CN1468924A - Synthesis of high-molar ratio potassium silicate adhesive and aqueous anticorrosive paint composition - Google Patents
Synthesis of high-molar ratio potassium silicate adhesive and aqueous anticorrosive paint composition Download PDFInfo
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- CN1468924A CN1468924A CNA031125107A CN03112510A CN1468924A CN 1468924 A CN1468924 A CN 1468924A CN A031125107 A CNA031125107 A CN A031125107A CN 03112510 A CN03112510 A CN 03112510A CN 1468924 A CN1468924 A CN 1468924A
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Abstract
The synthesis of high-molar ratio potassium silicate adhesive includes adding water soluble silica sol to low-molar ratio potassium silicate solution, adding small amount of silane as blocking agent and adhesion reinforcer, adding proper stabilizer, and adding organic polymer emulsion to improve the filming property of the adhesive. One kind of anticorrosive paint composition obtained through compounding the adhesive and zinc powder is also disclosed.
Description
Technical field
The present invention relates to the synthetic method of high molar ratio potassium silicate binder and be the paint composite of active substance, belong to the chemical composition technical field with it.
Background technology
The report of making coating with inorganic silicate is more, and the metso that adopts low mol ratio is arranged, and has also that to adopt mol ratio be 4.8: 1 lithium silicate, and what United States Patent (USP) 4162169 adopted is the high molar ratio potassium silicate binder.Narrate low whipping speed in this patent and be controlled at 3000～5000r/min, form under the state of eddy current, in the potassium silicate of low mol ratio, drip silica hydrogel solution, make that the mol ratio of silicon-dioxide and potassium oxide reaches 5.3: 1 in the final formation clear solution, used silica hydrogel is Powdered in the reaction, need be made into 35% the aqueous solution before using.In the potassium silicate binder of this kind high molar ratio, add zinc powder or aluminum paste as rust-stabilising pigment, can be used for the antirust of metal or aluminum products.
The problem that this patent exists is that high molar ratio potassium silicate binder package stability is poor, and the zinc-rich paint viscosity of being made by this tackiness agent is low, and thick being coated with property is poor, and is strict to the surface treatment of metal substrate.
Chinese patent 99103350 has been narrated the mol ratio that adopts precipitated silica to improve silicon-dioxide and potassium oxide in the potassium silicate solution.Theoretically, the potassium silicate mol ratio that is formed by this patent is improved, but precipitated silica only is the physics dispersing and mixing as a kind of pigment in potassium silicate solution, can not participate in reaction, and the variation of essence does not take place the structure of potassium silicate.Therefore, the coating made of coating of being made by this kind high molar ratio potassium silicate and low mol ratio potassium silicate does not have great improvement.
Summary of the invention
The purpose of this invention is to provide the synthetic method of making the high molar ratio potassium silicate binder, another purpose is to use this kind tackiness agent to make the water-based anticorrosive paint composition.
The synthesis technique of high molar ratio potassium silicate binder of the present invention:
1) in reactor, adds low mol ratio potassium silicate solution, heating and control stirring velocity are at 600～1000rpm, form eddy current, dropping accounts for 50～70% water-soluble silicon colloidal sol of low mol ratio potassium silicate solution, keep swirl stabilization, in 45～70 ℃ of insulation 20～60min, up to forming transparent heavy-gravity solution;
2) drip 0.5～20% the silane coupling agent account for low mol ratio potassium silicate solution;
3) drip the stabiliser solution that accounts for low mol ratio potassium silicate solution 10～30%;
4) add the organic polymer emulsion that accounts for low mol ratio potassium silicate solution 0.5～3%;
5) add suitable quantity of water, keep 0.5～1.5h, up to reaching required solid content 24～28%, the high molar ratio potassium silicate of formation filters, packing.
Also can add 1～2% the thickener soln that accounts for low mol ratio potassium silicate solution in the above-mentioned as required synthetic method.
The water-soluble thickener that the present invention is used, optional: the methylcellulose gum that contracts, Natvosol, sodium alginate etc. are made into 0.5～2.5% the aqueous solution in advance.
The potassium silicate solution of above-mentioned low mol ratio generally is that quartz sand and sylvite are made in high temperature, reaction under high pressure.Common mol ratio is 3.3: 1, and solid content is about 45%, and viscosity is bigger, and the impurity that contains is more.The present invention needs to dilute, filter refining before use.The potassium silicate solution that will hang down mol ratio with deionized water is diluted to 30～35% solution, and through filtering, the elimination mechanical impurity becomes transparent viscous solution.
