CN101135049A - Non-chromic environment protective oriented silicon steel insulating coating - Google Patents
Non-chromic environment protective oriented silicon steel insulating coating Download PDFInfo
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- CN101135049A CN101135049A CNA2006100307176A CN200610030717A CN101135049A CN 101135049 A CN101135049 A CN 101135049A CN A2006100307176 A CNA2006100307176 A CN A2006100307176A CN 200610030717 A CN200610030717 A CN 200610030717A CN 101135049 A CN101135049 A CN 101135049A
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Abstract
The present invention discloses one kind of environment friendly no-chromium insulating paint for oriented silicon steel. The paint consists of non-ionic surfactant of block polymer in 0.01-0.3 wt%, boric acid in 0.2-3 wt%, aluminum dihydrogen phosphate in 9-30 wt%, silica colloid in 8-20 wt%, and pure water for the rest. The paint can form insulating coating with no chromium causing environment trouble, high homogeneity, high corrosion resistance, high heat resistance and other excellent performance.
Description
Technical field
The present invention relates to a kind of coating, relate in particular to a kind of oriented silicon steel coating of environmental protection.
Background technology
Nineteen fifty, U.S. Armco company has proposed the C-5 coating the earliest, and this is a kind of inorganic phosphate magnesium coating.1973, Kawasaki, Japan system iron proposed to add on this basis the D coating of aluminum nitrate and chromic acid again.Then, Japanese Nippon Steel has proposed stress coating T-2 coating, and its composition is colloid silica, aluminium dihydrogen phosphate and chromic trioxide.Armco has also proposed the stress coating, and main ingredient is aluminum phosphate, trimagnesium phosphate, gluey SiO
2And chromic acid, be called the Carlite-3 coating.
Japanese Patent No.: clear 52-25296, clear 53-143737 disclose the stress coating of Kawasaki Steel, and component is colloid SiO
2, primary magnesium phosphate and chromic acid form, and add SiO
2, Al
2O
3Or TiO
2Fine powder takes place bondingly when preventing stress relieving, and propose to improve water tolerance with boric acid and vitriol replacement chromic acid.
All have chromic acid in the above-mentioned oriented silicon steel insulating coating, be used to improve rust-preventing characteristic, the water tolerance of vitriol coating and make phosphoric acid salt more stable, yet chromic acid is the material to environment and human body harmful.
On February 13rd, 2003, EU Committee and European Parliament issued two stereotyped commands, that is: the instruction (ROHS) of some objectionable impurities of restriction use in instruction of electronic and electrical equipment waste (WEEE) and the electronic and electrical equipment.Command request, the index that played harmful element in the electric equipment products of selling on the European Union market on July 1st, 2006 must be up to specification, and promptly the objectionable impurities that will limit has: cadmium, lead, mercury, sexavalent chrome, Polybrominated biphenyl, polymerization bromination biphenyl ether etc.Promptly taken the lead in requiring to enter in its regional electrical sheet containing the chromium element, will have more and more countries and area to propose similar requirement from now on.
In order to overcome the shortcoming that contains the harmful coating of chromium, silicon steel manufacturer considers to come the substitute chromium acid anhydrides with the material of other form both at home and abroad.External other material of interpolation that mostly is that adopts comes the substitute chromium acid anhydrides, but because the limitation of the new character of additive own has caused coating performance to have certain defective.
Japanese Patent No.: the spy opens flat 2000178760, Te Kaiping 2000169973, Te Kaiping 2000169972, it discloses Nippon Steel and has proposed to come the substitute chromium acid anhydrides with the organic acid metal-salt, for example: calcium formiate, zinc formate, formic acid manganese, tin acetate, oxalic acid and manganous tartrate etc., the result who applies shows that the coating tack is better, but solidity to corrosion and to improve the magnetic property ability general.
