CN103937941B - A kind of oriented silicon steel preparation method of extraordinary magnesium oxide boron additive material - Google Patents
A kind of oriented silicon steel preparation method of extraordinary magnesium oxide boron additive material Download PDFInfo
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- CN103937941B CN103937941B CN201310739116.2A CN201310739116A CN103937941B CN 103937941 B CN103937941 B CN 103937941B CN 201310739116 A CN201310739116 A CN 201310739116A CN 103937941 B CN103937941 B CN 103937941B
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Abstract
The present invention relates to technical field of magnesium oxide, be specifically related to a kind of preparation method of magnesium oxide additive.An oriented silicon steel preparation method for extraordinary magnesium oxide boron additive material, comprises the steps: 1) preparation of magnesium borate and magnesium hydroxide composite granule; 2) preparation of extraordinary magnesium oxide boron additive, obtains the extraordinary magnesium oxide boron additive of product grain-oriented Si steel sheet.Raw material used in the present invention is easy to get, cost is low, production technique is simple, equipment requirements is low, be easy to realize industrialization.Boron additive and the extraordinary magnesium oxide of silicon steel share, and can improve the Forming ability of grain-oriented Si steel sheet at high temperature annealing mesosilicic acid magnesium bottom, reduce the temperature of the formation of insulating film, the time of high temperature annealing.Preparation technology of the present invention is simple, production efficiency is high, and produce without byproduct in production process, product yield is up to 95%.
Description
Technical field
The present invention relates to technical field of magnesium oxide, be specifically related to a kind of preparation method of magnesium oxide additive.
Background technology
Grain-oriented Si steel sheet is the one of cold rolled silicon steel, has the advantages such as electromagnetism intensity is large, electrical loss is little, belongs to extraordinary electrician's steel.Grain-oriented Si steel sheet with extraordinary magnesium oxide be exclusively used in grain-oriented Si steel sheet produce in high temperature annealing separant and the generating material of forsterite tunicle.The Main Function of silicon steel magnesium oxide in grain-oriented Si steel sheet high temperature annealing:
1. prevent grain-oriented Si steel sheet coil of strip from sintering in annealing.
2. remove the impurity such as S, the P in oriented silicon steel.
3. can in high temperature annealing with the SiO on oriented silicon steel surface
2reaction generates forsterite tunicle, improves insulation resistance and the magnetic properties (coercive force) of grain-oriented Si steel sheet.
The extraordinary magnesia slurry of grain-oriented Si steel sheet is coated after on grain-oriented Si steel sheet, drying, curling, then carries out secondary high-temperature annealing.In the high temperature annealing stage, magnesium oxide and silicon-dioxide react.Carry out in the process of reacting at magnesium oxide and silicon-dioxide, due to the restriction of magnesium oxide material, problems such as causing both response capacitys weak, the Forming ability temperature that is weak, forsterite tunicle that therefore there is grain-oriented Si steel sheet forsterite tunicle (Magnesium Silicate q-agent bottom) in high temperature annealing is high, the high temperature annealing time is long.
Therefore need to seek the extraordinary magnesium oxide specialist additive of a kind of grain-oriented Si steel sheet, improve above-mentioned defect.Domestic and international at present also do not have systematic discussion about the extraordinary magnesium oxide specialist additive preparation method of grain-oriented Si steel sheet, although the extraordinary magnesium oxide coating material of grain-oriented Si steel sheet can also apply to the production of grain-oriented Si steel sheet, the high production of name oriented siliconized plate and the needs of energy-saving and emission-reduction and trend can not be met.
Summary of the invention
The object of the invention is to, a kind of oriented silicon steel preparation method of extraordinary magnesium oxide boron additive material is provided, solves above technical problem.
