Priming coat for steel

FIELD: protective materials.

SUBSTANCE: invention relates to a method for preparing priming coat for steel that is designated for assembly and applying upper coat. Steel in grounded with priming coat comprising a silicon dioxide-base binding substance containing silicon dioxide aqueous sol stabilized with aluminum oxide and, optionally, small amount of alkaline metal silicate. Indicated binding agent shows the mole ratio SiO2/M2O = at least 6:1 wherein M means the total amount of alkaline metal ions and ammonium ions. After drying the priming coat up to disappearance of stickiness in weal touch by a finger it is treated optionally with a solution that enhances the strength of the priming coat film.

EFFECT: improved and valuable properties of coat.

12 cl, 7 tbl, 21 ex

 

The present invention relates to a method of applying a primer coating to steel. In particular, the invention relates to the coating on the semi-finished steel products, which then have to be assembled using processes with intensive heat treatment and covered with a protective coating. Such semi-finished steel products can be used in the shipbuilding industry and for other large-scale structures such as oil platforms, and these include steel sheets, for example, a thickness of 6 to 75 mm, beams, spars, and various steel sections used as rigid walls. The most important process with intensive heat treatment is welding; almost all such semi-finished steel products are welding. Other important processes with intensive heat treatment are cutting, such as flame cutting, plasma cutting or laser cutting, and thermal shaping, when the steel is bent into shape when heated. These steel products are often exposed to the atmosphere during storage prior to Assembly and during Assembly, and they are usually covered with a coating called "priming coating of metal prefabricated or pre-installation primer coating to prevent corrosion of steel having places which before as all steel construction, such as a ship, will be coated with anti-rust paint, resulting in no problem applying a protective coating or the removal of corrosion products of steel. Most shipyards applying primer metal semi-finished product is as one of several treatments carried out on the production line, on which steel, for example, pre-heated, subjected to blasting or blasting to remove scale and corrosion products, put the first coat of metal semi-finished and passed through the drying chamber. In another embodiment, a primer coating of metal semi-finished product can be applied industrial machine for coating or steel supplier until delivery to the shipyard or other Assembly area.

Although the main function of the primer metal semi-finished product is to create a temporary corrosion protection during Assembly, shipbuilders prefer that it was not necessary to remove the primer metal semi-finished product, and you could leave it on steel during Assembly and after Assembly. Thus, steel, primer coated metal semi-finished product, must be able to weld without removing the primer metal semi-finished product and should enable causes the any type of protective anti-corrosion coatings, typically used on vessels and other steel structures, with good adhesion between the primer and then applied coating. Primer metal semi-finished product preferably should have the ability to weld without any negative impact on the quality of welding or the speed of the welding process and should have sufficient heat resistance to the primer metal semi-finished product has maintained its anti-corrosion properties in areas heated when cutting or welding on the opposite surface of the steel.

With the commercial success of primers metal-semi-finished products which are available today, are applied from a solvent of the coating based on prehydrolyzed tetraethylorthosilicate binders and zinc powder. These coatings contain large amounts of volatile organic solvent, usually about 650 grams per liter to stabilize the coloring binder and be able to apply the product in the form of a thin film, typically of a thickness of approximately 20 microns. Removing the volatile organic solvent can be dangerous to the environment and in many countries is regulated by laws. There is a need to be primed metal semi-finished product, which does not emit or emit much less volatile organic process is Italia. Examples of such coatings are coatings that are described in the publications US-A-4888056 and JP-A-7-70476.

Publication JP-A-6-200188 refers to the primers of the metal, semi-finished and mentions the possibility of using water-binder type binder based on water alkaline silicate salt. Coatings containing aqueous alkali metal silicate and powdered zinc, also proposed in the publication GB-A-1226360, GB-A-1007481, GB-A-997094, US-A-4230496 and JP-A-55-106271. Binders based on alkali silicate for anticorrosive coatings also mentioned in the publication US-A-3522066, US-A-3620784, US-A-4162169 and US-A-479824. In the publication EP-A-295834 mentioned coating containing a mixture of alkali metal silicate with a small amount of colloidal silicon dioxide powder Al2O3as filler and metal powder as a hardening agent. In the publication US-A-3721574 proposed coating containing a mixture of alkali metal silicate with a small amount of colloidal silicon dioxide, preferably modified Al2O3and zinc powder. Applicants found that a primer coating based on an aqueous alkaline silicate binders can provide adequate protection against corrosion and allow you to expose welding covered with them the steel surface, but create problems when grease is on top of the coating. Water silicates contain large amounts of alkali metal cations, which are necessary to keep the silicate in aqueous solution, and these ions are still present in the coating after it dries. Applicants have found that if a primer coating containing such large amounts of ions of an alkali metal cover on top of any conventional organic coating and then immersed in water, the formation of bubbles (local delamination of the coating). Conducted tests that showed that this problem can be reduced if the coating is exposed to the atmosphere shortly after priming of the metal, semi-finished or washed before applying the top coating. However, these processes are not compatible with use in modern high performance shipbuilding.

Aqueous sols of silicic acid having a very low content of alkali metal ions, are commercially available, but coverage on the basis of such sols are usually very bad (initial) the strength of the film from the viewpoint of adhesion, cohesion, hardness and resistance to abrasion and resistance in the water. Such poor physical properties of the coating makes it susceptible to damage during work or during subsequent processing. Because of this potentially is the need to restore coverage with high costs. The proposed improvements coatings based on Sol of silicon dioxide is described in the publication US-A-332082 in which add is not miscible with water, an organic amine, in the publication GB-A-1541022, which is added to the water-soluble acrylamide polymer in the publication GB-A-1485169, which is added to the silicate Quaternary ammonium or alkaline metal, and in the publication of JP 55100921, which add materials such as clays and/or oxides of metals such as Al2O3and the phosphate and/or ethyl silicate of aluminum. However, such coatings do not reach physical properties similar to the physical properties of coatings based on alkali metal silicates. Coatings on the basis of colloidal solution of silicon dioxide has a low level of education of bubbles when applying the top coating/dip. Although the content of soluble salts and osmotic pressure are low, the bubbles may still occur, since the coating has a very low resistance to the beginning of/the development of education due to their poor physical properties.