Japanese Patent No. spy opens that the Kawasaki Steel proposes to come the substitute chromium acid anhydrides respectively with lithium tetraborate, lime borate, aluminum borate, Tai-Ace S 150, ferric sulfate, manganous sulfate and aluminum oxide and zirconia solid particle in flat 2005068493, the result who applies shows that the coating tack is general, but solidity to corrosion, outward appearance and to improve the magnetic property ability better.The coating that this class does not contain chromium has satisfied environmental protection requirement really, but its weak point is: owing to lacked chromic trioxide in masking liquid, both caused liquid to become relatively poor for the wettability of substrate, and caused appearance of coat not good; Make the corrosion resisting property of coating become unsatisfactory again,, can't on comprehensive evaluation, obtain satisfied result so can only satisfy a certain or several performances of coating preferably.
Japanese Patent No.: the spy opens and puts down 10015484, and the spy opens flat 10015485 and discloses the chromium-free environment-friendly coating that is applied to non-oriented electrical steel.Propose in these patents to substitute dichromate, thereby when satisfying performance, reach environmental requirement with a large amount of different organism.But oriented silicon steel insulating coating also has the process of a step high temperature sintering after the low-temperature bake drying, so all inefficacies of carbonization at high temperature of the organism in such non-oriented electrical steel coating, and then has lost the characteristic of original coating.Moreover the inorganics component concentration is few and can not be after oven dry the substrate of oriented silicon steel be formed tension force in the environmental protection masking liquid of non-oriented electrical steel, so reach the basic demand that relies on coating to reduce iron loss, improve magnetic strength.
Summary of the invention
The object of the present invention is to provide a kind of oriented silicon steel insulating coating of chromium-free environment-friendly, not only eliminated the environmental issue that the chromium element brings fully, and can guarantee every excellent propertys such as coating uniformity, solidity to corrosion, thermotolerance.
By research and practice, decision is adopted has the block polyether nonionic surface active agent of good wettability, and has good anti-corrosion and boric acid resistance toheat is that component is added in the masking liquid.After the masking liquid of preparation applies like this, not only eliminated the environmental issue that the chromium element brings fully, and can guarantee every excellent propertys such as coating uniformity, solidity to corrosion, thermotolerance.
For achieving the above object, technical scheme of the present invention is,
The oriented silicon steel insulating coating of chromium-free environment-friendly, its chemical ingredients mass percent is:
The block polyether nonionic surface active agent, its solid consumption accounts for 0.01%~0.3% of masking liquid total mass;
Boric acid, its solid consumption accounts for 0.2%~3% of masking liquid total mass;
Aluminium dihydrogen phosphate accounts for 9%~30% of masking liquid total mass;
Colloid silica accounts for 8%~20% of masking liquid total mass;
Surplus is a pure water;
Wherein, in block polyether nonionic surface active agent propylene glycol polyoxyethylene polyoxypropylene block type polyethers, the polyoxyethylene of hydrophilic segment need account for 20~90% of its total amount; The polyoxypropylene of lipophilic group, its segment length b should be greater than 15, and molecular-weight average should be greater than 900; The HLB value should be in 0.5~30 scope.
Further, the block polyether nonionic surface active agent, its solid consumption accounts for 0.01%~0.2% of masking liquid total mass.
In block polyether nonionic surface active agent propylene glycol polyoxyethylene polyoxypropylene block type polyethers, the polyoxypropylene molecular-weight average of lipophilic group is between 1000~20000.
The content of boric acid consumption is 0.4%~2%; The content of aluminium dihydrogen phosphate is 12%~24%; The content of colloid silica is 10%~18%.
Wherein,
1. block polyether nonionic surface active agent
In order to improve the wettability of liquid, often in masking liquid, add some tensio-active agents and reduce its surface tension, so that masking liquid can wetting well solid surface to solid surface.Wherein, nonionic surface active agent has good wetting action as wetting agent, has the ability of strong reduction surface tension of liquid.
