CN100467558C - Oriented silicon steel insulation coating capable of improving punched piece performance - Google Patents
Oriented silicon steel insulation coating capable of improving punched piece performance Download PDFInfo
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- CN100467558C CN100467558C CNB2005101109021A CN200510110902A CN100467558C CN 100467558 C CN100467558 C CN 100467558C CN B2005101109021 A CNB2005101109021 A CN B2005101109021A CN 200510110902 A CN200510110902 A CN 200510110902A CN 100467558 C CN100467558 C CN 100467558C
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Abstract
This invention discloses an oriented silicon steel insulation coating, which can be used to improve the performance of the laminated sheet . It has the composition weight percentage as follows: polyether-modified silicon oil, the water solution with 1% weight proportion, accounts for 0.01%-2.0%, of which the radio of hydrophilic chains to hydrophobic chains ranges from 20/80 to 100/0; aluminium dihydrogen phosphate 3%-24%, colloidal silica 4%~16%, chromic anhydride 0.15%~4.50% and the rest is water. After coated in the oriented electrical steel, the said insulation coating can remarkably enhance the laminated sheet times by the intrinsic lubricity of silicone during the machining of oriented silicon steel, and hence greatly enhance the production efficiency. Besides, due to the favorable water-solubility of the polyether-modified silicon oil and the common heat-resistance of the silicone products, the said coating is easily prepared, uniformly coated, and has good dispersibility. The coated surface is in good quality, able to endure sintering with high temperature without thermal degradation.
Description
Technical field
The present invention relates to a kind of coating, relate in particular to a kind of oriented silicon steel coating.
Background technology
U.S. Armco company has proposed the C-5 coating the earliest, and this is a kind of inorganic phosphate magnesium coating.Kawasaki, Japan system iron has 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 (patent No.: clear 48-39338, clear 53-28043), and its composition is colloid silica, aluminium dihydrogen phosphate and chromic trioxide.
Most of oriented silicon steel insulating coatings all are to adopt pure inorganic composition to form.The advantage of inorganic coating is that high thermal resistance, electrical insulating property, tack are good.In addition, thermal expansivity is little makes greatly that with tensile stress iron loss further reduces.Yet, existing masking liquid is because its component all is an inorganics, hardness is bigger than normal after causing coating to apply, the punching poor-performing, have only (burr height＜50 μ m) about 1.5 ten thousand times, be unfavorable for the punching processing of oriented silicon steel when making E-I type small transformers, reduce the punching number of times greatly, increase frequency and production cost that enterprise changes workpiece, reduce production efficiency.
The glassy bottom (Magnesium Silicate q-agent film) of considering oriented silicon steel surface insulation coating below is very hard, and punching is had a significant impact.So in order to satisfy the manufacturing that oriented silicon steel can well be used in E-I type transformer, inorganic insulating membrane often falls to be coated with the pickling of glass Magnesium Silicate q-agent bottom in electrical steel manufacturer again.
U.S. Armco company proposes to remove with pickling the positive Magnesium Silicate q-agent (Mg on siliconized plate surface
2SiO
4) after, apply insulating coating again, can improve the punching number of times (patent No.: US 5547519) of oriented silicon steel sheet so to a certain extent.
Because Mg
2SiO
4MgO and SiO when being the oriented silicon steel high temperature annealing
2One deck glassy membrane that forms, this layer glassy membrane is very hard, thereby can reduce the punching number of times of siliconized plate.But in case after removing, can have influence on solidity to corrosion, the insulativity of final stress coating and the tensile stress that in steel, produces again.So this method has also been lost other useful coating characteristic when improving punching.In addition, scrub Mg
2SiO
4Glassy membrane has increased production process undoubtedly one, causes complicated operation, and production cost promotes and efficient is lower.
In order to overcome the shortcoming of inorganic coating, consider to add partial organic substances, increase the self lubricity of coating itself, and then improve the punching performance of oriented silicon steel sheet.The advantage such as original inorganic coating is high temperature resistant except having for this coating, good insulating and thermal expansivity are little, the more notable punching performance that improved, and improved sliding, wettability, levelling property to a certain extent, the coatingsurface quality also is improved.