There is a need in the aqueous primer metal semi-finished product with a low content of alkali metal ions, which has improved adhesion to the base and superior film strength in the light of the properties discussed above, in order to resist the initiation and development of the bubble.

<> In addition, there is a need for not forming bubbles aqueous primer for metal semi-finished product, which demonstrates the rapid manifestation of the physical properties of the coating after application of the primer metal semi-finished product, to ensure that the subsequent processing basics without the risk of damaging the floor.

Also of importance is the shelf life of the composition. To expand the possibilities of application of such coatings, the shelf life should be as long as possible.

The method according to the present invention to obtain a primer coating steel, which is designed for the Assembly and application of the top coating, offers a solution to the aforementioned problems and disadvantages. The method in accordance with the present invention for priming steel with a primer coating containing a binder on the basis of silicon dioxide, characterized in that the binder contains stabilized aluminum oxide aqueous Sol of silicon dioxide, and optionally a small amount of alkali metal silicate, and the specified binding substance has a molar ratio of SiO2/M2O, where M represents the total number of ions of the alkali metal and ammonium ions, of at least 6:1, and where after the primer coating has dried to the disappearance of stickiness when SLA is the first touch of fingers, it is not necessarily treated with a solution that increases the strength of the film.

The present invention also relates to a primer coating used in this way.

For the purposes of the present invention increases the strength of the film solution is a solution that increases the strength of the film primer coating and/or accelerates the manifestation of the strength of the film in time.

In this application, the concentration of aluminum oxide in the cover composition is indicated in% Al2O3by weight based on particle Sol of silicon dioxide or silicate in the composition.

The binder in the most preferred is a binder based on water Zola silicon dioxide. Such sols are delivered by the company Akzo Nobel under the registered trade name "Bindzil or by DuPont under the registered trade name "Ludox", although in the literature related to them, it is emphasized that conventional varieties of colloidal silicon dioxide are not a good film-forming agents. Available in various grades Zola having different particle size of colloidal silicon dioxide and containing various stabilizers. The particle size of colloidal silicon dioxide, for example, may be in the range from 3 to 100 nm; particle size closer to the lower bound of the range, for example, from 5 to 2, is preferred. The preferred particle size is in the range from 3 to 15 nm, even more preferably between 3 and 10 nm. The Sol of silicon dioxide preferably has a molar ratio of SiO2/M2O at least 25:1, more preferably at least 50:1, and may have a molar ratio of SiO2/M2O 200:1 or more. In addition, you can use a mixture of two or more colloidal solution of silicon dioxide having different molar ratio of SiO2/M2O, where the molar ratio of SiO2/M2O the mixture is at least 25:1. M represents the total number of ions of the alkali metal and ammonium, where M can represent, for example, Na, K, Li, etc. Sol can be stabilized with alkali, e.g. sodium hydroxide, potassium or lithium, or Quaternary ammonium hydroxide, or by using a water-soluble organic amine, such as alkanolamine. The coating composition preferably should practically not contain any stable ammonium Zola silicon dioxide, as the presence of stable ammonium Zola may cause gelatinization of the composition, particularly when the binder consists of predominantly stabilized ammonium Zola silicon oxide, and the coating composition also includes a powder qi is CA.

To improve shelf life covering composition comprises a stabilized alumina Sol. For the purposes of the present invention, the shelf life is defined as 50%degradation of the coating film when tested within 1 hour after application.

For optimum properties, preference is given to using modified alumina sols of silica, for example, Zola silicon dioxide, modified 0.05 to 2.0 wt.% aluminum oxide. In such sols, which are also called surface-modified Al-colloidal solution of silicon dioxide, the surface of the particles modify sodium aluminate associated with particles.

To obtain surface-modified Al Sol of silicon dioxide, the surface of the particles or Sol of silicon dioxide can be modified alumina using the method described R.K.Iler, The Chemistry of Silica (John Wiley and Sons, 1979), 407-409.

The surface of the particles or Sol of silica used in the examples of this application, modified as follows. A number Zola silica with pH ˜10 were maionizirebeli by passing through a strong cation exchange column. Received deionized Sol had a pH of ˜2. Three massive part of this deionized Sol with pH ˜2 were added to the two mass parts nedenominirovannyh Zola silicon dioxide is from pH ˜ 10 and intensively stirred. The resulting mixture had a pH value of 7.5-8. Then 30 minutes after mixing it with vigorous stirring was added approximately 1 mass part of sodium aluminate solution (10 wt.% in deionized water). Adding aluminate led to an increase in the pH of the mixture to the ˜10. Qualified in this field specialist other known methods of obtaining modified aluminum oxide Sol of silicon dioxide.

The optimal concentration of aluminum oxide in the composition is balanced between the expiration date and coating properties. Higher levels of aluminum oxide result in a longer shelf-life, but can also lead to a reduction in the rate of manifestation of the properties of the coating.

The Sol of silicon dioxide may be mixed with a small amount of alkali metal silicate, for example, lithium silicate, sodium silicate is lithium or potassium silicate, or with Quaternary ammonium silicate. Other examples of suitable mixtures of Sol-silicate can be found in the publication US 4902442. Adding a silicate of an alkali metal or ammonium can improve the characteristics of the initial film-forming Sol of silicon dioxide, but the amount of alkali metal silicate should be low enough to have a molar ratio of SiO2/M2O binder Zola, what about the least 6:1, preferably at least 8:1, and most preferably at least more than 15:1. In the case of the present invention a small amount of alkali metal silicate means that the mass ratio of the alkali metal silicate to solo silicon dioxide in the composition is less than 0.5, preferably less than 0.25, more preferably less than 0.1.