The oleophilic group of nonionic surface active agent is that the hydrophobic compound (as high-carbon fatty alcohol, alkylphenol, aliphatic amide etc.) that contains reactive hydrogen provides; Its hydrophilic group be can generate the ether of hydrogen bond with water by containing, the low molecular compound of free alkyl (as oxyethane, polyvalent alcohol, thanomin etc.) provides.Just because of these characteristics, determined nonionic surface active agent more superior than ionogenic surfactant in some aspects.Nonionogenic tenside is unionization in water, and its surfactivity is embodied by neutral molecule, so stability is high, is not subject to the influence that the strong electrolyte inorganic salts exists, and also is not subject to the influence of soda acid; In water and organic solvent, all there is the good solubility can (but structure is different difference) to some extent.
It is to be main body with oxyethane, propylene oxide or other alkene oxide that the present invention uses the block polyether nonionic surface active agent, is the nonionogenic tenside of the block copolymerization of initiator with some active hydrogen compounds.Can be divided into full embedding, assorted embedding, three types of assorted embeddings entirely by its polymerization methods.Wherein full embedding type polyethers is the most important and commonly used.Propylene glycol polyethylene oxide poly(propylene oxide) ether is one of them.
Propylene glycol polyethylene oxide poly(propylene oxide) ether also claims propylene glycol polyoxyethylene polyoxypropylene block type polyethers, is weak yellow liquid or solid.This product is the poloxamer (poloxamer) of U.S. Wynadotte chemical company initiative, trade(brand)name pluronic (Pluronic).Pluronic structurally can have very widely and to change, and the physical aspect of different Pluronic products all has existence from flowable liquid, paste, sufficiently rigid solid to Powdered.All Pluronic are 100% activess, and have nonirritant, characteristics that toxicity is little.Wherein Pluronic F68 (selecting for use among the embodiment) is exactly nontoxic.These series product are the full block ether of binary initiator, and its general formula is:
HO(C
2H
4O)
a-(C
3H
6O)
b-(C
2H
4O)
cH
Increase with the polyoxypropylene ratio, then lipophilicity strengthens.Increase with the polyoxyethylene ratio, then wetting ability strengthens.Polyoxyethylene is counted difference, and wettability also changes, and too much very fewly all can make the wettability variation.
The polyoxyethylene of hydrophilic segment need account for 20~90% of total amount of compound, and preferred 40%~50%; With the carbochain be C8, C9 be example, the polyoxyethylene number is 10~12 o'clock, no matter molecular weight is much, all is that wettability is best in this molecular weight grades.The molecular weight of polypropylene glycol is about at 1600 o'clock, and wettability is best.In addition, for this class tensio-active agent, when carbochain was C7~C10, wettability was best.The polyoxypropylene of lipophilic group, its segment length b should be greater than 15, and molecular-weight average should be greater than 900, generally between 1000~20000; The HLB value should be in 0.5~30 scope.
The representative Pluronic that sell in market, the like product of producing as U.S. Wynadotte chemical company and German BASF chemical company all can use.
Block polyether nonionic surface active agent (Pluronic) consumption (solid consumption) generally accounts for 0.01%~0.3% of masking liquid total mass, with 0.01%~0.2% for well, preferably ratio control 0.015%~0.05%.
2. boric acid
Improve corrosion resistance coating energy and thermotolerance.
Boric acid consumption (solid consumption) generally accounts for 0.2%~3% of masking liquid total mass, with 0.4%~2% for well, preferably ratio control 0.5%~0.8%.
3. aluminium dihydrogen phosphate
Aluminium dihydrogen phosphate is a kind of novel inorganic synthetic materials, and normal temperature solidifies down, and liquid and solid state chemistry bonding force are strong, has high temperature resistant, antidetonation, antistripping and the good characteristics of insulating property.Be mainly used in electrical industry, resistor furnace for heat treatment and electric insulation, can be used as inorganic paint and organic coating is used.In this masking liquid, play the caking agent effect, improve the tack of insulating coating and glassy membrane bottom.
Aluminium dihydrogen phosphate (Al (H
2PO
4)
3) consumption generally accounts for 9%~30% of masking liquid total mass, with 12%~24% for well, preferably ratio control 14%~20%.
4. colloid silica
Colloid silica is that ultra-fine particles that diameter is counted nanometer to hundred nanometer is dispersed in the oyster white colloidal solution in the water.Ion at the colloid silica particle surface is the hydration type, because of water molecules covers wetting ability is arranged.As the compounding ingredient of coating to improve associativity, fastness, wearability and stain resistance.