Japan Nippon Steel proposes to apply a certain amount of organic resin (as polyvinylamine, polypropylene amine, Resins, epoxy) on glassy membrane, property sheared and sliding are obviously improved, and the tensile stress of generation is bigger, and iron loss reduces the (patent No.: clear 62-14405, flat 2-128405, flat 3-28321).
This type coating is similar to half organic coating that non orientating silicon steel is used, this coating can improve the punching number of times really, but its drawback is: economically, itself production cost technology of raw materials such as polyvinylamine is higher, product price is high, and this has limited the production utilization in reality greatly.On the technology, after applying, toasting insulating coating, also need through 850 ℃ of pyritous coating sintering, if use above-mentioned general organic resin, all thermolysiss in a large number of organism under this high temperature make organic composition lose efficacy, thereby can not play the effect of the raising punching performance of original expectation.
By the investigation to domestic and international oriented silicon steel, to the inquiry of patent, document etc., the oriented silicon steel insulating coating that can find to have good punching performance is still blank at home; Taked many methods in order to improve the punching number of times abroad: United States Patent (USP) relies on removes hard glassy membrane (Mg
2SiO
4) improve punching, but this method has been sacrificed other important coating performances.The Japanese Patent shearing of adding organic resin improved oriented electrical steel, coating heat resistance is poor, the little problem of property degree is sheared in raising but this method exists.
Summary of the invention
The objective of the invention is to be doped with the insulating coating of polyether modified silicon oil by exploitation, then it is coated on the oriented electrical steel, rely on the oilness of organosilicon self, improve the punching number of times that the oriented silicon steel sheet adds man-hour significantly, thereby promoted production efficiency to a great extent.In addition,, make that the masking liquid allocation process is easy because polyether modified silicon oil has the high thermal resistance that good water-solubility and organosilicon product generally have, good dispersity, coating is even, and it is good to apply the rear surface quality, can stand high temperature sintering and not thermolysis.
For achieving the above object, technical scheme of the present invention is:
This oriented silicon steel insulating coating has following a few part to constitute:
1.
Polyether modified silicon oil
Add polyether modified silicon oil in the coating, can on coating and air interface, form one deck polysiloxane film.The latter both can stop or slow down the volatilization of solvent in the coating, also can reduce in the drying process because of thermograde and surface tension variations and cause the influence of internal flow of filming coatingsurface, thereby improve surface mobility, prevent from or reduce coating in drying process, to bubble and form depression.Owing to have characteristics such as low surface tension, excellent lubrication (metal to metal), good dispersiveness and thermostability, low toxicity or nontoxicity, production cost are low, make the side group polyether silicone oil be highly suitable for water-based paint.
Polyether modified silicon oil is very big polyether segment and the polysiloxane segment of do as one likes energy difference, links by chemical bond to form.Binding between polyether segment and the siloxanes segment has dual mode again, promptly links by Si-O-C key or Si-C key.Because the latter is stable to water, we select the polyether silicone oil of Si-C class side chain type.Its typical molecular structural formula is as follows:
Hydrophilic polyether segment gives that it is water-soluble, and the hydrophobic polydimethylsiloxane segment of lyophoby is given its low surface tension.The concrete structure and the composition of polyether silicone oil depend primarily on purposes.Known, the structure of polyethers (comprises molar mass, hydrophilic chain link (C
2H
4O) and hydrophobic chain link (C
3H
6O) ratio, content and END CAPPED GROUP kind (alkyl, alkoxyl group and acyloxy)).The polydimethylsiloxane specification (comprises molar mass, Me
2The ratio of SiO chain link and MeHSiO chain link etc.) and the mode of connection of polyethers and polysiloxane and ratio etc. all water-soluble, the pure dissolubility of multipolymer and surfactivity etc. are had material impact.
Thereby, change m, n, x, y and R just can obtain the polyether silicone oil of different performance, select suitable polyether silicone oil can satisfy the desired properties of coating.