Above-mentioned water-soluble silicon colloidal sol molecular formula is H
2SiO
3, be with SiO
2Be the dispersion of fundamental unit in water, its micelle particle grain size scope is generally at 5～40nm.The present invention has strict demand to the quality of water-soluble silicon colloidal sol, and its solid content is 25～30%, and transparent, is water white.
Above-mentioned siloxanes coupling agent is the low molecule silicoorganic compound that a class has special construction, has water misciblely, also has non-water-soluble.It act as siloxanes and meets water generation hydrolysis reaction, generates the silanol base, and the effect of chain sealing is played in the high molar ratio potassium silicate reaction of hydroxyl that contains and formation.Meanwhile, the structure of silane self makes itself and metal substrate surface form chemical bond, has improved sticking power greatly.The selected silane of the present invention is water miscible, can be in methyltrimethoxy silane, Union carbide A-162, γ-An Bingjisanyiyangjiguiwan, N-β (the amino-ethyl)-silane such as γ-An Jibingjisanyiyangjiguiwan one or more.
As stabiliser solution of the present invention is alkaline, can adopt oxyhydroxide, low molecule quaternary amine alkali, ammoniacal liquor and the tertiary amine etc. of basic metal or alkaline-earth metal.Generally be made into 20～30% the aqueous solution, contain impurity in the solution, need to filter refining.The high molar ratio potassium silicate that act as of this solution provides conforming of an alkalescence, keeps the stability of solution.Otherwise the high molar ratio potassium silicate of formation will turn white, thickening in a short time, until gel.
Adding of the present invention and high molar ratio potassium silicate have the organic synthesis emulsion of consistency, improve film-forming properties, strengthen paint film adhesion and snappiness, comprise polymer emulsions such as vinylformic acid, water-base epoxy, chlorinatedpolyolefins, rubber-like.
Above-mentioned high molar ratio potassium silicate binder is called the first component, is that active substance and second component are mixed with water-based paint compositions with the first component, and the weight ratio of first component and second component is 1: 2～3.Described second component contains 80% super-fine zinc dust at least.
Can also comprise in the above-mentioned second component: color stuffings such as zinc flake, ultra-fine ferrophosphorus powder, zinc oxide, ultra-fine mica powder, talcum powder, wollastonite, improve the performance such as water-fast, anticorrosion film.
In aforementioned coating composition, also can add various auxiliary agents such as an amount of inhibiter, dispersion agent.
Described inhibiter can be the one or more combination thing of poly-phosphate, chromic salt, phosphoric acid salt, dichromate, carbonate etc.
Advantage of the present invention is owing to add water-soluble silicon colloidal sol, makes the easier and low mol ratio potassium silicate of silicon-dioxide participate in reaction, the easier control of technology.Stirring velocity generally is controlled at about 1000r/min, can reach the eddy current state, reduced because of speed too high, the easy evaporable disadvantage of moisture, energy-saving effect is remarkable; Owing to added alkaline stabiliser solution, improve the back in mol ratio and add, the package stability of high molar ratio potassium silicate is improved, prolonged work-ing life.Owing to adopt organic polymer emulsion to improve, strengthen paint film adhesion and snappiness.
The coating that the present invention makes does not contain organic solvent, nontoxic, pollution-free, after the potassium silicate binder of high molar ratio and zinc powder mix at normal temperatures, self cure forms hard filming fast, good with the sticking power of metal substrate, zinc content reaches more than 85% in the dry film, has corrosion-resistant admirably, high temperature resistant, weather-proof and shielding property.The corrosionproof protection that can be widely used in steel construction such as vehicle, boats and ships, bridge, drilling unit, coastal facility, pipeline, basin.
Embodiment
To demonstrate the present invention below, wherein per-cent all is unit with weight.
Table 1 is that to make about 600g mol ratio be 5.1～6.2: 1, solid content is five typical case's enforcements of 25～30% high molar ratio potassium silicate binder.
