CN101486871A - Preparations of underwater coating heavy anti-corrosive paint and coating resin - Google Patents
Preparations of underwater coating heavy anti-corrosive paint and coating resin Download PDFInfo
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Abstract
The invention discloses a method for preparing an underwater application heavy-duty coating and coating resin. The heavy-duty coating is prepared by adding epoxy hardener into the coating resin, wherein, the epoxy hardener is made by carrying out polymerization modification deep processing to screened hardener basic materials. The coating resin is made by carrying out deep processing to screened epoxy resin and has chelating and rust conversion function and good siderophile property. The underwater application anti-corrosion coating can be fast hardened in fresh and sea water, with the hardening time being within 30min, and is characterized by low surface treatment, innocuity, no VOC emission, good acid, alkali, water and salt resistance, good adhesion, and the like.
Description
Technical field
The present invention relates to paint field, be specifically related to the preparation method of underwater coating heavy corrosion protection coating and coating resin.
Background technology
Underwater coating heavy corrosion protection coating has very important meaning to the underwater operation engineering, be military affairs or civilian aspect underwater coating heavy corrosion protection coating it is all had far-reaching influence.
Military requirement: China's naval equipment (as capital ship, submarine so that seaplane carrier in the future) is executed the task in the ocean for a long time, be about three to five years the period of generally returning the depressed place maintenance, as in the meantime, indivedual positions on naval vessel are bumped because of wiping or other is former thereby when causing a layer portion paint film to lose efficacy, repair as too late, can cause the paint film global failure of whole ship, cause immeasurable loss.As repair and need stop to execute the task to debark and return the depressed place maintenance, also cause greater loss.In addition, military harbour and the long period of soaking military equipment in the ocean also can not move to land and keep in repair, therefore develop and a kind ofly novel can hang down surface treatment in fresh water or seawater, directly the coating that loses of painting anticorrosion is obviously very necessary, has far-reaching strategic importance.
Civilian demand: the offshore oil production equipment (as marine drilling platform, submerged pipeline etc.) of Chinese large-sized and the large-scale long period of soaking equipment (as equipment for hydroelectric station, commercial dock and large vessel etc.) in water, when taking place, corrosion wants to keep in repair very difficulty at the environment of exclusion of water, reach the ideal preservative effect if there is a kind of anticorrosive coating directly to repair at underwater work, then the protection against corrosion protection to the equipment of long period of soaking in water is a breakthrough revolution, has epoch making significance.Meanwhile, this technical products can be used non-underwater environment, because its low surface treatment, zero VOC discharging and water-fast and wet environment can be widely used in bridge, mining equiment, hydraulic power equipment.Especially in the protection against corrosion of chemical gas tank, oil tank.
Countries in the world are infusion of financial resources research and development painting under water coating products one after another all, and that releases ripe series product at present has only Portugal excellent long paint company.Especially its ES323 painting under water product is respectively in the U.S., Brazil, Germany, Holland, Norway, Spain, Britain, France, Greece, Arab and Southeast Asian countries widespread use, Chinese Navy also once used this product in the part significant points, but can't big area promote because of too expensive (about 350 yuan of the per kilogram) of coating.U.S. Ya Meilong company is the key supplier of the military coating of the U.S. always, wholeheartedly developing the painting under water product, world heavy-duty coating giants such as Denmark Hempel company, Japanese Northwest company, Norway assistant pier company are developing the painting under water coating products one after another.Say that from technology the research direction of painting under water coating all is to develop along the solventless epoxy coating direction in the world at present, excellent imperial company uses sophisticated product and also all is based on the basis of Resins, epoxy basis material.Simultaneously, from the research of painting under water coating in the world, find, because the pre-treatment work of equipment is very difficult in the water, can not reach strict rust cleaning effect, therefore all painting under water coating all must possess low surface treatment properties, the curing speed of coating must guarantee a fast speeds simultaneously, otherwise is just washed away by sea water immersion before coating does not have enough time to solidify.