Technical problem solved by the invention can realize by the following technical solutions:
An oriented silicon steel preparation method for extraordinary magnesium oxide boron additive material, comprises the steps:
1) preparation of magnesium borate and magnesium hydroxide composite granule: aqueous solution light magnesium oxide powder being added while stirring certain boride concentrations, at the temperature of 20 DEG C ~ 30 DEG C, react 30 minutes ~ 60 minutes, the content controlled in powder is 2.0wt% ~ 4.0wt% magnesium borate, obtains magnesium borate and magnesium hydroxide composite granule;
2) preparation of extraordinary magnesium oxide boron additive: the magnesium borate obtained in step 1) and magnesium hydroxide composite granule add class antimony compounds solution and nanometer magnesia powder carries out hybrid reaction, temperature of reaction controls at 40 DEG C ~ 60 DEG C, its class antimony compounds accounts for the 4.5wt%-5.5wt% of mixture, and nanometer magnesia powder content accounts for the 4.5wt%-5.5wt% of mixture;
Carried out drying and roasting by the product obtained after hybrid reaction again, oven dry and maturing temperature control at 150 DEG C ~ 260 DEG C, obtain the extraordinary magnesium oxide boron additive of product grain-oriented Si steel sheet after crushed.
After the present invention adopts above-mentioned technique, the boron additive obtained, as extraordinary magnesium oxide additive, is exclusively used in grain-oriented Si steel sheet production, greatly can improves the response capacity of magnesium oxide and silicon-dioxide, play the Mg being reduced in siliconized plate Surface Creation
2siO
4the temperature of film, reduces the time of high temperature annealing, also serves effect of energy simultaneously.
In step 1), described boride preferably adopts boric acid or sodium tetraborate, and described light magnesium oxide powder and described boride, deionized water react and generate magnesium borate and magnesium hydroxide composite granule at the temperature of 20 DEG C ~ 30 DEG C.
In step 1), the mol ratio of described light magnesium oxide powder and described boride is 5000.0:6.4 ~ 12.8.
Step 2) in, described class antimony compounds content controls at 5wt%, and described nanometer magnesia powder content controls at 5wt%.
Step 2) in, described nanometer magnesia powder particle diameter is between 10nm ~ 60nm.The nanometer magnesia powder that the present invention selects has the advantage that nanometer powder purity is high, particle diameter is little, particle size distribution is narrow.
Step 2) in the boron additive that obtains at grain-oriented Si steel sheet solid content total in extraordinary magnesium oxide at 400ppm ~ 800ppm.
Beneficial effect: owing to adopting above technical scheme, tool of the present invention has the following advantages:
1. raw material used in the present invention is easy to get, cost is low, production technique is simple, equipment requirements is low, be easy to realize industrialization;
2. boron additive and the extraordinary magnesium oxide of silicon steel share, and can improve the Forming ability of grain-oriented Si steel sheet at high temperature annealing mesosilicic acid magnesium bottom, reduce the temperature of the formation of insulating film, the time of high temperature annealing.
3. preparation technology of the present invention is simple, production efficiency is high, and produce without byproduct in production process, product yield is up to 95%.
4. the siliconized plate of preparation meets the environmental requirement of country and European Union with extraordinary magnesium oxide boron additive product.
Accompanying drawing explanation
Fig. 1 is schematic flow sheet of the present invention.
Embodiment
The technique means realized to make the present invention, creation characteristic, reaching object and effect is easy to understand, setting forth the present invention further below in conjunction with concrete diagram.
With reference to Fig. 1, a kind of oriented silicon steel preparation method of extraordinary magnesium oxide boron additive material, comprises the steps:
1) preparation of magnesium borate and magnesium hydroxide composite granule: adopt light magnesium oxide powder, boric acid or sodium tetraborate to be raw material as boride, deionized water, the mol ratio of light magnesium oxide powder and boride is 5000.0:6.4 ~ 12.8.
Light magnesium oxide powder is added while stirring the aqueous solution of certain boride concentrations, at the temperature of 20 DEG C ~ 30 DEG C, react 30 minutes ~ 60 minutes, the content controlling powder mesoboric acid magnesium is 2.0wt% ~ 4.0wt% that magnesium borate and magnesium hydroxide composite granule account for mixture, obtains magnesium borate and magnesium hydroxide composite granule.
