agitation 0.5h obtains 14.6g composite bands rust and turned Agent is standby.
(5) 30g deionized waters are weighed in the three-necked flask with agitating device, magnetic agitation is separately added into thereto Obtained composite band rust transforming agent in 5g aluminium triphosphates, 4g trbasic zinc phosphates and 3.5g sericites and 13g above-mentioned steps (4), then It is placed in XQM-6 planetary ball mills, revolution speed is adjusted to 140rpm, rotational velocity is adjusted to 460rpm, and grinding 6h obtains raw material It is standby.
(6) raw material 55.5g obtained in above-mentioned steps (5) is weighed in the three-necked flask with agitating device, rotating speed Be adjusted to 60rpm, respectively it is slow add thereto 1.25g defoamers tributyl phosphate, 0.15g wetting agent Tego Wet KL 245, Aqueous self-lubricating dispersion obtained by 0.2g levelling agents and 23g above-mentioned steps (3), 150rpm is adjusted to by rotating speed, stirring Add ambient self-crosslinking water-base epoxy obtained in 25g above-mentioned steps (2) after 30min thereto again.Continue to stir after 1.5h, Add thereto again after 2.5g pH adjusting agent formic acid, stirring 20min, that is, a kind of underloading aqueous rusty self-lubricating coat in use is made.
Embodiment 3
(1) preparation of aqueous epoxy curing agent:
1. 37g aromatic multi-amine and 33g butanediol ether are weighed, is added into 250ml three-necked flask, water-bath adds Heat after 150rpm speed stirring 1h, then is added dropwise 0.5g oxalic acid, obtains 68.6g solution As standby thereto to 58 DEG C.
2. 73g novolac epoxy resins are weighed and 4g butanediols ether is put into another 250ml there-necked flask, heating water bath is arrived 85 DEG C, stirred with 150rpm rotating speed, after novolac epoxy resin is completely dissolved, add 14.6g triethanolamines, react 2h, plus 0.6g oxalic acid, obtains 89.5g solution Bs standby.
3. the step of weighing 2g lauryls glycidol ether, 50g 2. in obtained solution B in new tri- mouthfuls of burnings of 250ml In bottle, then obtained solution A in adding 22g steps thereto 1., the rotating speed stirring and heating water bath with 200rpm are to 85 DEG C 3h is reacted, 70.6g aromatic multi-amine novolac epoxy resins are obtained.
4. obtained aromatic multi-amine novolac epoxy resin is stirred under rotating speed 1500rpm in weighing 40.5g steps 3., plus 6.5g water is carried out after phase reversal 3h, and 45.8g aqueous epoxy curing agents are made.
(2) preparation of ambient self-crosslinking water-base epoxy:1.0g formic acid is weighed in three mouthfuls of burnings of the 250ml with agitating device In bottle, rotating speed is adjusted to 60rpm, adds 32.0g aqueous epoxy curing agents in the state of being stirred on side, is added thereto after 10 minutes 150g aqueous epoxy resins, continue to stir 30min, obtained ambient self-crosslinking water-base epoxy 180.1g is standby.
(3) preparation of aqueous self-lubricating dispersion:
1. the preparation of Tissuemat E aqueous liquid dispersion:
A. 61g water is weighed in the four-hole boiling flask with agitating device 250ml;
B. 0.01gN is weighed, N- diethylanilines and 0.1g benzoyl peroxides are dissolved in 4g dimethylbenzene;
C. the product in step b is put into the four-hole boiling flask in step a, then be separately added into thereto 3g acrylic acid and 18g Tissuemat E powder, is warming up to 50 DEG C, leads to N280min is swelled, then is warming up to predetermined 85 DEG C of reaction temperature, 1.5h is reacted Afterwards, then thereto 1.8g lauryl sodium sulfate and 0.3g Tween 80s are added, 98 DEG C are warming up to, 35min is emulsified, naturally cools to 45 DEG C of dischargings, obtain 82.9g Tissuemat E aqueous liquid dispersions.