Colloid silica (SiO
2) consumption generally accounts for 8%~20% of masking liquid total mass, with 10%~18% for well, preferably, ratio control 12%~15%.
The auxiliary component of above 4 kinds of main components or needs is mixed, just obtained required chromium-free environment-friendly oriented silicon steel insulating coating.Mixing can be carried out in having the reactor of stirring.Masking liquid adds the coating machine feeder system and just can apply.
Adopt this masking liquid that directional silicon steel is carried out dual coating, again coating is toasted and high temperature sintering, just can obtain every excellent property, especially the directional silicon steel of environmental protection.
Beneficial effect of the present invention
Do not contain chromium element in the oriented silicon steel of manufacturing of the present invention to environment and human body harmful, product belongs to environmentally friendly machine, can export to countries and regions such as European Union, both increased economic benefit, promoted social effect again, and appearance of coat, tack, solidity to corrosion and magnetic property improve situation can both reach excellent results.
Embodiment
Embodiment is referring to table 1, table 2.
Colloid silica (SiO
2) consumption generally accounts for 8%~20% of masking liquid total mass, with 10%~18% for well, preferably, ratio control 12%~15%.
Table 1 unit: mass percent
Block polyether nonionic surface active agent (%) | Boric acid (%) | Aluminium dihydrogen phosphate (%) | Colloid silica (%) | |
Embodiment 1 | 0.01 | 3.0 | 9.0 | 20.0 |
Embodiment 2 | 0.05 | 2.6 | 13.2 | 19.5 |
Embodiment 3 | 0.11 | 2.2 | 16.5 | 18.2 |
Embodiment 4 | 0.15 | 1.7 | 20.2 | 16.6 |
Embodiment 5 | 0.19 | 1.3 | 23.1 | 14.1 |
Embodiment 6 | 0.23 | 0.9 | 26.4 | 11.8 |
Embodiment 7 | 0.27 | 0.5 | 27.9 | 10.3 |
Embodiment 8 | 0.30 | 0.2 | 30.0 | 8.0 |
Embodiment 9 | 0.015 | 2.0 | 11.8 | 17.5 |
Embodiment 10 | 0.20 | 0.8 | 24.0 | 15.0 |
Comparative example 1 | 0.00 | 2.8 | 10.6 | 23.1 |
Comparative example 2 | 0.80 | 1.4 | 32.4 | 5.7 |
Comparative example 3 | 0.10 | 3.6 | 21.5 | 9.8 |
Comparative example 4 | 0.35 | 0.1 | 6.4 | 17.3 |
Annotate: 1, the mass percent residual content is a pure water.
2, the block polyether nonionic surface active agent is selected the Pluronic F68 that German BASF AG produces, trade(brand)name polyoxyethylene-polyoxypropylene multipolymer for use.Can also select the propylene glycol block polyether F38 of Hangzhou etherealize worker of a specified duration company limited for use.
Table 2. coating performance result
Appearance of coat | Tack | Solidity to corrosion | Magnetic property improves ability | ||
△B 8 (T) | △P 17/50 (W/Kg) | ||||
Embodiment 1 | ◎ | ◎ | ◎ | 0.033 | -0.312 |
Embodiment 2 | ◎ | ◎ | ◎ | 0.038 | -0.371 |
Embodiment 3 | ◎ | ◎ | ◎ | 0.040 | -0.309 |
Embodiment 4 | ◎ | ◎ | ◎ | 0.051 | -0.302 |
Embodiment 5 | ◎ | ◎ | ◎ | 0.043 | -0.297 |
Embodiment 6 | ◎ | ◎ | ◎ | 0.032 | -0.316 |
Embodiment 7 | ◎ | ◎ | ◎ | 0.046 | -0.320 |
Embodiment 8 | ◎ | ◎ | ◎ | 0.038 | -0.281 |
Embodiment 9 | ◎ | ◎ | ◎ | 0.037 | -0.360 |
Embodiment 10 | ◎ | ◎ | ◎ | 0.039 | -0.345 |
Comparative example 1 | × | △ | ◎ | 0.033 | -0.306 |
Comparative example 2 | △ | ◎ | △ | 0.007 | -0.082 |
Comparative example 3 | ◎ | △ | ◎ | 0.013 | -0.113 |
Comparative example 4 | ◎ | △ | × | 0.039 | -0.298 |
Annotate: 1) appearance of coat: ◎: good; △: general; *: poor.