The Sol of silicon dioxide alternative or additionally may contain dissolved or dispergirovannoyj organic resin. The organic resin is preferably a latex, for example a latex of butadiene-styrene copolymer, latex of styrene-acrylic copolymer latex, a vinyl acetate-ethylene copolymer dispersion polyvinyl butyral, silicone/siloxane dispersion or dispersion of acrylic latex. Examples of suitable latex dispersions, which can be used are XZ94770 and XZ94755 (both Dow Chemicals), Airflex® 500, Airflex® EP3333 DEV, Airflex® CEF 52 and Flexcryl® SAF34 (all Air Products), Primal® E-330DF and Primal® MV23LO (both Rohm and Haas), and Silres® MP42 E, Silres® M50E and SLM 43164 (all Wacker Chemicals). Water-soluble polymers, such as acrylamide polymers, can be used but are less preferred. Organic resins are preferably used in an amount up to 35 wt.% based on solid binder. In the case of compositions is s, containing binder with particles of colloidal silica with an average particle size equal to or below 10 nm, the organic resin is preferably used in an amount up to 20 wt.%, more preferably in the amount of 1-15 wt.% based on solid binder. In the case of compositions containing the binder with the particles of colloidal silica with an average particle size of more than 10 nm, for example between 12 and 22 nm, or between 12 and 16 nm, it is preferable to use an increased amount of an organic resin to 35 wt.% based on solid binder. Higher amounts of organic resin can lead to porosity of the weld during subsequent welding. It was shown that addition of an organic resin improves the adhesion/cohesion, which is measured by the method of cross-hatch test.

Alternatively, a Sol of silicon dioxide may contain silane bonding agents, which contain alkoxysilane group and the organic residue containing functional group such as amino, epoxy or isocyanate group. Silane binding agent preferably is aminosilane, such as gamma aminopropyltriethoxysilane or gamma aminopropyltrimethoxysilane, or a partial hydrolyzate, although epoxysilane, such as gamma glycidoxypropyltrimethoxysilane can also be used. Silane binding agent preferably is present in an amount up to 30 wt.%, for example, 1-20 wt.%, based on silicon dioxide.

The binder in the primer coating may alternatively or additionally contain an aqueous solution of a silicate of an alkali metal or ammonium, stable siliconates, substituted, at least one anionic group with a lower pKa value than the pKa of silicic acid, such as carboxylate or sulphonate group. Such binders are preferably a solution having a molar ratio of SiO2/M2About in the range from 8:1 to 30:1 and the pH value in the range from 7 to 10.5, prepared by lowering the pH of a solution of silicate and siliconate cationic exchange. Therefore, siliconate can be added in relatively low quantities, for example, at a molar ratio of from 1:2 to 1:20, to the alkali metal silicate with the usual ratio of SiO2/K2About a 3.9:1. Then the amount of solid components can be reduced, in order to facilitate the processing and further improve the stability. At this stage, the solution has a pH of 12-12 .5. The solution is subjected to ion exchange using standard ion-exchange resin. Ions To+replace ions of N+by reducing the content of alkali binder and pH. In the absence of silico the ATA silicate would gel with decreasing pH. Were obtained transparent, stable, stable solutions with a pH up to, but not below 8. The obtained binder typically has a molar ratio of SiO2/K2About in the range of 8-20:1 and can be concentrated, if desired, to increase the solids content. The binder is a clear, stable solution and is stable in the presence of zinc, but the coating on the basis of such subjected to ion exchange binders have relatively poor strength of the film in comparison with coatings based on alkali silicate binders.

Preferably used binder having a pH value in the range from 9 to 11.5, more preferably in the range from 9.5 to 11. Without claim to any particular theory to explain the effect of pH on the properties of the film, it seems that the increase of pH leads to an increase in the amount of soluble silica in solution. This, apparently, has the ability to affect the hardening of the gel in situ after application of the coating composition. In addition, the regulation of pH may be due to the increase shelf life. When the obtained commercial by Zola silicon dioxide can be selected Sol with a high pH value and/or the pH value Zola can be adjusted. The pH value can be skorrektiroval is about, for example, by changing the number of Al2O3or adding affecting the pH of the agent that increases the shelf life, such as dimethylaminoethanol (DMAE), or by adding dilute sulfuric acid, or by adding sodium hydroxide.

For example, commercially available 22 nm sols of silica typically have a pH of from about 8.5 to 9. Raising the pH interval of such sols to 10-11 significantly improves the speed of manifestation of the properties of the coating.

Primer coating preferably contains zinc powder and/or a zinc alloy. Such zinc powder preferably has a volumetric average particle size from 2 to 12 microns, and most preferably such zinc powder is a product sold by the industry as zinc dust having an average particle size of from 2 to 8 microns. Zinc powder protects the steel by galvanic mechanism and can also form a protective layer of corrosion products of zinc, which increases corrosion protection coating. All or part of the zinc powder may be replaced by zinc alloy. The amount of zinc powder and/or alloy in the coating is typically at least 10% and can reach up to 90% vol. coatings based on the dry film. Powder zinc and/or alloy essentially can be completely personalize the pig is the orientations of the coating, or may, for example, up to 70%, for example, from 25 to 55% vol. coatings based on the dry film, and the coating also contains an additional corrosion inhibitor, which may, for example, be a molybdate, phosphate, tungstate or Vanadate, described in the publication US-A-5246488, ultrasonically titanium dioxide described in the publication KR 8101300, and/or zinc oxide, and/or a filler such as silicon dioxide, calcined clay, aluminum silicate, talc, barites, mica, magnesium silicate or calcined aluminosilicate.

In the case of compositions containing the binder with the particles of colloidal silica with an average particle size equal to or below 10 nm, the amount of powder of zinc and/or alloy in the coating ranges from 40 to 60%, preferably between 45 and 55% vol. coatings based on the dry film. In the case of compositions containing the binder with the particles of colloidal silica with an average particle size above 10 nm, for example between 12 and 22 nm, or between 12 and 16 nm, the amount of powder of zinc and/or alloy in the coating is between 35 and 50%.

However, in combination with pigments based on zinc can be used by other pigments. Examples of other non zinc pigments are conductive fillers, such as phosphide di-iron (Ferrophos®), micaceous iron oxide, and others. The use of such conductive n is zinc pigments can reduce the content of zinc, while maintaining effective corrosion protection. To obtain the optimum properties of the coating, fillers preferably effectively dispersed in the coating composition. Types and sizes used diluents can be selected to obtain the appropriate state of dispersion. For example, when you choose pigment filler Satintone (Lawrence Industries)should be used, the average particle size below 3 μm, preferably below 2 microns.

Preferably the volume concentration of the pigment (GST) in the coating is between 40 and 75%. The concentration of more than 75% of the film characteristics deteriorate, but at a concentration below 40% of the zinc is not enough to ensure effective corrosion protection. In the case of compositions containing the binder with the particles of colloidal silica with an average particle size of below 10 nm, the GST is preferably between 55 and 75%, more preferably between 65 and 75%. In the case of compositions containing the binder with the particles of colloidal silica with an average particle size equal to or more than 10 nm, can be obtained improved initial properties of the coating when using the GST between 40 and 65%, more preferably between 45 and 55%.