2. the preparation of aqueous dispersion of polytetrafluoroethyland:72g high purity water, 0.5g perfluorooctanoic acids is added into polymeric kettle With 0.015g benzoyl peroxides, polymeric kettle is closed, stirring is opened, rotating speed is adjusted to 80rpm, is 1.5MPa in pressure, temperature is Carry out vacuum experiment and pressurize experiment at 17 DEG C, it is qualified after be passed through high pure nitrogen thereto, in the course of the polymerization process continuously to add Mode add 21g tetrafluoroethene, maintain after the constant 6h of polymerization pressure, stop charging and stir, use N2Exclude unreacted list Body, obtains 91.1g to aqueous dispersion of polytetrafluoroethyland.
3. 36g Tissuemat Es aqueous liquid dispersion and 57g aqueous dispersion of polytetrafluoroethyland are weighed, is stirred in magnetic stirring apparatus 1.5h is mixed, the aqueous self-lubricating dispersions of 90.3g are obtained standby.
(4) preparation of composite band rust transforming agent:Weigh 4.5g tannic acid to be dissolved in 10g water, then add thereto 0.5g pyrogallic acids, finally instill 0.5g ethanol solution thereto, and magnetic agitation 0.5h obtains 14.7g composite bands rust and turned Agent is standby.
(5) 35g deionized waters are weighed, magnetic agitation is separately added into 6g aluminium triphosphates, 5g trbasic zinc phosphates and 4g thin,tough silk thereto Obtained composite band rust transforming agent in mica and 15g above-mentioned steps (4), then be placed in XQM-6 planetary ball mills, revolve round the sun Speed is adjusted to 140rpm, and rotational velocity is adjusted to 460rpm, and grinding 6h obtains raw material for standby.
(6) raw material 65g obtained in above-mentioned steps (5) is weighed in the three-necked flask with agitating device, and rotating speed is adjusted It is slow respectively to add 1.5g defoamers tributyl phosphate, 0.2g wetting agent Tego Wet KL 245,0.3g thereto to 60rpm Obtained aqueous self-lubricating dispersion in levelling agent and 25g above-mentioned steps (3), rotating speed is adjusted to after 150rpm, stirring 30min Add ambient self-crosslinking water-base epoxy obtained in 29g above-mentioned (2) thereto again.Continue to stir after 1.5h, then add thereto Enter after 4g pH adjusting agent formic acid, stirring 20min, that is, a kind of underloading aqueous rusty self-lubricating coat in use is made.
Embodiment 4
(1) preparation of aqueous epoxy curing agent:
1. weigh in 42g aromatic multi-amine and 38g butanediol ether, the three-necked flask for being added into a 250ml, water-bath 62 DEG C are heated to, after 200rpm speed stirring 1.5h, then 0.7g oxalic acid is added dropwise thereto, obtains 78.7 solution As standby.
2. 78g novolac epoxy resins are weighed and 7g butanediols ether is put into another 250ml there-necked flask, heating water bath is arrived 85 DEG C, stirred with 200rpm rotating speed, after novolac epoxy resin is completely dissolved, add 19.5g triethanolamines, react 3h, plus 0.9g oxalic acid, obtains 101.6 solution Bs standby.
3. the step of weighing 3g lauryls glycidol ether, 55g 2. in obtained solution B in three mouthfuls of new 250ml In flask, then obtained solution A in adding 27g steps thereto 1., with 400rpm rotating speed stirring and heating water bath to 85 DEG C reaction 3~4h, obtain 81.3g aromatic multi-amine novolac epoxy resins.
4. obtained aromatic multi-amine novolac epoxy resin is under 1500~1800rpm of rotating speed in weighing 43.5g steps 3. Stirring, plus 8.5g water are carried out after phase reversal 5h, and 49.2g aqueous epoxy curing agents are made.