2) tack: ◎: good; △: general; *: poor.
3) solidity to corrosion: ◎: good; △: general; *: poor.
As can be seen, in actual example 1~10, in suitable masking liquid composition proportion scope, appearance of coat, tack, solidity to corrosion and magnetic property improve situation can both reach excellent results from table 1 and 2.Suitable being added with of Pluronic helps improve the coating apparent mass, but add-on is too much very few, all can make the apparent mass variation, but also can have influence on magnetic property (comparative example 1 and 2).And the suitable add-on of boric acid helps to improve corrosion resistance coating.Equally, if addition is improper, also can have influence on magnetic property and tack (comparative example 3 and 4).
The invention process is coated to masking liquid to toast with high temperature sintering on the cold rolled silicon steel substrate with roller coating machine and gets final product.
Claims (10)
1. the oriented silicon steel insulating coating of chromium-free environment-friendly, its chemical ingredients mass percent is:
The block polyether nonionic surface active agent, its solid consumption accounts for 0.01%~0.3% of masking liquid total mass;
Boric acid, its solid consumption accounts for 0.2%~3% of masking liquid total mass;
Aluminium dihydrogen phosphate accounts for 9%~30% of masking liquid total mass;
Colloid silica accounts for 8%~20% of masking liquid total mass;
Surplus is a pure water;
Wherein, in block polyether nonionic surface active agent propylene glycol polyoxyethylene polyoxypropylene block type polyethers, the polyoxyethylene of hydrophilic segment need account for 20~90% of its total amount; The polyoxypropylene of lipophilic group, its segment length b should be greater than 15, and molecular-weight average should be greater than 900; The HLB value should be in 0.5~30 scope.
2. the oriented silicon steel insulating coating of chromium-free environment-friendly as claimed in claim 1 is characterized in that, described block polyether nonionic surface active agent, and its solid consumption accounts for 0.01%~0.2% of masking liquid total mass.
3. the oriented silicon steel insulating coating of chromium-free environment-friendly as claimed in claim 1 is characterized in that, described block polyether nonionic surface active agent, and its solid consumption accounts for 0.015%~0.05% of masking liquid total mass.
4. the oriented silicon steel insulating coating of chromium-free environment-friendly as claimed in claim 1, it is characterized in that, in block polyether nonionic surface active agent propylene glycol polyoxyethylene polyoxypropylene block type polyethers, the polyoxypropylene molecular-weight average of lipophilic group is between 1000~20000.
5. the oriented silicon steel insulating coating of chromium-free environment-friendly as claimed in claim 1 is characterized in that, the content of described boric acid consumption is 0.4%~2%, by mass percentage.
6. the oriented silicon steel insulating coating of chromium-free environment-friendly as claimed in claim 1 is characterized in that, the content of described boric acid consumption is 0.5%~0.8%, by mass percentage.
7. the oriented silicon steel insulating coating of chromium-free environment-friendly as claimed in claim 1 is characterized in that, the content of described aluminium dihydrogen phosphate is 12%~24%, by mass percentage.
8. the oriented silicon steel insulating coating of chromium-free environment-friendly as claimed in claim 1 is characterized in that, the content of described aluminium dihydrogen phosphate is 14%~20%, by mass percentage.
9. the oriented silicon steel insulating coating of chromium-free environment-friendly as claimed in claim 1 is characterized in that, the content of described colloid silica is 10%~18%, by mass percentage.
10. the oriented silicon steel insulating coating of chromium-free environment-friendly as claimed in claim 1 is characterized in that, the content of described colloid silica is 14%~20%, by mass percentage.
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