Begin the domestic eighties to have carried out some basic researchs with regard to the painting under water product, study for a long period of time the application of underwater epoxy resin of Changsha chemical institute, annual country drops into a large amount of scientific and technological funds to Qingdao Haiyang research institute, the corrosion and protection of primary study ocean environment equipment, this institute has also carried out the basic research of some painting under water.Along with going deep into of reform and opening-up, forward-looking private enterprise also recognizes the market outlook that painting under water coating is following huge in China's coating industry, as Aston, Shenzhen coating Asdon63919 product, the painting under water technical elements is also obtained certain application effect.
The made coating products of this technical products belongs to solventless coatings, and promptly zero VOC discharging is the green chemical industry product that meets national requirements for environmental protection.
Summary of the invention
The object of the present invention is to provide a kind of VOC free discharging,, solidify in the seawater, have good acidproof, alkaline-resisting, water-fast and salt tolerant part performance, the sticking power painting under water coating that tool is good at fresh water.
For realizing the object of the invention, we will carry out modification to the Resins, epoxy that screens, and its tool huge legendary turtle is closed changes rust function and good affinity for iron.In the common Resins, epoxy, a kind of dihydroxyphenyl propane Racemic glycidol ether type epoxy is commonly referred to bisphenol A epoxide resin, accounts for 90% of Resins, epoxy ultimate production, is generally the first-selected product of heavy-duty coating.Screening Resins, epoxy, emphasis will take in from following characteristic index:
A) oxirane value (E): the equivalents of the epoxy that contains in the 100g resin, contain two end epoxy group(ing) in each Resins, epoxy molecule, so molecular weight is big more, oxirane value is more little.
B) epoxy equivalent (weight) (Q): contain the gram number of an equivalent epoxy, Q is just in time opposite with E with the relation of molecular resin amount, Q=100/E
C) hydroxyl value (OH): the hydroxyl value that contains in the 100g resin, corresponding hydroxyl equivalent in addition.
D) viscosity: this research product is because belong to solvent-free product, and for preparation has the coating of suitable working viscosity, the viscosity of resin film forming matter is just very important.
Selected Resins, epoxy is (specific requirement) lower molecular weight bisphenol A epoxide resin among the present invention, 2, and 2-bis (p (2,3-epoxypropoxy) phenyl) propane, DGEBA.
We handle by the deep processing modification that reactor carries out appropriateness Resins, epoxy, pigment, filler, make its brushing when steel surface, rapid and steel surface carries out huge legendary turtle and closes, the carrying out of in film forming process, closing along with huge legendary turtle, with the crystal water extruding coating in moisture in the steel surface pin hole and the rust, the solidification process of coating is actual to be exactly that huge legendary turtle is closed conversion process, and the dried fully Gu Shiao of coating closes end of processing.
Along with firm rusty scale surface, carry out huge legendary turtle through the epoxy base material of modification iron molecule same and rusty scale and close, constantly get rid of the moisture content in the iron rust, may (therefore not have the existence of water thereby cut off the further corrosive of iron rust, electrochemistry can not be carried out), thus reach the purpose that huge legendary turtle is closed changes rust.
Introduce concrete synthesis modification method below
This synthetic two-step approach that adopts, at first synthetic A resin, resynthesis B resin, the B resin that has synthesized are used for the main resin of first component of the preparation of coating, and be specific as follows:
A resin synthesizing formula and technology
Weight ratio
1. phenol 100
2. formaldehyde 150
3. tannin 100
4. silver powder, zinc powder, ethylene glycol monoethyl ether, dimethylbenzene, boiling water mixing solutions 4
5. oxalic acid 1
6. reactive thinner 150
Add up to 505
Weigh up 1+2 by formula ratio and put into reactor, stir and to be warming up to 40 ℃, add after No. 3 raw materials are warming up to 60 ℃, kept 1.5-2 hour.Add No. 4 raw materials and be warming up to 80 ℃ of insulations 2-2.5 hour, tannin is dissolved fully, be thick.Add No. 5 raw materials 80 ℃ of insulations 1-1.5 hour, solution reaches golden yellow phase, and the silver powder uniform distribution has pulled thread.Be warming up to 90 ℃ of insulations 4-5.5 hour again, be warming up to reflux temperature reaction 5-8 hour again, vacuumize dehydration after inspection by sampling is qualified, add 6 and stir 1-1.5 hour even back, be used to make the main resin of coating first component as the A resin.