(2) preparation of ambient self-crosslinking water-base epoxy:0.8g formic acid is weighed in the three-necked flask with agitating device, Rotating speed is adjusted to 75rpm, aqueous epoxy curing agent made from 21g above-mentioned steps (1) is added in the state of being stirred on side, after 10 minutes 83g aqueous epoxy resins are added thereto, continue to stir 30min, the ambient self-crosslinking water-base epoxy that 100.9g is made is standby.
(3) preparation of aqueous self-lubricating dispersion:
1. the preparation of Tissuemat E aqueous liquid dispersion:
A. 69g water is weighed in the four-hole boiling flask with agitating device;
B. 0.05gN is weighed, N- diethylanilines and 0.2g benzoyl peroxides are dissolved in 6g dimethylbenzene;
C. the product in step b is put into the four-hole boiling flask in step a, then be separately added into thereto 4g acrylic acid and 24g Tissuemat E powder, is warming up to 55 DEG C, leads to N2100min is swelled, then is warming up to predetermined 87 DEG C of reaction temperature, 2h is reacted Afterwards, 2.4g lauryl sodium sulfate and 0.6g Tween 80s are added thereto, 102 DEG C are warming up to, and are emulsified 40min, are naturally cooled to 45 DEG C of dischargings, are made 92.7g Tissuemat E aqueous liquid dispersions.
2. the preparation of aqueous dispersion of polytetrafluoroethyland:Added into polymeric kettle 77g high purity water, 0.75g perfluor it is pungent The benzoyl peroxide of sour ammonium and 0.03g, closes polymeric kettle, opens stirring, and rotating speed is adjusted to 100rpm, is 1.6MPa in pressure, At 21 DEG C of temperature control carry out vacuum experiment and pressurize experiment, it is qualified after be passed through high pure nitrogen thereto, in the course of the polymerization process with The mode continuously added adds 25g tetrafluoroethene, maintains after the constant 7h of polymerization pressure, stops charging and stirs, uses N2Exclude Unreacted monomer, obtains 100.75g aqueous dispersion of polytetrafluoroethyland.
3. 43g Tissuemat Es aqueous liquid dispersion and 64g aqueous dispersion of polytetrafluoroethyland are weighed, is stirred in magnetic stirring apparatus 1.5h is mixed, the aqueous self-lubricating dispersions of 106.8g are obtained standby.
(4) preparation of composite band rust transforming agent:Weigh 5.5g tannic acid to be dissolved in 15g water, then add thereto 1.5g pyrogallic acid, finally instills 1g ethanol solution thereto, and magnetic agitation 0.5h obtains 21.7g composite bands rust and turned Agent is standby.
(5) 25g deionized waters are weighed in the three-necked flask with agitating device, magnetic agitation is separately added into thereto 4g aluminium triphosphates, 3g trbasic zinc phosphates and 3g sericites and 11g composite bands rust transforming agent, then it is placed on XQM-6 planetary ball mills In, revolution speed is adjusted to 140rpm, and rotational velocity is adjusted to 460rpm, and grinding 6h obtains 46g raw material for standby.
(6) raw material 46g obtained in above-mentioned steps (5) is weighed in the three-necked flask with agitating device, and rotating speed is adjusted To 50rpm, respectively it is slow add thereto the polyether-modified silicon of 1g defoamers, 0.1g wetting agent BYK-346,0.1g levelling agents and Aqueous self-lubricating dispersion obtained by 20g above-mentioned steps (3), adds thereto again after rotating speed is adjusted into 70rpm, stirring 30min Enter the ambient self-crosslinking water-base epoxy obtained by 20g above-mentioned steps (2).Stir after 1.5h, then add 1g salicylic acids thereto, stir Mix after 20min, that is, a kind of underloading aqueous rusty self-lubricating coat in use is made.
Embodiment 5
(1) preparation of aqueous epoxy curing agent:
1. weigh in 42g aromatic multi-amine and 38g butanediol ether, the three-necked flask for being added into a 250ml, water-bath 62 DEG C are heated to, after 200rpm speed stirring 1.5h, then 0.7g oxalic acid is added dropwise thereto, obtains 78.9 solution As standby.