2) preparation of extraordinary magnesium oxide boron additive: the magnesium borate obtained in step 1) and magnesium hydroxide composite granule add class antimony compounds solution and nanometer magnesia powder carries out hybrid reaction, temperature of reaction controls at 40 DEG C ~ 60 DEG C, its class antimony compounds content controls at 5wt%, nanometer magnesia powder content controls at 5wt%, and its particle diameter is between 10nm ~ 60nm.
Again the product obtained after hybrid reaction is carried out drying and roasting, oven dry and maturing temperature control at 150 DEG C ~ 260 DEG C, obtain the extraordinary magnesium oxide boron additive of product grain-oriented Si steel sheet after crushed, boron additive at grain-oriented Si steel sheet with solid content total in extraordinary magnesium oxide at 400ppm ~ 800ppm.After boron additive completes, also need to detect, then packaging makes the finished product.
Embodiment one:
1) preparation of magnesium borate and magnesium hydroxide composite granule: aqueous solution light magnesium oxide powder being added while stirring certain boric acid concentration, at the temperature of 20 DEG C, react 60 minutes, the content controlled in powder is 2.0wt% magnesium borate, and the mol ratio of light magnesium oxide powder and boric acid is 5000.0:6.4.
2) preparation of extraordinary magnesium oxide boron additive: the magnesium borate obtained in step 1) and magnesium hydroxide composite granule add class antimony compounds solution and nanometer magnesia powder, temperature of reaction controls at 40 DEG C, its class antimony compounds content controls at 5wt%, nanometer magnesia powder content controls at 5wt%, again the product obtained after hybrid reaction is carried out drying and roasting, oven dry and maturing temperature control at 150 DEG C, obtain the extraordinary magnesium oxide boron additive of product grain-oriented Si steel sheet after crushed, its at grain-oriented Si steel sheet with solid content total in extraordinary magnesium oxide at 400ppm.
Embodiment two:
1) preparation of magnesium borate and magnesium hydroxide composite granule: aqueous solution light magnesium oxide powder being added while stirring certain boride concentrations, at the temperature of 30 DEG C, react 30 minutes, the content controlled in powder is 2.0wt% magnesium borate, and the mol ratio of light magnesium oxide powder and boric acid is 5000.0:6.4.
2) preparation of extraordinary magnesium oxide boron additive: the magnesium borate obtained in step 1) and magnesium hydroxide composite granule add class antimony compounds solution and nanometer magnesia powder, temperature of reaction controls at 60 DEG C, its class antimony compounds content controls at 5wt%, nanometer magnesia powder content controls at 5wt%, again the product obtained after hybrid reaction is carried out drying and roasting, oven dry and maturing temperature control at 180 DEG C, obtain the extraordinary magnesium oxide boron additive of product grain-oriented Si steel sheet after crushed, its at grain-oriented Si steel sheet with solid content total in extraordinary magnesium oxide at 400ppm.
Embodiment three:
1) preparation of magnesium borate and magnesium hydroxide composite granule: aqueous solution light magnesium oxide powder being added while stirring certain boride concentrations, at the temperature of 20 DEG C, react 60 minutes, the content controlled in powder is 4.0wt% magnesium borate, and the mol ratio of light magnesium oxide powder and boric acid is 5000.0:12.8.
2) preparation of extraordinary magnesium oxide boron additive: the magnesium borate obtained in step 1) and magnesium hydroxide composite granule add class antimony compounds solution and nanometer magnesia powder, temperature of reaction controls at 40 DEG C, its class antimony compounds content controls at 5wt%, nanometer magnesia powder content controls at 5wt%, again the product obtained after hybrid reaction is carried out drying and roasting, oven dry and maturing temperature control at 150 DEG C, obtain the extraordinary magnesium oxide boron additive of product grain-oriented Si steel sheet after crushed, its at grain-oriented Si steel sheet with solid content total in extraordinary magnesium oxide at 800ppm.