The volume concentration of the pigment (GST) is a volumetric percentage of pigment in the dry paint film. Critical about the roadways to the concentration of pigment (KRCS) is usually defined as the volume concentration of the pigment, in which the binder is present in a quantity just sufficient to create fully absorbed in the layer of binder on the surfaces of the pigment and filling in all the gaps between the particles are tightly Packed system. The critical volume concentration of the pigment can be determined by wetting the dry pigment with quantity of linseed oil, just enough to form coherent (solid) mass. This method gives a value known as the "oil absorption", from which calculate the critical volume concentration of pigment. The method of determining the oil absorption is described in British Standard 3483 (BS3483).

The solids content in the primer coating is typically at least 15 vol.% and preferably is in the range from 20 to 35 vol.%. Volumetric content of solid components is a theoretical value calculated on the basis of all components present in the coating composition. The coating usually has such a viscosity that it could be easily applied in the usual devices for coating, such as spraying, particularly airless spray or high-volume spray low pressure device (WAND) with a coating having a dry film thickness less than 40 microns, predpochtitel is but between 12 and 25 to 30 microns.

Optionally, the coating composition may contain additional additives, well known qualified in this field specialists, for example, thixotropic agents and/or agents that regulate the rheological properties (organic clay, xanthan gum, cellulose thickeners, preferredability, acrylic compounds, and others), defoamers (especially when there are latex modifiers) and, optionally, secondary prolonging the shelf life of fillers such as chromates (e.g., sodium dichromate) or tertiary amines (e.g. triethylamine or dimethylaminoethanol). Preferred thixotropic and/or regulate the rheological properties of the agents are Bentonite EW (company Elementis), which is a silicate of magnesium, sodium (organic clay), Bentonite WH (firm Rockwood), which is a water-silicate, Laponite RD (Rockwood), which is an aqueous silicate of magnesium, lithium, sodium, and Rheolate 425 (Elementis), which is a patented acrylic suspension in water. Preferred defoamers are Foamaster NDW (Cognis) and Dapro 1760 (Elementis). Found that other compounds that may be present in the composition for other purposes, can also act as secondary agents that increase shelf life. For example, adding anticorrosion the frame pigment Molywhite or styrene-butadiene latex may result in a slight lengthening shelf life. Preferred secondary increase shelf life extenders are tertiary amines, which provide increased shelf life without chromates. Usually covering the system is available in the form of two (or more) component system when the components are thoroughly mixed prior to coating.

Upon receipt of a composition with a suitable shelf-life speed manifestations of the properties of the film depends on how subsequently turn coated with a covering layer.

To achieve a rapid effect of the floor covering can then be processed increases the strength of the film solution. In this method before processing solution that increases the strength of the film, the primer coating is dried prior to the disappearance of stickiness with a weak touch of a finger.

The manifestation of the properties of the coating can also be accelerated by immersing the coated base in water or keeping in an atmosphere with a relative humidity of at least 50%, preferably at least 80%. This method may further include processing increases the strength of the film solution. This method is the subject of a separate patent publication.

When the speed of drying is not a problem, we can give is not subjected to post-processing the coating to dry at a relative humidity is, for example, between 25 and 50%. The development properties of the coating will occur more slowly, but, in the end, will be the good properties of the coating.

The time of the disappearance of stickiness with a weak finger contact is usually from about 10 to 15 minutes at ordinary temperatures from 15 to 20°or 3 to 4 min at 40°to cover with a dry film thickness (tsp) 15-20 μm. The drying time also depends on air flow and film thickness. At 35°and the air flow of 0.5 m/s drying time of a coating with a dry film thickness of 20 μm is approximately 2 minutes This time can be further reduced by increasing the temperature.

In General, the drying time can be reduced by increasing the temperature of the basics, increasing air temperature, air flow, or by any combination of these methods.

It is preferable to carry out drying of the primer coating at 10-60°C, preferably at 25-50°With forced air flow, preferably in a stream of air at least 0.1 m/s, especially if the application of a primer coating, drying and the application of optional increase the strength of the solution carried out on the production line. Achieving rapid drying is a very important condition of the coating on the production line at Sudostroitelny the x factories and steel mills.

The coating solution for processing before drying primer to the state of disappearance sticky when touched with a finger does not increase the film strength.

The solution, which increases the strength of the film primer coating is typically an aqueous solution of an inorganic salt or a solution of a material containing reactive silicon-containing group. Improving the film strength can be determined by a significant increase in hardness, abrasion resistance and usually adhesion. Hardness can be measured using the method of determining the pencil hardness scale (British Standard 3900, part E19 (1999) (pencil hardness required for deflection)). Abrasion resistance can be measured using the dual abrasion, in which the coating automatically rubs and which can be carried out dry or wetted with water. Although a significant increase in resistance to abrasion either a dry or wet already could be considered as increasing the strength of the film primer coating, it was found that processing in accordance with the invention improves the abrasion resistance of both dry and wet condition. Adhesion can be measured by the method of cross-hatch test, which is described in British Standard 3900 part E6 (1992).

The number increases strongly the th film solution applied to the primer coating, is typically in the range of 0.005 to 0.2, preferably from 0.01 to 0.08 liters per square meter of the surface of the primer coating (l/m2in the case of coating applied at the standard dry film thickness (15-20 μm). This amount of solution can usually be applied by spraying. Needless to say, the concentration or the volume of solution for further processing must be improved if the coating is applied in larger quantities, for example, when the dry film thickness >20 μm.

Previously as a post-processing for conciliating coatings based binder containing a silicate of an alkali metal, proposed leaching, but this method involves applying a large amount of water for leaching of salts of the alkali metal of the coating, with SiO2/M2Of from about 3:1 to 4:1. Spraying the equivalent amount of water by itself or deletion primer through a steam chamber on the production line at normal line speeds (that is, the exposure time is <2 min) does not lead to a significant increase in film strength.

Without pretending to any theory to explain the increase in film strength, I believe that, when the solution treatment is an aqueous solution of inorganic salt, or places the dissolution and re-deposition of silicon dioxide, or salts act as a hardening agent between the particles Zola. When the solution to handle contains reactive particles of silicon dioxide, they can be deposited between the particles of the Sol of silicon dioxide, improving their binding. Applicants have found that the same hardening materials when added to the primer composition of the coating during application or after application to the base does not increase the strength of the formed film primer coating.