Table 1 high molar ratio potassium silicate binder formulation examples
| Raw material | Embodiment | ||||
| ????1 | ????2 | ????3 | ????4 | ????5 | |
| 33% low mol ratio potassium silicate g | ????300 | ????300 | ????300 | ????300 | ????300 |
| 26% silica hydrosol g | ????150 | ????188 | ????210 | ????150 | ????180 |
| Silane g | ????5 | ????5 | ????5.5 | ????6 | ????3 |
| 20% stabiliser solution g | ????58 | ????85 | ????51 | ????50 | ????45 |
| 40% organic polymer emulsion g | ????6 | ????6 | ????6 | ????5 | ????5 |
| 2% thickener soln g | ????4 | ????5 | |||
| Water g | ????62 | ????19 | ????27 | ????92 | ????80 |
| Mol ratio (SiO 2∶K 2O) | ????5.3 | ????5.2 | ????5.8 | ????5.5 | ????6.1 |
| Viscosity (being coated with-4 glasss) s | ????14.5 | ????12.4 | ????15.3 | ????11.3 | ????13.2 |
| Solid content % | ????26.0 | ????26.5 | ????27.4 | ????25.6 | ????26.2 |
| Density g/cm 3 | ????1.19 | ????1.20 | ????1.21 | ????1.18 | ????1.19 |
With the embodiment 1 of table 1 is that example explanation preparation method is as follows: the potassium silicate solution of getting the 300g mol ratio and being 3.3: 1 adds in the container, heats up, and mixing speed 700rpm produces eddy current; When temperature rises to 40 ℃, drip 150g water-soluble silicon colloidal sol at the eddy current place, adjust stirring velocity at any time, keep swirl stabilization, after dripping, formation temperature is 45～70 ℃ a transparent viscous solution; Dropwise 5 g methyltrimethoxy silane, 2min drips once, and at this moment, soltion viscosity has bigger variation, can suitably reduce stirring velocity, after methyltrimethoxy silane drips off, is incubated about 40～60min; Dropwise 5 8g potassium hydroxide stabiliser solution subsequently, stir about 20min; Drip 6g benzene emulsion and 4g sodium alginate thickener soln more respectively; Drip 62g water at last, more even for making mixing, can adjust stirring velocity to 1000rpm, insulation 20～60min filters the binder solution of final formation, packing, and its traditional performance tested.
Table 2 is typical examples of preparation water-based paint compositions.
Table 2 water-based paint compositions formulation examples
| Embodiment | ||||||
| Raw material part | ????1 | ????2 | ????3 | ????4 | ????5 | |
| High molar ratio potassium silicate binder (first component) | ????28 | ????26 | ????27 | ????30 | ????25 | |
| The second component | 325 order zinc powders | ????70 | ????65 | ????68 | ????56 | |
| 500 order zinc powders | ????4 | ????70 | ||||
| Zinc flake | ????1 | ????0.5 | ||||
| Ultra-fine ferrophosphorus powder | ????11 | |||||
| Titanium dioxide | ????2 | ????1 | ||||
| Zinc oxide | ????0.5 | |||||
| Aluminium triphosphate | ????1 | |||||
| Potassium bichromate | ????0.5 | ????0.5 | ||||
| Ultra-fine mica powder | ????0.6 | ????1.5 | ????2 | ????1.5 | ||
| Wollastonite | ????1.1 | ????0.5 | ????2 | ????0.5 | ||
| Talcum powder | ????0.3 | ????1 | ????2 | |||
| First/second (weight ratio) | ????1∶2.6 | ????1∶2.8 | ????1∶2.7 | ????1∶2.3 | ????1∶3.0 | |
Embodiment 1 with table 2 is that example explanation preparation method is as follows: the high molar ratio potassium silicate solution that takes by weighing 28 parts is made the first component, under agitation, slowly add 70 part of 325 order zinc powder in the second component successively, 0.6 part ultra-fine mica powder, 1.1 parts of wollastonites and 0.3 part of talcum powder, after adding, stir about 15～30min, stir, filter with the 40-100 mesh filter screen, on steel plate, carry out brush board or spray plate then through oil removing, sandblasting, time by standard code is carried out various Performance Detection, and its performance index are as follows:
Viscosity (efflux cup No. 6 of ISO): 〉=6s
Fineness :≤80 μ m
Solid content: 〉=75%
Density: 〉=2.9g/cm
3
The color of filming: grey
Time of drying: surface drying≤20min does solid work≤2h
Sticking power (2mm draws lattice): 1 grade
Pliability test :≤20mm
Shock-resistance: 〉=30cm
Pencil hardness: 〉=5H
Surface resistivity:＜10
7Ω
Anti-3% salt solution (1000h): no abnormal
Oil-proofness (1000h): no abnormal
Solvent resistance (1000h): no abnormal
Salt spray resistance moisture-proof heat (1000h): do not have bubble, come off, corrosion phenomena, cut place non-corroding
Moisture-proof heat (1000h): do not have bubble, come off, corrosion phenomena
Anti-artificial accelerated aging (1000h): do not have change substantially.