2. 78g novolac epoxy resins are weighed and 7g butanediols ether is put into another 250ml there-necked flask, heating water bath is arrived 85 DEG C, stirred with 200rpm rotating speed, after novolac epoxy resin is completely dissolved, add 19.5g triethanolamines, react 3h, plus 0.9g oxalic acid, obtains 101.4 solution Bs standby.
3. the step of weighing 3g lauryls glycidol ether, 55g 2. in obtained solution B in three mouthfuls of new 250ml In flask, then obtained solution A in adding 27g steps thereto 1., with 400rpm rotating speed stirring and heating water bath to 85 DEG C reaction 3~4h, obtain 81.7g aromatic multi-amine novolac epoxy resins.
4. obtained aromatic multi-amine novolac epoxy resin is under 1500~1800rpm of rotating speed in weighing 43.5g steps 3. Stirring, plus 8.5g water are carried out after phase reversal 5h, and 49.4g aqueous epoxy curing agents are made.
(2) preparation of ambient self-crosslinking water-base epoxy:0.8g formic acid is weighed in the three-necked flask with agitating device, Rotating speed is adjusted to 75rpm, aqueous epoxy curing agent made from 21g above-mentioned steps (1) is added in the state of being stirred on side, after 10 minutes 83g aqueous epoxy resins are added thereto, continue to stir 30min, the ambient self-crosslinking water-base epoxy that 101.1g is made is standby.
(3) preparation of aqueous self-lubricating dispersion:
1. the preparation of Tissuemat E aqueous liquid dispersion:
A. 69g water is weighed in the four-hole boiling flask with agitating device;
B. 0.05gN is weighed, N- diethylanilines and 0.2g benzoyl peroxides are dissolved in 6g dimethylbenzene;
C. the product in step b is put into the four-hole boiling flask in step a, then be separately added into thereto 4g acrylic acid and 24g Tissuemat E powder, is warming up to 55 DEG C, leads to N2100min is swelled, then is warming up to predetermined 87 DEG C of reaction temperature, 2h is reacted Afterwards, 2.4g lauryl sodium sulfate and 0.6g Tween 80s are added thereto, 102 DEG C are warming up to, and are emulsified 40min, are naturally cooled to 45 DEG C of dischargings, are made 93.5g Tissuemat E aqueous liquid dispersions.
2. the preparation of aqueous dispersion of polytetrafluoroethyland:Added into polymeric kettle 77g high purity water, 0.75g perfluor it is pungent The benzoyl peroxide of sour ammonium and 0.03g, closes polymeric kettle, opens stirring, and rotating speed is adjusted to 100rpm, is 1.6MPa in pressure, At 21 DEG C of temperature control carry out vacuum experiment and pressurize experiment, it is qualified after be passed through high pure nitrogen thereto, in the course of the polymerization process with The mode continuously added adds 25g tetrafluoroethene, maintains after the constant 7h of polymerization pressure, stops charging and stirs, uses N2Exclude Unreacted monomer, obtains 101.25g aqueous dispersion of polytetrafluoroethyland.
3. 43g Tissuemat Es aqueous liquid dispersion and 64g aqueous dispersion of polytetrafluoroethyland are weighed, is stirred in magnetic stirring apparatus 1.5h is mixed, the aqueous self-lubricating dispersions of 106.6g are obtained standby.
(4) preparation of composite band rust transforming agent:Weigh 5.5g tannic acid to be dissolved in 15g water, then add thereto 1.5g pyrogallic acid, finally instills 1g ethanol solution thereto, and magnetic agitation 0.5h obtains 21.4g composite bands rust and turned Agent is standby.
(5) 30g deionized waters are weighed in the three-necked flask with agitating device, magnetic agitation is separately added into thereto Obtained composite band rust transforming agent in 5g aluminium triphosphates, 4g trbasic zinc phosphates and 3.5g sericites and 13g above-mentioned steps (3), then It is placed in XQM-6 planetary ball mills, revolution speed is adjusted to 140rpm, rotational velocity is obtained after being adjusted to 460rpm, grinding 6h 55.5g raw material for standby.