B resin synthesizing formula and technology
Weight ratio
1. reactive thinner 50
2.A resin 70
3.100% contains liquid bisphenol A Resins, epoxy 400 admittedly
4. the secondary synthetic fatty acid 55
5. reactive thinner 70
Add up to 645
Weigh up 1+2 by formula ratio and put into reactor, stirring is warming up to 50 ℃, add No. 3 raw materials and be warming up to reflux temperature 135-170 ℃ of reaction 10-12 hour, remove generation water, to the anhydrous raw material that adds again No. 4 that refluxes, continue to stop heating 170-180 ℃ of reaction 4-6 hour, be cooled to 120 ℃, add 5 uniform mixing.Filtering and sampling send system lacquerer section as the B resin after the assay was approved, is used to make the first component coating.
The preferred glycidyl allyl ether of reactive thinner in described A resin, the B resin formula.
B resin technology index is as follows:
1. viscosity: 10-15pa.m
2. proportion: 1.15-1.19
In order to realize that painting under water coating solidifies in fresh water, seawater, need in coating, add epoxy hardener, i.e. the component B of coating.At present, the epoxy hardener of the various trades mark of commercial use mainly is the solidifying agent of polyamine and modification thereof, generally is divided into; A) polyamine: as quadrol, diamines, diethylenetriamine etc.B) polyamide curing agent.C) epoxy-polyamine affixture solidifying agent.D) pnenolic aldehyde amine hardener.E) ketoimine solidifying agent.
Painting under water coating is the non-solvent epoxy type, must consider when selecting solidifying agent and mix short factor duration of service.
In addition, the control of Resins, epoxy and amine hardener consumption, the corresponding epoxy group(ing) of a reactive hydrogen on the amino is carried out crosslinking reaction theoretically, and available following formula calculates:
W
e=Ma/H
n×E
W in the formula
eThe gram number that-100% Resins, epoxy is consumed
The relative molecular mass of Ma-amine
H
n-reactive hydrogen number
E-Resins, epoxy oxirane value
The solidifying agent of the present invention's screening is the means screening by test, finally adopts the painting under water solidifying agent of synthetic 100% solids content of high amine value polyamide resin and poly aldehyde and many ketone.
The process of coating process solidifying agent is a modification deep-processing process under the synthetic water, press certain technology, control certain hour and temperature by reactor, the solidifying agent base mateiral that has screened is carried out the polymeric modification deep processing, make it reach mixed coating and have draining affinity for iron energy, quicken the penetrating quality of curing speed and iron and steel in the water simultaneously.
Solidifying agent C resin synthesizing formula and technology
Weight ratio
1. many kinds of polyketone synthesis (being called for short many ketone) 90
2. polyamide resin 250
3. the nonyl phenol resin 180
4. poly aldehyde 48
Add up to 568
By the prescription weighing, add 1,2,3,4 raw materials to reactor, start is stirred and is warming up to 70 ℃, stops heating, and the control temperature in the kettle (prevented thermal response in 1-1.5 hour less than 80 ℃ 80 ℃ of insulations.Temperature surpasses 96 ℃ can the vigorous reaction boiling), be warming up to 90 ℃ of insulations 1-2 hour again, be warming up to 100 ± 5 ℃ of insulations 1-2 hour again, divide and to remove the water that generates, stopped reaction vacuumizes dehydration, vacuumize the recovery low-boiling-point substance afterwards again, the after-filtration that stirs as the C resin, is the main raw material of coating curing agent component B.
The preferred Paraformaldehyde 96 of poly aldehyde in the described C resin formula.
Underwater coating heavy corrosion protection coating of the present invention is formed (weight ratio) by first component and solidifying agent second component; Described first component is to be base-material with the B resin, adds coating again and grinds together with universal pigment, filler, auxiliary agent etc., through paint, adjust the mixture after the viscosity; Described second component is C resin or the mixture be made up of C resin and tertiary amines curing catalyst.
Underwater coating heavy corrosion protection coating prescription one: first component: component B=4:1 (weight ratio);
Wherein first component prescription is:
Raw material weight %
B resin 50
Anti-sag agent (Ployethylene Wax) 1
Iron oxide red 10
Silica powder 8
Magnesium Silicate q-agent 8
Ground barium sulfate 8
Lime carbonate 15
Add up to 100
The second component is the C resin.