When optional damage increases the strength of the film solution is an aqueous solution of inorganic salt, then he usually has a concentration of at least 0.01 M, and preferably at least of 0.03 M solution Concentration of inorganic salts can be up to 0.5 M or 1 M or even more. The inorganic salt may be a salt of monovalent cation, such as a salt of an alkali metal or ammonium, divalent cation, such as zinc, magnesium, calcium, copper (II) or iron (II), trivalent cations such as aluminum or cerium (III), or tetravalent cation, such as cerium (IV), and monovalent anion such as a halide, such as fluoride, chloride or bromide, or nitrate, or polyvalent anion, such as sulfate or phosphate. Can also be used mixtures of the above salts. what reamers solutions of inorganic salts, which was found effective are the solutions of magnesium sulfate, zinc sulfate, potassium sulfate, aluminum sulfate, iron sulfate, sulfate, cerium (IV), copper sulfate, sodium chloride and potassium chloride, although chlorides may not be preferred due to their ability to accelerate the corrosion process. The weight concentration of the solution of the inorganic salt is preferably in the range of 0.5-20 wt.%.

One of the examples of the material containing the active silicon-containing group, is a silicate. Increasing the film strength of the solution may be a solution of alkali metal silicate such as potassium silicate or lithium silicate, or a solution of ammonium silicate, or it can be siliconed alkali metal, for example a solution of alkylsilane. The preferred concentration of such a solution is in the range of 0.5-20 wt.%.

When optional damage increases the strength of the film solution is a solution of inorganic salts or alkali metal silicate added material will increase the salt content of the silicate of zinc in the primer coating. This will lead to an increase in osmotic driving force, when the coating is applied to the upper floor and, consequently, the probability of osmotic blistering when immersed covered the basics. The number is the primary objective of the applied inorganic salts or alkali metal silicate preferably is sufficiently low, so that the molar ratio of SiO2/M2O binder primer coating remained above 6:1, preferably more than 8:1 and most preferably more than 10:1. To achieve this result, the number of the applied inorganic salt or silicate of an alkali metal to increase the strength of the solution is preferably less than 10 g/m2based on dry weight, most preferably less than 5 g/m2in the case of a coating with a dry film thickness of 15-20 μm.

An alternative example of a material containing reactive silicon-containing group is an alkoxysilane or alloccasion, such as acetoxysilane. For example, it may be tetraalkoxysilane (alkalitolerant), such as tetraethoxysilane or tetraisopropoxide, or tralkoxydim, such as methyltrimethoxysilane (RTMS, Aldrich) or bistrimethylammonium. The alkoxysilane may contain additional functional groups, for example, tralkoxydim can have the formula RSi(OR1)3where each group R1is a 1-3C-alkyl, and R represents an alkyl or aryl group, substituted amino, alkylamino, dialkylamino group, amide group, halogen atom, urethane, epoxy, isocyanate, aziridine, sulphonate, carboxylate, phosphate or hydroxyl the Oh group. Preferred examples are aminosilane, such as triethoxysilylpropyl (Aminosilane A1100, Witco), triethoxysilylpropyl (Aminosilane A1110, Witco), trimethoxypropylsilane (Aminosilane A1120, Witco), trimethoxypropylsilane (Aminosilane A1130, Witco) or bactrimisotretinoin. In addition, the alkoxysilane may be a bis(tralkoxydim), for example, alkylene or polydimethylsilane chain, closed groups-SiOR'3. The alkoxysilane may be at least partially hydrolyzed, for example, can be used partially hydrolyzed tetraalkoxysilane or hydrolyzed allyltriethoxysilane or aminoalkylsilanes. The alkoxysilane is preferably applied from aqueous solution, although the aqueous solution may contain dissolved in water, an organic solvent, for example an alcohol, such as ethanol.

In addition, it was found that orthosilicate in this way are also very effective reinforcing properties of agents. Aqueous solutions of tetraethylorthosilicate (TMOS) and tetraethylorthosilicate (TEOS) are effective agents for further processing. The best results are obtained if TMOS or TEOS thrown hydrolysis at pH 1-2. At this pH value the shelf life of the solutions for the subsequent processing may exceed 7 days.

To ncentrate alkoxysilane or orthosilicates in optional caused by solution treatment is preferably in the range of 1-25 wt.%.

Using alkoxysilanes and/or orthosilicates in optional caused the solution to handle is the preferred because these compounds contribute to the priming of metal prefabricated actually zero amount of water-soluble salts.

Optional coating solution for processing, and also, preferably, drying the treated primer coating to the disappearance of the stickiness of the coating at a weak touch of a finger, can be carried out on the production line after applying a primer coating of steel and drying of this coating to the disappearance of the stickiness of the coating at a weak touch of a finger. The amount used is not necessarily caused to increase the film strength of the solution is preferably 0.005 to 0.2 l/m2the surface of the primer coating, most preferably of 0.08 l/m2or less, if the coating process and dried in the operating mode on the line for coatings with a dry film thickness of 15-20 μm. The drying time of the coating, treated in this number increases the film strength of the solution is usually from about 5 to 10 minutes at 15-20°From or from about 1.5 to 2 minutes at 40°C. the drying Time can also be reduced by making the primed base in the air flow.

In General, the drying time can be reduced is but due to the temperature increase of the base, increasing air temperature, air flow, or by any combination thereof.

Optional stacking solution for treatment is preferably applied and dried at a temperature in the range of 10-60°C, preferably 25-50°With forced air flow, preferably in a stream of air at least 0.1 m/s Solution for processing can be applied using standard spray equipment for airless spray or high-volume spray at low pressure, or by using atomized spray through the easy installation of the second dispenser further along the line of the primer metal semi-finished product after spray gun for applying primer. Alternatively, the solution may be applied using the technology of aerosol deposition. The solution treatment can be applied on both sides of the base, for example, on both sides of the steel sheet for use in shipbuilding, regardless of the orientation of the base; the volume of solution required to increase the strength of the film is such that the solution can be deposited on the underside of the leaf without draining or scapania. Other methods of application, such as application roller, it is also possible, but not preferred. Processed primer coating should only be allowed to dry on the basics and there is no need for any subsequent washing or heating; once processed, the primer dries, with the covered product, you can work in the usual way.