(6) raw material 55.5g obtained in above-mentioned steps (5) is weighed in the three-necked flask with agitating device, rotating speed 60rpm is adjusted to, it is slow respectively to add the polyether-modified silicon of 1.25g defoamers, 0.15g wetting agent BYK-346,0.2g levellings thereto Aqueous self-lubricating dispersion obtained by agent and 23g above-mentioned steps (3), 150rpm is adjusted to by rotating speed, stirring 30min after again to Wherein add ambient self-crosslinking water-base epoxy obtained by 25g above-mentioned steps (2).Continue to stir after 1.5h, then add thereto After 2.5g pH adjusting agent salicylic acids, stirring 20min, that is, a kind of underloading aqueous rusty self-lubricating coat in use is made.
Embodiment 6
(1) preparation of aqueous epoxy curing agent:
1. weigh in 42g aromatic multi-amine and 38g butanediol ether, the three-necked flask for being added into a 250ml, water-bath 62 DEG C are heated to, after 200rpm speed stirring 1.5h, then 0.7g oxalic acid is added dropwise thereto, obtains 78.7 solution As standby.
2. 78g novolac epoxy resins are weighed and 7g butanediols ether is put into another 250ml there-necked flask, heating water bath is arrived 85 DEG C, stirred with 200rpm rotating speed, after novolac epoxy resin is completely dissolved, add 19.5g triethanolamines, react 3h, plus 0.9g oxalic acid, obtains 101.1 solution Bs standby.
3. the step of weighing 3g lauryls glycidol ether, 55g 2. in obtained solution B in three mouthfuls of new 250ml In flask, then obtained solution A in adding 27g steps thereto 1., with 400rpm rotating speed stirring and heating water bath to 85 DEG C reaction 3~4h, obtain 81.4g aromatic multi-amine novolac epoxy resins.
4. obtained aromatic multi-amine novolac epoxy resin is under 1500~1800rpm of rotating speed in weighing 43.5g steps 3. Stirring, plus 8.5g water are carried out after phase reversal 5h, and 49.8g aqueous epoxy curing agents are made.
(2) preparation of ambient self-crosslinking water-base epoxy:0.8g formic acid is weighed in the three-necked flask with agitating device, Rotating speed is adjusted to 75rpm, aqueous epoxy curing agent made from 21g above-mentioned steps (1) is added in the state of being stirred on side, after 10 minutes 83g aqueous epoxy resins are added thereto, continue to stir 30min, the ambient self-crosslinking water-base epoxy that 101.8g is made is standby.
(3) preparation of aqueous self-lubricating dispersion:
1. the preparation of Tissuemat E aqueous liquid dispersion:
A. 69g water is weighed in the four-hole boiling flask with agitating device;
B. 0.05gN is weighed, N- diethylanilines and 0.2g benzoyl peroxides are dissolved in 6g dimethylbenzene;
C. the product in step b is put into the four-hole boiling flask in step a, then be separately added into thereto 4g acrylic acid and 24g Tissuemat E powder, is warming up to 55 DEG C, leads to N2100min is swelled, then is warming up to predetermined 87 DEG C of reaction temperature, 2h is reacted Afterwards, 2.4g lauryl sodium sulfate and 0.6g Tween 80s are added thereto, 102 DEG C are warming up to, and are emulsified 40min, are naturally cooled to 45 DEG C of dischargings, are made 94.2g Tissuemat E aqueous liquid dispersions.