Underwater coating heavy corrosion protection coating prescription two: first component: component B=5:1 (weight ratio), wherein the first component consists of:
Raw material weight %
B resin 50
Anti-sag agent (Ployethylene Wax) 1
The moistening dispersing auxiliary 0.25 of BYK
Soybean lecithin 0.2
Boron-moisten soil 1
Plasticizer DIDP 8
Titanium dioxide 10
Iron oxide red 5
Silica powder 8
Fibrous talc 11
Ground barium sulfate 13
Glass flake 20
Glycidyl allyl ether 10
Add up to 137.45
The second component is made up of C resin and tertiary amines curing catalyst, and it is as follows to fill a prescription,
Raw material weight %
C resin 80
Tertiary amines curing catalyst 20
Add up to 100
Compared with prior art, painting under water protective system provided by the invention fast setting in fresh water, seawater, set time is in 30 minutes, and has low surface treatment, nontoxic, the VOC free discharging, acidproof, alkaline-resisting, water-fast and salt tolerant part performance that tool is good, the characteristics such as sticking power that tool is good.
Embodiment
Further specify the present invention with specific embodiment below, but be not restriction the present invention.
Embodiment 1
The A resin
1. reinforced (1) phenol is heated to mobile, sucks 100kg in the still (stirring start) with vacuum
(2) formaldehyde 37% rolls and mixes, and vacuum sucks 150kg in the still (stirring start)
2. vapor phase temperature adds tannin 100kg to 45-50 ℃ in pre-reaction (1) the intensification still, and the reinforced time is about 1 hour.
(2) stir, be warming up to 80 ℃, be incubated 1-1.5 hour.
(3) add silver powder, zinc powder, ethylene glycol monoethyl ether, dimethylbenzene, the boiling water mixing solutions was waited for 4kg, 80-82 ℃ of insulation 2-2.5 hour.
3. formal reaction (1) adds oxalic acid 1kg
(2) 85 ℃ of reactions of heating and heat preservation are 1 hour.
(3) 90 ℃ of reactions of heating and heat preservation are 4 hours.
(4) heating and heat preservation 100-102 ℃ was reacted 5-6 hour.
4. sampling detects: the about 100ml of sampling at the bottom of the still, to drop in the water, and when not stirring, material sinks under water fast, stirs a little, is dispersed into small-particle, leaves standstill 10-15 minute at once, and the color of water is yellow slightly transparent, and material goes to draw with hand have been understood thread.
5. vacuumize dehydration
The vapor phase temperature vacuum tightness water yield in the time still
85 ℃ of 0.6-0.7 were a large amount of in 10 minutes
69 ℃ of 0.7-0.85 were a large amount of in 30 minutes
1 hour 62 ℃ 0.9 a small amount of
1.5 hour 61 ℃ of 0.9 a small amount of
6. dissolving stops heating, and vacuum sucks the about 150kg of glycidyl allyl ether thinner, stirs 1 hour.
7. get material and detect, viscosity is qualified, waits until subsequent processing.
The B resin
1. enrich among the reactor B
(1) adds solvent-free polyketone class 250kg. and add A resin 350kg.
(2) add bisphenol A epoxide resin 2000kg, start stirs.
(3) add dimeracid 225kg in still.
(4) add 350kg glycidyl allyl ether thinner in the B reactor.
2. beginning temperature reaction
Vapor phase temperature ℃ in the timed interval oil temperature ℃ still
1 hour 80 38
1 hour 90 45
1 hour 100 63
1 hour 100 80
1 hour 110 90
1 hour 120 106 (beginning to reflux)
1 hour 120 116
1 hour 140 125
1 hour 150 129
1 hour 160 138
1 hour 170 140
1 hour 180 142
1 hour 190 145
1 hour 190 148
1 hour 190 150
The reaction two-stage: (adding dimeracid 225kg)
1 hour 190 150
1 hour 190 152
1 hour 190 155
Stopped heating in 1 hour 190 155, cooling vacuumize anhydrous after, add the discharging that stirs of 350kg glycidyl allyl ether thinner.
The C resin
1. reinforced
(1) increases amine value polyamide resin 250kg in reactor C
(2) add nonyl phenol 180kg.