Hydrophilic chain link (the C of polyether modified silicon oil used in the present invention (the polyether modified silicon oil massfraction is 1%～2% the aqueous solution, promptly contains the aqueous solution of the polyether modified silicon oil of 1%～2% massfraction)
2H
4O) and hydrophobic chain link (C
3H
6O) proportional range is 20/80～100/0, considers that masking liquid has forming process with 30/70～90/10 for well.
The representative polyether modified silicon oil that sell in market, the BYK-301,307,331,333,335,341,345,346,348 that produces as German Bi Ke chemical company; Baysilone OL 17, OL 31, OL 44 that Bayer A.G produces; Wet KL 245, the Wet 250 of Germany Di Gao chemical company, Glide ZG 400,410,435,440; Japan east shake PolyflowKL-245, the Glanol 115 of chemical company; The WREAMA of Taiwan three change Industrial Co., Ltd.s etc. can use.
Polyether modified silicon oil (non-volatile content) consumption generally accounts for 0.01%～2.0% of prescription total mass, with 0.025%～1.0% for well.
2.
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 3%～24% of masking liquid total mass.
3.
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 4%～16% of masking liquid total mass.
4.
Chromic trioxide
Chromic trioxide improves the oilness of masking liquid and makes in the phosphoric acid salt free phosphoric acid more stable.
Chromic trioxide (CrO
3) consumption generally accounts for 0.15%～4.50% of masking liquid total mass.
The auxiliary component of above 4 kinds of main components or needs is mixed, just obtained required oriented silicon steel insulating coating with good punching performance.Mixing can be carried out in having the reactor of stirring.Coating adds the coating machine feeder system and just can apply.
The present invention is to be that major ingredient and the various additives of mixing thinner, filler, toughner, tinting material, fire retardant, rust-preventive agent, anti-settling agent, thixotropic agent or defoamer, surface conditioner, tackifier, pigment dispersing agent, sanitas etc. are as required formed with above-mentioned four kinds of compositions.
Adopt this masking liquid that directional silicon steel is applied, again coating is toasted and high temperature sintering, just can obtain every excellent property, especially the good directional silicon steel of punching.
Have the application of the masking liquid of raising punching performance in the oriented silicon steel coatings art: the oriented silicon steel insulating coating overwhelming majority uses pure inorganic paint in the world at present, the present invention proposes to be added into the production of carrying out the oriented silicon steel coating in the inorganic masking liquid with organosilicon first, mainly refer to water-soluble good polyether modified silicon oil is applied to oriented electrical steel, make the oriented silicon steel of punching excellent performance.
Select for use polyether modified silicon oil well to mix with water-borne coatings, convenient preparation masking liquid can utilize its resistant to elevated temperatures characteristic to make coating can stand 850 ℃ of pyritous sintering again.Final oilness by means of polyether modified silicon oil self promotes the punching number of times of oriented silicon steel greatly.
The check analysis method of this masking liquid
For the masking liquid that is doped with polyether modified silicon oil, after preferably stirring with the dimethylbenzene dilution of 4 times of amounts earlier, centrifugation divides and removes contained inorganic component (aluminium dihydrogen phosphate, colloid silica and chromic anhydride).Available EI after the inorganic component drying, X diffraction or electron microscope are determined its composition.Get part organosilicon xylene solution, casting film-forming on the KBr crystal, the structure that IR determines polysiloxane is surveyed in dry back.Concrete IR spectroscopic analysis is as shown in table 2:
After in analyzing masking liquid, containing polyether modified silicon oil, also need further to hydrophilic chain link (C in the organosilicon
2H
4O) and hydrophobic chain link (C
3H
6O) ratio is tested, and analyzes and adopts cloud point method and HLB value.Measure cloud point can add 1% (massfraction) in test tube polyether silicone oil solution 15ml, stop heating after being warming up to muddiness, the temperature that stirs when observing solution down and becoming limpid by muddiness is cloud point.Can find the C of mapping cloud point by tabling look-up
2H
4O/C
3H
6O proportional range, cloud point are higher, show that wetting ability is bigger, C
2H
4O/C
3H
6The O ratio is high more.