2. the preparation of aqueous dispersion of polytetrafluoroethyland:Added into polymeric kettle 77g high purity water, 0.75g perfluor it is pungent The benzoyl peroxide of sour ammonium and 0.03g, closes polymeric kettle, opens stirring, and rotating speed is adjusted to 100rpm, is 1.6MPa in pressure, At 21 DEG C of temperature control carry out vacuum experiment and pressurize experiment, it is qualified after be passed through high pure nitrogen thereto, in the course of the polymerization process with The mode continuously added adds 25g tetrafluoroethene, maintains after the constant 7h of polymerization pressure, stops charging and stirs, uses N2Exclude Unreacted monomer, obtains 101.3g aqueous dispersion of polytetrafluoroethyland.
3. 43g Tissuemat Es aqueous liquid dispersion and 64g aqueous dispersion of polytetrafluoroethyland are weighed, is stirred in magnetic stirring apparatus 1.5h is mixed, the aqueous self-lubricating dispersions of 106.3g are obtained standby.
(4) preparation of composite band rust transforming agent:Weigh 5.5g tannic acid to be dissolved in 15g water, then add thereto 1.5g pyrogallic acid, finally instills 1g ethanol solution thereto, and magnetic agitation 0.5h obtains 21.2g composite bands rust and turned Agent is standby.
(5) 35g deionized waters are weighed, magnetic agitation is separately added into 6g aluminium triphosphates, 5g trbasic zinc phosphates and 4g thin,tough silk thereto Obtained composite band rust transforming agent in mica and 15g above-mentioned steps (4), then be placed in XQM-6 planetary ball mills, revolve round the sun Speed is adjusted to 140rpm, and rotational velocity is adjusted to 460rpm, and grinding 6h obtains raw material for standby.
(6) raw material 65g obtained in above-mentioned steps (5) is weighed in the three-necked flask with agitating device, and rotating speed is adjusted To 60rpm, respectively it is slow add thereto the polyether-modified silicon of 1.5g defoamers, 0.2g wetting agent BYK-346,0.3g levelling agents and Obtained aqueous self-lubricating dispersion in 25g above-mentioned steps (3), rotating speed is adjusted to after 150rpm, stirring 30min again thereto Add ambient self-crosslinking water-base epoxy obtained in 29g above-mentioned (2).Continue to stir after 1.5h, then add 4g pH thereto and adjust Save after agent salicylic acid, stirring 20min, that is, a kind of underloading aqueous rusty self-lubricating coat in use is made.
Comparative example
Preparation method and consumption be the same as Example 1, but without the aqueous self-lubricating dispersion obtained by embodiment 1.2nd, originally The performance test of invention underloading aqueous rusty self-lubricating coating
1. resistance to salt water is tested:Pre- processing of rust removing is carried out to the Q235 steel plates with rust under normal temperature, makes its rusty scale thickness in 30 μ M or so, is then coated on surface of steel plate by the coating obtained by embodiment 1,2,3,4,5,6 and comparative example respectively, spontaneously dries After mass fraction is put into soak 72h in 5%NaCl solution, surface is observed after drying.
2. salt mist experiment:The steel plate that embodiment 1,2,3,4,5,6 and comparative example coating is respectively coated is placed in salt fog cabinet In;The salting liquid that mass fraction is 5% is wherein made into deionized water, at a temperature of 25 DEG C, pH is measured 6.5 with acidometer Between~7.2, density is 1.03~1.04g/L;Neutral salt fog chamber temperature is set as 35 ± 1 DEG C, relative humidity is 96 ± 2 DEG C (%), salt fog deposition velocity is:After being sprayed through 24h, per 80cm2It is 1~2ml/h on area.
Q325 steel plates are tested area with a vertical 15 in salt fog cabinet~30Angle, can be placed in salt fog cabinet not On same level face, casing must not be contacted, it is impossible to contact with each other.One spray salt fog cycle of regulation is continuous spraying 8h, constant temperature and humidity 16h is incubated under environment.
3. frictional wear experiment:By the aqueous rusty self-lubricating coating obtained by embodiment 1,2,3,4,5,6 and comparative example Surface of steel plate is coated on, in 150N load, 20mm/s speed, under conditions of the 300s testing times, fretting wear is carried out to it real Test.As a result it is as shown in the table.