(3) add polyketone 90kg, start is stirred.
(4) add solid formaldehyde 48kg, heat up.
2. reaction
Vapor phase temperature ℃ in the timed interval oil temperature ℃ still
Rose 25 in 0 hour
1 hour 55 42
1 hour 65 48
1 hour 73 54
1 hour 77 62
Stopped to heat 72 in 1 hour
1 hour 82 80
1 hour 93 85
(insulation) 89 in 1 hour 100
1 hour 107 92
(insulation) 95 in 1 hour 115
1 hour 103
1 hour 105
1 hour 105
3. vacuum hydro-extraction
The warm vacuum tightness water yield of vapor phase temperature oil in the time still
30 minutes 98 ℃ 120 ℃ 0.4 medium
1 hour 90 ℃ 125 ℃ 0.6 a large amount of
1.5 hours 76 ℃ 130 ℃ 0.75 a large amount of
2 hours 72 ℃ 140 ℃ 0.8 a large amount of
3 hours 70 ℃ 140 ℃ 0.8 a large amount of
3.5 hour 73 ℃ 140 ℃ 0.9 a small amount of
4 hours 80 ℃ 140 ℃ 0.9 a small amount of
4 hours 40 minutes 88 ℃ 140 ℃ 0.9 nothings
4. stop heating, stir discharging.
As binder resin, add the coating universal pigment with the B resin again, filler, auxiliary agent etc. grind together, through paint, adjust viscosity, through packing as coating first component after the assay was approved.Concrete prescription is as follows:
The first component
Raw material weight %
1. the B resin 50
2. anti-sag agent (Ployethylene Wax) 1
3. iron oxide red 10
4. silica powder 8
5. Magnesium Silicate q-agent 8
6. ground barium sulfate 8
7. lime carbonate 15
Add up to 100
Technical indicator:
The actual measurement of index standard
Fineness 80u 72u
Viscosity greater than 100KU greater than 100KU
Proportion 1.55-1.85 1.65
Sagging 200u 525u
Surface drying was less than 1 hour 48 minutes surface dryings (30 ℃ of water temperatures)
Blade coating is good under water
Component B:
Raw material weight %
C resin 100
Add up to 100
Construction blending ratio: first component: component B=4:1 (weight ratio)
The application under water of this coating, constructional method adopts blade coating, and the construction surface treatment can be by artificial rust cleaning or water blast gun rust cleaning, and must not there be loosening floating rust on the construction surface in principle.
Embodiment 2
Needing the good occasion of brushing characteristic, as follows by adjusting the formula material ratio:
The first component
Raw material weight %
1. the B resin 50
2. anti-sag agent (Ployethylene Wax) 1
3. the moistening dispersing auxiliary 0.25 of BYK
4. the soybean lecithin 0.2
5. boron-moisten soil 1
6. plasticizer DIDP 8
7. titanium dioxide 10
8. iron oxide red 5
9. silica powder 8
10. fibrous talc 11
11. ground barium sulfate 13
12. glass flake 20
13. glycidyl allyl ether thinner 10
Add up to 137.45
Technical indicator:
The actual measurement of index standard
Fineness 80u 72u
Viscosity 90-100KU 97KU
Proportion 1.35-1.75 1.55
Sagging 200u 400u
1.5 hours 100 minutes surface dryings (30 ℃ of water temperatures) of surface drying
Brushability is good under water
Component B:
Raw material weight %
C resin 80
Tertiary amines curing catalyst 20
Add up to 100
Construction blending ratio: first component: component B=5:1 (weight ratio)
Application under water, constructional method are adopted and are brushed, and the construction surface treatment can be by artificial rust cleaning or water blast gun rust cleaning, and must not there be loosening floating rust on the construction surface in principle.By being mixed in proportion, the depths sends the frogman directly to brush in the requirement construction part again.