This optional method of treatment increases the hardness, cohesion and abrasion resistance of the primer metal semi-finished product without making such drawback as the formation of bubbles when applying the top coating. Furthermore, the method speeds up the manifestation of such positive characteristics. This manifestation can be even faster when treated with a solution that increases the strength of the film. Accelerated manifestation of such properties improves resistance to damage during handling and Assembly in shipbuilding or steel mills. In addition to these positive effects primed basis has the characteristics required in the market of metal primers intermediate product, namely, corrosion resistance 6 months when exposed to open air, the beautiful characteristics of the welding/cutting and the ability to application of the top coating using a wide range of primer coating without the formation of bubbles or notevoli.

For example, when the coating based on Sol of silicon dioxide filled with zinc, optionally treated with a solution that increases the strength of the film, the resistance of the dry abrasion 10 minutes after the coating is increased at least five-RA is, while the resistance wet abrasion resistance usually increases 10 times or more. The pencil hardness scale usually varies from 2M to T or more. The molar ratio of SiO2/M2About the primer coating can, for example, be lowered from 50-200 to 15-35, if increasing the strength of the film solution is a solution of inorganic salt or a solution of alkali metal silicate, but during normal dry film thickness of 15-20 μm in the case of primer coatings for metal semifinished product, it still remains above the level at which there is a significant formation of bubbles. The molar ratio of SiO2/M2About can be stored even at a higher level, if increasing the strength of the solution is a solution of alkoxysilane. Processed primer coating can be covered with a top coating on the basis of utverzhdenii an amine epoxy resin or any other coating for severe operating conditions, such as polyurethane coating, when the film thickness of 100 to 200 μm, and after keeping for curing for 7 days basis may be immersed in pure and sea water for 6 months (the longest period tested to date) at 40°without the formation of bubbles.

The invention is also explained using the following examples. The examples are intended to Illustra the AI of the invention and are in no way intended to limit its scope.

Determination of the particle size of the colloidal solution of silicon dioxide used in the examples, carry out titration method, which is described in the publication G.W.Sears, Anal. Chem., 12, 1981 (1956). Using this method can be defined as the specific surface area in square meters per gram. For spherical particles Zola surface area is transferred to the particle size.

The mass percentage of aluminum oxide modified with aluminum oxide sols of silica used in the examples was determined by x-ray fluorescence spectroscopy.

Used in these examples, the source compounds have the following origins:

Ludox® SM Sol of silicon dioxide with a concentration of 30 wt.%, the average particle size of 7 nm, the molar ratio of SiO2/Na2O 50:1, DuPont, pH of 10.3

Bindzil® AT/360 modified alumina Sol of silicon dioxide with a concentration 22-27 wt.%, the average particle size of 7 nm, the molar ratio of SiO2/Na2O 50:1, Akzo Nobel (Eka Chemicals), pH of 9.8-10

Nyacol colloidal solution of silicon dioxide with a concentration of 40 wt.%, the average particle size 16 nm, the molar ratio of SiO2/Na2O 105:1, Akzo Nobel (Eka Chemicals), pH of 9.8

Nyacol Al modified aluminum oxide option Nyacol, pH of 9.9

XZ 94770 organic styrene/butadiene latex with 50 vol.% solids, Dow Chemicals

Huber 90C calcined aluminosilicate pigment of napolnitel is with an average particle size of 0.7 μm, JM Huber/Marlow Chemicals

Zinc dust metal powder with an average particle size of 7 μm, Trident Alloys

Molywhite 212 mixed molybdate calcium and zinc, anti-corrosive pigment with a particle size of 4.1 μm, Sherwin Williams

Minex 20 sodium potassium aluminosilicate pigment filler with an average particle size 2,95 μm, North Cape Minerals

Bentone EW thixotropic silicate of sodium-magnesium, Elementis.

Examples 1-5

To assess the impact of the content of aluminum oxide on the shelf life primer metal intermediate product prepared several compositions with a concentration of solids 28 vol.%. Primer coating has a volume concentration of pigment 71,0%, which is 1.4 times higher than the critical volume concentration of pigment.

Used in example 1, a composition is prepared from the following ingredients.

Componentwt.%
The Sol of silicon dioxide30,6
Water13,5
Bentonite thixotropic clay0,2
Zinc dust48,2
Huber 90C7,5

For examples 2 through 5 composition is prepared from the following ingredients.

Componentwt.%
Sol diox is Yes silicon 36,0
Water8,1
Bentonite thixotropic clay0,2
Zinc dust48,2
Huber 90C7,5

The primer is prepared by mixing a Sol of silicon dioxide with water and a thixotropic agent, and the resulting binder is mixed with pigments before applying to the steel, as it usually takes place in the case conciliate coatings. The obtained primer coating applied to the steel panel size 15 cm × 10 cm with a dry film thickness of 15-20 μm at 35°C and relative humidity of 30%. The primer coating is dried at room conditions (20°, OB 60%).

Shelf life is the time after mixing of all components, when, after coating, see the deterioration of coating properties after 1 hour after application. In these tests it was determined 50%deterioration of coating properties after 1 hour after application to show that its validity period has increased.

Table 1
Example No.The Sol of silicon dioxidewt.% aluminium oxideShelf life
11Ludox SM-30-60 min
2Bindzil 25AT/3600,274-6 hour
3Bindzil 25AT/3600,3924-48 hour
4Bindzil 25AT/3600,49>48 hours
5Bindzil 25AT/3600,69>60 hours
1Comparative example

Examples 6-9

Prepare the primer composition of the coating metal semifinished product of examples 1, 2, 3 and 4. Through of 0.5, 1.5, 4, 6 and/or 24 h after mixing components of the composition are applied to the steel panel size 15 cm × 10 cm with a dry film thickness of 15-20 μm at 35°C and relative humidity of 30%. The primer coating is dried at room conditions (23°C, RH 60%).