The addition that can be seen that aqueous self-lubricating dispersion from the data in table significantly reduces the coefficient of friction of coating, With good self-lubricating property.

Claims (4)

1. a kind of steel surface underloading aqueous rusty self-lubricating coating, it is characterised in that the coating is by following parts by weight of component Composition:
Described aqueous self-lubricating dispersion is 36~43 parts of Tissuemat E aqueous liquid dispersions and 57~64 parts of polytetrafluoroethylene (PTFE) water The compound of property dispersion liquid;
The composite band rust transforming agent is that 4.5~5.5 parts of tannic acid and 1.5~0.5 parts of pyrogallic acid are dissolved in 10~15 In the water of part, then it is added dropwise thereto obtained in 0.5~1 part of ethanol solution;
The defoamer is tributyl phosphate or polyether-modified silicon;
The wetting agent is Tego Wet KL 245 or BYK-346;
The levelling agent is isophorone and DAA in mass ratio 1:1 mixed liquor;
The pH adjusting agent formic acid and one kind or mixed liquor in salicylic acid.
2. steel surface underloading aqueous rusty self-lubricating coating as claimed in claim 1, it is characterised in that it is described it is aqueous from Tissuemat E aqueous liquid dispersion in lubrication dispersion is through the following steps that prepared:
A. 61~69 parts of water are weighed in the four-hole boiling flask with agitating device;
B. 0.01~0.05 part of N is weighed, N- diethylanilines and 0.1~0.2 part of benzoyl peroxide dissolve in 4~6 parts of dimethylbenzene In;
C. the product in step b is put into the four-hole boiling flask in step a, then be separately added into thereto 3~4 parts of acrylic acid and 18~24 parts of Tissuemat E powder, is warming up to 50~55 DEG C, leads to N280~100min is swelled, then is warming up to predetermined reaction temperature 85~87 DEG C, react after 1.5~2h, then add 1.8~2.4 parts of lauryl sodium sulfate and 0.3~0.6 part of tween thereto 80,98~102 DEG C are warming up to, 35~40min is emulsified, naturally cools to 45 DEG C of dischargings, that is, Tissuemat E aqueous liquid dispersion is made.
3. steel surface underloading aqueous rusty self-lubricating coating as claimed in claim 1, it is characterised in that it is described it is aqueous from Aqueous dispersion of polytetrafluoroethyland in lubrication dispersion is through the following steps that prepared:
The high purity water of 72~77 parts of addition, 0.5~0.75 part of dispersant perfluorooctanoic acid and 0.015~0.03 into polymeric kettle Part initiator benzoyl peroxide, close polymeric kettle, open stirring, rotating speed is adjusted to 80~100rpm, pressure be 1.5~ 1.6MPa, temperature control be 17~21 DEG C at carry out vacuum experiment and pressurize experiment, it is qualified after be passed through high pure nitrogen thereto, 21~25 parts of tetrafluoroethene is added in the way of continuously adding in polymerization process, maintains after the constant 6~7h of polymerization pressure, stops Charging and stirring, use N2Unreacted monomer is excluded, that is, obtains aqueous dispersion of polytetrafluoroethyland.