Claims (8)
1. a underwater coating heavy corrosion protection coating is made up of first component and solidifying agent second component, and described first component is to be base-material with the B resin, adds the coating universal pigment again, and filler, auxiliary agent etc. grind together, through paint, adjusts the mixture after the viscosity; Described second component is C resin or the mixture be made up of C resin and tertiary amines curing catalyst;
B resin in the described first component is composed as follows:
Weight ratio
Reactive thinner 50
A resin 70
100% contains liquid bisphenol A Resins, epoxy 400 admittedly
Secondary synthetic fatty acid 55
Reactive thinner 70
Add up to 645
A resin in the described B resin is composed as follows:
Weight ratio
Phenol 100
Formaldehyde 150
Tannin 100
Silver powder, zinc powder, ethylene glycol monoethyl ether, dimethylbenzene, boiling water mixing solutions 4
Oxalic acid 1
Reactive thinner 150
Add up to 505
Described C resin composed as follows,
Weight ratio
Solvent-free many ketone 90
Polyamide resin 250
Nonyl phenol resin 180
Poly aldehyde 48
Reactive thinner 300
Add up to 868
2. coating according to claim 1, described reactive thinner is a glycidyl allyl ether.
3. coating according to claim 1 is characterized in that, first component: component B=4:1 (weight ratio); Described first component prescription is:
Raw material weight %
B resin 50
Anti-sag agent 1
Iron oxide red 10
Silica powder 8
Magnesium Silicate q-agent 8
Ground barium sulfate 8
Lime carbonate 15
Adding up to 100 described second components is the C resin.
4. coating according to claim 1 is characterized in that, first component: component B=5:1 (weight ratio), and described first component consists of:
Raw material weight %
B resin 50
Anti-sag agent 1
The moistening dispersing auxiliary 0.25 of BYK
Soybean lecithin 0.2
Boron-moisten soil 1
Plasticizer DIDP 8
Titanium dioxide 10
Iron oxide red 5
Silica powder 8
Fibrous talc 11
Ground barium sulfate 13
Glass flake 20
Glycidyl allyl ether thinner 10
Add up to 137.45
Described second component is made up of C resin and tertiary amines curing catalyst, the C resin: tertiary amines curing catalyst=80:20 (weight ratio).
5. the preparation method of A resin in claim 1 coating comprises following steps:
(1) will put into reactor by load weighted phenol of prescription and formaldehyde, and stir and be warming up to 45-50 ℃,
(2) add the tannin raw material, be warming up to 60 ℃ after, kept 1.5-2 hour;
(3) mixing solutions that adds silver powder etc. is warming up to 80-82 ℃, is incubated 2-2.5 hour, and tannin is dissolved fully, is thick;
(4) add the oxalic acid raw material 80 ℃ of insulations 1-1.5 hour, solution reaches golden yellow phase, and the silver powder uniform distribution is warming up to 90 ℃ of insulations 4-5.5 hour again, is warming up to reflux temperature reaction 5-8 hour again, vacuumizes dehydration after inspection by sampling is qualified;
(5) add reactive thinner and stir 1-1.5 hour even back as the A resin.
6. the preparation method of B resin in claim 1 coating comprises following steps:
(1) will put into reactor by reactive thinner and the described Resin A of claim 1 that formula ratio weighs up, and stir and be warming up to 50 ℃,
(2) add 100% and contain liquid bisphenol A Resins, epoxy admittedly, be warming up to reflux temperature 135-170 ℃ of reaction 10-12 hour, remove generation water,
(3) to the anhydrous dimeracid raw material that adds again that refluxes, continue to stop heating 170-180 ℃ of reaction 4-6 hour, be cooled to 120 ℃,
(4) with the reactive thinner uniform mixing, filtering and sampling is after the assay was approved as the B resin.
7. C process for preparing resins in claim 1 coating comprises following steps:
(1) will put into reactor by the load weighted solvent-free many ketone of prescription, polyamide resin, nonyl phenol resin and poly aldehyde raw material, start is stirred and is warming up to 70 ℃, stops heating, controls temperature in the kettle less than 80 ℃, 80 ℃ of insulations 1-1.5 hour,
(2) be warming up to 90 ℃ of insulations 1-2 hour again, be warming up to 100 ± 5 ℃ of insulations 1-2 hour again, divide and to remove the water that generates, stopped reaction vacuumizes dehydration,
(3) vacuumize the recovery low-boiling-point substance afterwards again, add the raw material reactive thinner, the after-filtration that stirs is as the C resin.
8. according to the described C process for preparing resins of claim 7, it is characterized in that poly aldehyde is Paraformaldehyde 96.
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