The abrasion resistance of coated panels (test double wear) is determined after 1 hour and after 24 hours. In the test double abrasion test surface is moistened with two drops of water (in a double case of wet abrasion), then RUB the cotton-wool swab with a little pressure. One pass back and forth is a dual abrasion. The results are expressed as the number of dual abrasion to remove the coating. If the coating withstands 100 dual abrasion, the final dry film thickness (tsp) is compared with the original value. If the thickness of the dry the film is reduced by more than 25%, the results are expressed as >100. If the dry film thickness is reduced by less than 25%, the results are expressed as ≫100. The results are shown in table 2.

Table 2
Example No.The Sol of silicon dioxidewt.% aluminium oxideThe time between mixing and application (h)DHS, in 1 hourDHS, 24 hour
6a1Ludox SM-Fresh (0)70≫100
6b1Ludox SM-0,542>100
6c1Ludox SM-1,5614
6d1Ludox SM-422
7aBindzil 25AT/3600,27Fresh (0)60≫100
7bBindzil 25AT/3600,270,520≫100
7cBindzil 25AT/3600,27613>100
7cBindzil 25AT/3600,27 24824
8aBindzil 25AT/3600,39Fresh (0)60≫100
8bBindzil 25AT/3600,390,553≫100
8cBindzil 25AT/3600,39650≫100
8dBindzil 25AT/3600,392450≫100
9aBindzil 25AT/3600,47Fresh (0)1025
9bBindzil 25AT/3600,470,5825
9cBindzil 25AT/3600,4761125
9dBindzil 25AT/3600,47241227
1Comparative example

2Primer composition formed a gel to be applied on the canvas.

Examples 10-13

Prepare the primer composition of the coating metal semifinished product of examples 1, 2, 3 and 4. Through of 0.5, 1.5, 4, 6 and/or 24 h after mixing components of the composition are applied to the steel panel size 15 cm·10 cm thick dry p is Enki 15-20 μm at 35° C and relative humidity 30%.

After drying of the coating to the disappearance of stickiness with a weak touch of a finger, they are treated with 5%solution of partially hydrolyzed (pH 2) TEOS (tetraethylorthosilicate) in water. Then the primer coating is dried at room conditions (23°C, RH 60%). The abrasion resistance of coated panels (test double wear) is determined after 1 hour and after 24 hours after treatment with a solution of TEOS. The results are shown in table 3.

Table 3
Example No.The Sol of silicon dioxidewt.% aluminium oxideThe time between mixing and application (h)DHS, 1 h3DHS, 24 hour4
10a1Ludox SM-0,5>100≫100
10b1Ludox SM-1,518>100
10c1Ludox SM-422
11aBindzil 25AT/3600,270,5>100≫100
11bBindzil 25AT/3600,27/td> 650>100
11cBindzil 25AT/3600,27242424
12aBindzil 25AT/3600,390,5>100≫100
12bBindzil 25AT/3600,396>100≫100
12cBindzil 25AT/3600,3924>100≫100
13aBindzil 25AT/3600,470,527≫100
13bBindzil 25AT/3600,47630≫100
13cBindzil 25AT/3600,472427≫100
1Comparative example

2Primer composition formed a gel to be applied on the basis of

3Measurement of the wet dual abrasion spend 1 hour after treatment TEOS

4Measurement of the wet dual abrasion spend after 24 hours after treatment TEOS

Example 14

To assess the impact of different ways of conditioning the coating after application of the following ingredients in preparing the compositions with a concentration of solids 28 vol.%. Primer coating has a volume concentration of pigment 70%, at 1,06 times the critical volume concentration of pigment.

Componentwt.%
The Sol of silicon dioxide Bindzil 25AT/36032,5
(0.39 wt.% aluminium oxide)
Zinc41,6
Minex 209,1
Molywhite 2122,2
Bentone EW0,2
Water12,6
XZ947701,8

The primer is prepared by mixing a Sol of silicon dioxide with water and Bentone, and the resulting binder is mixed with pigments before applying to the steel. The obtained primer coating applied to the steel panel size 15 cm × 10 cm with a dry film thickness of 15-20 μm at 35°C and relative humidity of 30%. The primer coating is dried at room conditions (20°, OB 60%).

In the experience 14a after drying to extinction stickiness weak when you touch your finger it is treated with 5%solution of ZnSO4water.

In the experience 14b is covered with a panel maintained at 23°and OB 60%.

In the experience of 14C-covered panel incubated at 23°and OB 35%.

The abrasion resistance of the coated panel is th (test double wear) is determined after 10 min, 1 hour and after 24 hours after conditioning. In addition to this measure the hardness of corydaline scale. The results are shown in table 4.

Table 4
Example No.Air conditioning after applying theDHS/TX, 10 min1DHS/TX, 1 h2DHS/TX, 24 hour3DHS/TX, 48 h4
14a5% ZnSO4≫100/6T≫100/6Tnot MEAs.not MEAs.
14b23°C, RH 60%28/2T≫100/4T≫100/6Tnot MEAs.
14c23°C, RH 35%20/TM25/T53/4T≫100/4T
1Measurement of the wet dual abrasion and hardness by pencil scale performed after 10 min of treatment

2Measurement of the wet dual abrasion and hardness by pencil scale spend 1 hour after processing

3Measurement of the wet dual abrasion and hardness by pencil scale carried out within 24 hours after processing

4Measurement of the wet dual abrasion and hardness ka is andsnow scale carried out within 48 hours after processing

Examples 15 and 16

To assess the impact of modifications of aluminum oxide on the shelf life and speed of manifestation of the properties of the sols prepared compositions with a concentration of solids 28 vol.% and the volume concentration of the pigment is 50%0,72 from the critical volume concentration of pigment.

The formulation is prepared from the following ingredients:

Componentwt.%
The Sol of silicon dioxide35,0
Zinc42,2
Minex 201,7
Molywhite 2122,2
Bentone EW0,2
Waterthe 15.6
XZ947703,1

These formulations are prepared by two primer coating using two different sols of silica, namely: 16 nm Sol Nyacol for comparative example 15 and 16 nm Sol Nyacol A1 for example 16. The obtained primer coating applied to the steel panel size 15 cm × 10 cm immediately after 2 h, 5 h and 24 h after mixing the composition with a dry film thickness of 15-20 μm at 35°C and relative humidity of 30%. The primer coating is dried at room conditions (20°, OB 60%).

The abrasion resistance of coated panels (test double toughened the Institute of economy and management) is determined after 1 hour and after 24 hours after coating. In addition, measure the pencil hardness scale. The results are shown in table 5.