4. a kind of preparation method of steel surface underloading aqueous rusty self-lubricating coating as claimed in claim 1, its feature It is to comprise the following steps:
(1) preparation of aqueous epoxy curing agent:
A, the aromatic multi-amine for weighing 37~42 parts and 33~38 parts of butanediol ether, are added into three-necked flask, water-bath adds Heat is stirred after 1~1.5h to 58~62 DEG C with 150~200rpm speed, then 0.5~0.7 part of oxalic acid is added dropwise thereto, is obtained Solution A is standby;
B, weigh 73~78 parts of novolac epoxy resins and 4~7 parts of butanediol ether are put into another three-necked flasks, heating water bath is arrived 85 DEG C, stirred with 150~200rpm rotating speed, after novolac epoxy resin is completely dissolved, add 14.6~19.5 part of three ethanol Amine, reacts 2~3h, plus 0.6~0.9 part of oxalic acid, obtains solution B standby;
C, obtained solution A is weighed in 2~3 parts of lauryl glycidol ethers, 50~55 parts of step a in three mouthfuls of 250ml In flask, then solution B obtained in 22~27 parts of step b is added thereto, with 200~400rpm rotating speed stirring and water-bath 85 DEG C of 3~4h of reaction are heated to, aromatic multi-amine novolac epoxy resin is obtained;
D, weigh in 81~87 parts of step c obtained aromatic multi-amine novolac epoxy resin and stirred under 1500~1800rpm of rotating speed Mix, plus 13~17 parts of water carry out that aqueous epoxy curing agent is made after 3~5h of phase reversal;
(2) preparation of ambient self-crosslinking water-base epoxy:0.5~0.8 part of formic acid is weighed in the three-necked flask with agitating device In, rotating speed is adjusted to 50~75rpm, and water-base epoxy made from 16~21 parts of above-mentioned steps (1) is added in the state of being stirred on side and is consolidated Agent, adds 75~83 parts of aqueous epoxy resins thereto after 10 minutes, continue to stir 30min, obtained ambient self-crosslinking water Property epoxy is standby;
(3) preparation of aqueous self-lubricating dispersion:Weigh 36~43 parts of Tissuemat E aqueous liquid dispersions and 57~64 parts of polytetrafluoros Ethene aqueous liquid dispersion, stirs 1.5h in magnetic stirring apparatus, obtains aqueous self-lubricating dispersion standby;
(4) preparation of composite band rust transforming agent:4.5~5.5 parts of tannic acid are weighed to be dissolved in 2~4 parts of ethanol solution, then to its The middle pyrogallic acid for adding 1.5~0.5 parts, magnetic agitation 0.5h obtains composite band rust transforming agent standby;
(5) 25~35 parts of deionized waters are weighed, magnetic agitation is separately added into 4~6 parts of aluminium triphosphates, 3~5 parts of phosphorus thereto Composite band rust transforming agent obtained by sour zinc, 3~4 parts of sericites and 11~15 parts of above-mentioned steps (4), then it is placed on XQM~6 In planetary ball mill, revolution speed is adjusted to 140rpm, and rotational velocity is adjusted to 460rpm, and grinding 6h obtains raw material for standby;
(6) 46~65 parts of raw material obtained in above-mentioned steps (5) is weighed in the three-necked flask with agitating device, and rotating speed is adjusted To 50rpm, respectively it is slow add thereto 1~1.5 part of defoamer, 0.1~0.2 part of wetting agent, 0.1~0.3 part of levelling agent and Aqueous self-lubricating dispersion obtained by 20~25 parts of above-mentioned steps (3), 150rpm is adjusted to by rotating speed, after stirring 30min again to Wherein add ambient self-crosslinking water-base epoxy made from 20~29 parts of steps (2);Continue to stir after 1.5h, then add 1 thereto ~4 parts of pH adjusting agents, are adjusted to 3~5 by the pH of coating, produce target product.
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CN112176328A (en) * 2020-09-27 2021-01-05 常州大学 Rust conversion agent based on 3,4, 5-trihydroxybenzoic acid and preparation method thereof
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CN108659702A (en) * 2018-06-14 2018-10-16 上海安弗柯林工业科技有限公司 A kind of food-grade ball valve slip coating and preparation method
CN109535939A (en) * 2019-01-16 2019-03-29 深圳市永宏半导体生物科技有限公司 Anti-corrosive primer and its application
CN112176328A (en) * 2020-09-27 2021-01-05 常州大学 Rust conversion agent based on 3,4, 5-trihydroxybenzoic acid and preparation method thereof
CN114369410A (en) * 2021-12-30 2022-04-19 广州千顺工业材料有限公司 Black water-based graphene electromagnetic wave shielding coating and preparation method thereof

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Application publication date: 20170829