Claims (10)
1. the synthetic method of a high molar ratio potassium silicate binder is characterized in that, comprises the following steps:
1) in reactor, adds low mol ratio potassium silicate solution, heating and control stirring velocity are at 600～1000rpm, form eddy current, dropping accounts for 50～70% water-soluble silicon colloidal sol of low mol ratio potassium silicate solution, keep swirl stabilization, in 45～70 ℃ of insulation 20～60min, up to forming transparent heavy-gravity solution;
2) drip 0.5～20% the silane coupling agent account for low mol ratio potassium silicate solution;
3) drip the stabiliser solution that accounts for low mol ratio potassium silicate solution 10～30%;
4) add the organic polymer emulsion that accounts for low mol ratio potassium silicate solution 0.5～3%;
5) add suitable quantity of water, keep 0.5～1.5h, up to reaching required solid content 24～28%, the high molar ratio potassium silicate of formation filters, packing.
2. according to the synthetic method of the high molar ratio potassium silicate binder of claim 1, it is characterized in that, also can add 1～2% the thickener soln that accounts for low mol ratio potassium silicate solution in the synthetic method.
3. according to the synthetic method of the high molar ratio potassium silicate binder of claim 2, it is characterized in that described thickening material is selected from: the methylcellulose gum that contracts, Natvosol, sodium alginate are made into 0.5～2.5% the aqueous solution in advance.
4. according to the synthetic method of the high molar ratio potassium silicate binder of claim 1, it is characterized in that the mol ratio of described low mol ratio potassium silicate solution is 3.3: 1, solid content is 45%.
5. according to the synthetic method of the high molar ratio potassium silicate binder of claim 1, it is characterized in that, described silane coupling agent is water miscible, is selected from methyltrimethoxy silane, Union carbide A-162, γ-An Bingjisanyiyangjiguiwan, N-β (the amino-ethyl)-silane such as γ-An Jibingjisanyiyangjiguiwan one or more.
6. according to the synthetic method of the high molar ratio potassium silicate binder of claim 1, it is characterized in that described stabiliser solution is alkaline, be selected from oxyhydroxide, low molecule quaternary amine alkali, ammoniacal liquor and the tertiary amine etc. of basic metal or alkaline-earth metal.
7. according to the synthetic method of the high molar ratio potassium silicate binder of claim 1, it is characterized in that described organic polymer emulsion comprises: polymer emulsions such as vinylformic acid, water-base epoxy, chlorinatedpolyolefins, rubber-like.
8. coating composition, it is characterized in that, will be according to claim 1 synthetic high molar ratio potassium silicate binder as the first component, with the first component is that active substance and second component are mixed with water-based paint compositions, the weight ratio of first component and second component is 1: 2～3, and described second component contains 80% super-fine zinc dust at least.
9. coating composition according to Claim 8 is characterized in that, can also comprise in the described second component: zinc flake, ultra-fine ferrophosphorus powder, zinc oxide, ultra-fine mica powder, talcum powder, wollastonite.
10. coating composition according to Claim 8 is characterized in that, also can add an amount of inhibiter in coating composition.
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| CN1297614C (en) * | 2004-03-30 | 2007-01-31 | 赵力 | Method for preparing high modulus potassium metasilicate solution for coating |
| CN100406531C (en) * | 2005-09-16 | 2008-07-30 | 湖南华迪电力环保工程技术有限公司 | Anticorrosive flue paint |
| CN101121856B (en) * | 2007-09-14 | 2011-01-19 | 合肥华清金属表面处理有限责任公司 | Heat-proof corrosion-resistant coating used for automobile exhaust tube |
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| CN1297614C (en) * | 2004-03-30 | 2007-01-31 | 赵力 | Method for preparing high modulus potassium metasilicate solution for coating |
| CN100406531C (en) * | 2005-09-16 | 2008-07-30 | 湖南华迪电力环保工程技术有限公司 | Anticorrosive flue paint |
| CN101121856B (en) * | 2007-09-14 | 2011-01-19 | 合肥华清金属表面处理有限责任公司 | Heat-proof corrosion-resistant coating used for automobile exhaust tube |
| CN102503344A (en) * | 2011-10-20 | 2012-06-20 | 北京市农林科学院 | Antiseepage material and preparation method thereof |
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| CN108148510A (en) * | 2017-12-28 | 2018-06-12 | 苏州科技大学 | A kind of normal temperature self-drying type inorganic nano material adhesive |
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