Examples 17 and 18

To assess the impact of the size of the modified aluminum oxide sols on the properties of the primer coating of metal prefabricated prepare two compositions with a volume concentration of the pigment is 50%. In example 17 composition is prepared from the following ingredients.

Componentwt.%
The Sol of silicon dioxide Bindzil 25AT/36050,8
(7 nm)of 25.5 wt.% in the water
Zinc42,2
Minex 203,5
Molywhite 2122,2
Bentone EW0,2
Water-
XZ947703,1

For example 18 to prepare the composition of example 16. The primer coating is dried at room conditions (20°, OB 60%).

The abrasion resistance of coated panels (test double wear) is determined after 1 hour and after 24 hours after coating. In addition, measure the pencil hardness scale. The results are shown in table 6.

That the face 6
Example No.The Sol of silicon dioxideSize Zolawt.% aluminium oxideDHS/TX 1 hour1DHS/TX 24 hour2
17Bindzil AT/3607 nm0,4425/T≫100/3T
18Nyacol Al16 nm0,4430/TM≫100/3T
1Measurement of the wet dual abrasion and hardness by pencil scale performed within 1 hour after application
2Measurement of the wet dual abrasion and hardness by pencil scale performed within 1 hour after application

Examples 19-21

To assess the impact of the modification of aluminum oxide and adding dimethylaminoethanol (DMAE), as a secondary increase shelf-life of the agent on the speed of manifestation of the properties and shelf life of small nuclei, prepare a few songs. The volume concentration of the pigment was 50.0%0,72 from the critical volume concentration of pigment.

In example 19 to prepare a composition having a volume solids concentrations by 28%, from the following ingredients.

Component wt.%
Ludox SM 7 nm46,7
Zinc42,2
Minex 201,7
Molywhite 2122,2
Bentone EW0,2
Watera 3.9
XZ947703,1

For example 20 to prepare a composition having a volume solids concentrations for 26%of the following ingredients.

Componentwt.%
Bindzil 25AT/360 7 nm (of 0.44 wt.% aluminium oxide)50,7
Zinc42,2
Minex 201,6
Molywhite 2122,2
Bentone EW0,2
XZ947703,1

For example 21 to prepare the composition of example 20 and mixed with DMAE. The number of DME in the mixture is 1 wt.% based on the total weight of the mixture.

The abrasion resistance of coated panels (test double wear) is determined after 1 hour after coating. In addition, measure the pencil hardness scale. In these experiments, it is assumed that on the expiry date indicates 50%reduction characteristics of the coating, measured within 1 hour after application. The results are shown below in table 7.

Table 7Example

No.The Sol of silicon dioxidewt.% aluminium oxidewt.% DMAEThe time between mixing and application (h)DHS/TX 1 hour2Viable19a1Ludox SM--fresh (0)33/TM 19b1Ludox SM--0,512/M<30 min19c1Ludox SM--14/M 20aBindzil 25AT/3600,44-fresh (0)32/TM 20bBindzil 25AT/3600,44-0,526/TM˜1 hour20sBindzil 25AT/3600,44-118/M 20dBindzil 25AT/3600,44-28/M 21aBindzil 25AT/3600,441fresh (0)67/H  21bBindzil 25AT/3600,4410,564/M SBindzil 25AT/3600,441164/TM2-4 hours21dBindzil 25AT/3600,441251/TM EBindzil 25AT/3600,441429/TM 1Comparative example

2Measurement of the wet dual abrasion and hardness by pencil scale performed within 1 hour after application

1. The method of applying a primer coating on the steel is intended for the Assembly and application of the top coating, in which the steel primed with a primer coating containing a binder on the basis of silicon dioxide, characterized in that the binder contains stabilized aluminum oxide aqueous Sol of silicon dioxide, and optionally a small amount of alkali metal silicate, and the specified binding substance has a molar ratio of SiO2:M2O, where M represents the total number of ions of the alkali metal and ammonium ions, of at least 6:1 and dipole, as a primer coating has dried to the disappearance of stickiness with a weak touch of a finger, it is not necessarily treated with a solution that increases the strength of the film.

2. The method according to claim 1, wherein the stabilized alumina Sol of silicon dioxide is a surface-modified aluminum oxide Sol of silicon dioxide.

3. The method according to claim 1 or 2, characterized in that the binder contains from 0.05 to 2.0 wt.% of aluminum oxide, calculated as the mass percent of Al2About3based on the Sol of silicon dioxide, and particles optional silicate in composition.

4. The method according to any one of claims 1 to 3, characterized in that the binder is a colloidal solution of silicon dioxide with a molar ratio of SiO2:M2O at least 25:1.

5. The method according to any one of claims 1 to 4, characterized in that the particles of silicon dioxide have an average particle size equal to or smaller than 22 nm.

6. The method according to claim 5, characterized in that the particles of silicon dioxide have an average particle size equal to or smaller than 16 nm.

7. The method according to any one of claims 1 to 6, characterized in that the primer coating further comprises zinc powder and/or a zinc alloy.

8. The method according to any one of claims 1 to 7, characterized in that the primer coating further comprises an organic resin.

9. The method according to any and what claims 1 to 8, characterized in that after drying of the primer coating to the disappearance of stickiness with a weak touch of a finger, covered with a basis immersed in water or, alternatively, soak in the atmosphere with a relative humidity of at least 50%.

10. The method according to any one of claims 1 to 9, characterized in that the pH of the binder on the basis of silicon dioxide is brought to a pH in the range from 9.5 to 11.

11. The composition of the primer coating for steel bases containing binder on the basis of silicon dioxide, characterized in that the binder contains stabilized aluminum oxide aqueous Sol of silicon dioxide and, optionally, a small amount of alkali metal silicate, and the specified binding substance has a molar ratio of SiO2/M2O, where M represents the total number of ions of the alkali metal and ammonium ions, of at least 6:1.

12. Primer coating according to claim 11, characterized in that the binder is a modified aluminum oxide Sol of silicon dioxide containing from 0.05 to 2.0 wt.% of aluminum oxide, calculated as the mass percent of Al2O3based on the Sol of silicon dioxide, and particles optional silicate present in the composition.

13. Primer coating according to claim 11 or 12, characterized in that the particles on the silica or silicate are medium size equal to or less than 22 nm.



 

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< / BR>
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