The HLB value is the equilibrium value of hydrophilic group and oleophilic group in the molecule, can be 0～40 variation, be worth greatly more, and the expression wetting ability is good more, C
2H
4O/C
3H
6The O ratio is high more.The emulsion of measuring the simple a kind of method of HLB value and being with the tensio-active agent preparation of known HLB value contrasts and gets.
The main infrared signature absorption frequency of table 1. polyether modified silicon oil
| Group | Frequency/cm -1 | Analyze |
| In the Si-Me polysiloxane: Me 3SiO 0.5(M) Me 2SiO (D) MeSiO 1.5(T) | 1275～1245,865～750 1250,840,755 1260,860 (weak), 800 1270,780～760 | Si-Me in the siloxanes is at 1260cm -1The place, peak shape is strong and sharp, simultaneously at 865～750cm -1There are one or more strong peaks at the place.Some contains Me 3SiO 0.5Compound, at 1250cm -1The place splits into bimodal.Dimethyl silica chain link (D) is at 860cm -1Quite weak peak appears in the place, in many multipolymers that contain the D chain link, and 860cm -1Peak shift to 845cm -1, and grow. |
| Si-O-Si | 1130～1000 | At 1130～1000cm -1In one or more very strong peaks appear; Sily oxide and cyclosiloxane (oligomerization |
| Degree) a Si-O-Si peak only occurs, when siloxane chain increased or is with side chain, the Si-O-Si peak broadened and is complicated, bimodal or a plurality of overlapping peakss occur. | ||
| C-O-C | 1210～1050 | C-O-C is the feature structure of ethers, has two kinds of stretching vibrations of symmetry and unsymmetrically to absorb.Because the quality of oxygen approaches carbon, make the stretching vibration of the C-O of ether absorb the similar of position and C-C, be positioned at the fingerprint region of C-C stretching vibration, but moment of dipole changes greatly during the C-O vibration, make its absorption intensity bigger, help difference with C-C.Therefore its characteristic is strong. |
We are by research and practice, and it is that organic constituent is added in the inorganic masking liquid that the polyether modified silicon oil with good aqueous solubility is adopted in decision.After the masking liquid of preparation applies like this, can not only improve the punching number of times of siliconized plate, and because organosilyl self character also still can keep the high thermal resistance of coating, and improve the oilness of coatingsurface.
Existing prescription of table 2. and comparison of the present invention
Beneficial effect of the present invention
This insulating coating that is doped with polyether modified silicon oil of exploitation, be coated on it on the oriented electrical steel after, rely on the oilness of organosilicon self, improve the punching number of times that the oriented silicon steel sheet adds man-hour significantly, thereby promoted production efficiency greatly.In addition,, make that the masking liquid allocation process is simple because polyether modified silicon oil has the high thermal resistance that good water-solubility and organosilicon product generally have, good dispersity, coating is even, and it is good to apply the rear surface quality, can stand high temperature sintering and not thermolysis.
Embodiment
Specific embodiment is referring to table 3, table 4.
As can be seen from Table 4, in actual example 1～8, along with increasing of polyether modified silicon oil add-on, the punching number of times promotes significantly, reaches as high as 300,000 times.And in comparative example 1 and 3, because masking liquid does not add silicone ingredients, the oriented silicon steel sheet punching number of times that causes applying pure inorganic coating has only 1.5 ten thousand times.Certainly, the polyether modified silicon oil addition neither be The more the better, in comparative example 2 and 4, though more organic composition makes the punching number of times bring up to 450,000 times, but causes the appearance of film variation.
The invention process is coated to masking liquid to toast with high temperature sintering on the cold rolling electric substrate with roller coating machine and gets final product, and therefore can be applicable to the manufacturer of domestic oriented silicon steel.
The insulating coating main application that contains organosilicon class polyether modified silicon oil is to significantly improve the punching of E-I type transformer with directional silicon steel.Do not increasing production process, do not reduce under the prerequisite of production efficiency, rely on advantages such as its distinctive water-soluble, thermotolerance, dispersiveness and oilness, make that the masking liquid allocating technology is easy, coating good-looking, material punching performance significantly improve, the cost of spare and accessory parts reduces greatly.This shows, in view of many advantage of this insulating coating and cost and benefit two aspects of being valued by manufacturer, market can become very urgent to the demand of oriented silicon steel with good punching, and half organic coating that is used on the oriented silicon steel also is to initiate at home.
The polyether modified silicon oil that table 3. is commercially available
| No | Polyether modified silicon oil | Trade(brand)name | Name of manufacturing factory | Non-volatile part (DIN53216,10min, 150 ℃) |
| 1 | Polyether-modified dimethyl polysiloxane | BYK-348 | Germany Bi Ke chemical company | ≥96％ |
| 2 | Polysiloxane-polyether copolymer | Wet KL 245 | Germany Di Gao chemical company | 95～100％ |
Claims (5)
1. can improve the oriented silicon steel insulating coating of punching performance, its composition quality per-cent is,
Polyether modified silicon oil, 0.01%～2.0%;
Wherein, polyether modified silicon oil is that massfraction is 1%～2% the aqueous solution, and the proportional range of wherein hydrophilic chain link and hydrophobic chain link is 20/80～100/0;
Aluminium dihydrogen phosphate, 3%～24%;
Colloid silica, 4%～16%;
Chromic trioxide, 0.15%～4.50%;
All the other are water.
2. the oriented silicon steel insulating coating that improves the punching performance as claimed in claim 1 is characterized in that, described polyether modified silicon oil content is 0.025%～1.0%, the mass percent meter.
3. the oriented silicon steel insulating coating that improves the punching performance as claimed in claim 1 or 2 is characterized in that, the proportional range of hydrophilic chain link and hydrophobic chain link is 30/70～90/10 in the described polyether modified silicon oil.
4. the oriented silicon steel insulating coating that improves the punching performance as claimed in claim 1 is characterized in that, hydrophilic chain link is C in the described polyether modified silicon oil
2H
4O, hydrophobic chain link are C
3H
6O.
5. the oriented silicon steel insulating coating that improves the punching performance as claimed in claim 1 or 2 is characterized in that, the BYK-301,307,331,333,335,341,345,346,348 that described polyether modified silicon oil selects for use German Bi Ke chemical company to produce; BaysiloneOL 17, OL 31, OL 44 that Bayer A.G produces; Wet KL 245, the Wet 250 of Germany Di Gao chemical company, Glide ZG 400,410,435,440; Japan east shake Polyflow KL-245, the Glanol 115 of chemical company; The WREAMA of Industrial Co., Ltd. is changed in Taiwan three.
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|---|---|---|---|
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| CN100467558C true CN100467558C (en) | 2009-03-11 |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN102558923B (en) * | 2012-01-04 | 2016-12-14 | 无锡华精新材股份有限公司 | The coatings that a kind of orientation silicon steel belt surface is coated with |
| CN104530782B (en) * | 2015-01-15 | 2017-02-22 | 上海迪升防腐新材料科技有限公司 | Phosphate coating solution and preparation method thereof |
| CN111171608A (en) * | 2020-01-22 | 2020-05-19 | 上海迪升防腐新材料科技有限公司 | Insulating masking liquid and preparation method and application thereof |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1048554A (en) * | 1989-07-05 | 1991-01-16 | 新日本制铁株式会社 | The grain-oriented magnetic steel sheet and the insulating coating method of forming thereof |
| CN1291661A (en) * | 1999-09-14 | 2001-04-18 | 新日本制铁株式会社 | Orientation electric steel plate with excellent film covering characteristics and its making method |
-
2005
- 2005-11-29 CN CNB2005101109021A patent/CN100467558C/en active Active
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1048554A (en) * | 1989-07-05 | 1991-01-16 | 新日本制铁株式会社 | The grain-oriented magnetic steel sheet and the insulating coating method of forming thereof |
| CN1291661A (en) * | 1999-09-14 | 2001-04-18 | 新日本制铁株式会社 | Orientation electric steel plate with excellent film covering characteristics and its making method |
Non-Patent Citations (1)
| Title |
|---|
| 无取向硅钢表面绝缘涂层. 储双杰，翟标，戴元远.材料保护，第31卷第1期. 1998 * |
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