Embodiment four:
1) preparation of magnesium borate and magnesium hydroxide composite granule: aqueous solution light magnesium oxide powder being added while stirring certain boride concentrations, at the temperature of 30 DEG C, react 30 minutes, the content controlled in powder is 4.0wt% magnesium borate, and the mol ratio of light magnesium oxide powder and boric acid is 5000.0:12.8.
2) preparation of extraordinary magnesium oxide boron additive: the magnesium borate obtained in step 1) and magnesium hydroxide composite granule add class antimony compounds solution and nanometer magnesia powder, temperature of reaction controls at 60 DEG C, its class antimony compounds content controls at 5wt%, nanometer magnesia powder content controls at 5wt%, again the product obtained after hybrid reaction is carried out drying and roasting, oven dry and maturing temperature control at 180 DEG C, obtain the extraordinary magnesium oxide boron additive of product grain-oriented Si steel sheet after crushed, its at grain-oriented Si steel sheet with solid content total in extraordinary magnesium oxide at 800ppm.
More than show and describe ultimate principle of the present invention and principal character and advantage of the present invention.The technician of the industry should understand; the present invention is not restricted to the described embodiments; what describe in above-described embodiment and specification sheets just illustrates principle of the present invention; without departing from the spirit and scope of the present invention; the present invention also has various changes and modifications, and these changes and improvements all fall in the claimed scope of the invention.Application claims protection domain is defined by appending claims and equivalent thereof.
Claims (6)
1. an oriented silicon steel preparation method for extraordinary magnesium oxide boron additive material, is characterized in that, comprise the steps:
1) preparation of magnesium borate and magnesium hydroxide composite granule: aqueous solution light magnesium oxide powder being added while stirring certain boride concentrations, described boride adopts boric acid or sodium tetraborate, at the temperature of 20 DEG C ~ 30 DEG C, react 30 minutes ~ 60 minutes, the content controlled in powder is 2.0wt% ~ 4.0wt% magnesium borate, obtains magnesium borate and magnesium hydroxide composite granule;
2) preparation of extraordinary magnesium oxide boron additive: in step 1) in the magnesium borate that obtains and magnesium hydroxide composite granule adds class antimony compounds solution and nanometer magnesia powder carries out hybrid reaction, temperature of reaction controls at 40 DEG C ~ 60 DEG C, its class antimony compounds content controls at 4.5wt%-5.5wt%, and nanometer magnesia powder content controls at 4.5wt%-5.5wt%;
Carried out drying and roasting by the product obtained after hybrid reaction again, oven dry and maturing temperature control at 150 DEG C ~ 260 DEG C, obtain the extraordinary magnesium oxide boron additive of product grain-oriented Si steel sheet after crushed.
2. a kind of oriented silicon steel according to claim 1 preparation method of extraordinary magnesium oxide boron additive material, it is characterized in that, step 1) in, described light magnesium oxide powder and described boride, deionized water react and generate magnesium borate and magnesium hydroxide composite granule at the temperature of 20 DEG C ~ 30 DEG C.
3. a kind of oriented silicon steel according to claim 1 preparation method of extraordinary magnesium oxide boron additive material, is characterized in that, step 1) in, the mol ratio of described light magnesium oxide powder and described boride is 5000.0:6.4 ~ 12.8.
4. the preparation method of extraordinary magnesium oxide boron additive material of a kind of oriented silicon steel according to claim 1,2 or 3, it is characterized in that, step 2) in, described class antimony compounds content controls at 5wt%, and described nanometer magnesia powder content controls at 5wt%.
5. a kind of oriented silicon steel according to claim 4 preparation method of extraordinary magnesium oxide boron additive material, is characterized in that, step 2) in, described nanometer magnesia powder particle diameter is between 10nm ~ 60nm.
6. a kind of oriented silicon steel according to claim 5 preparation method of extraordinary magnesium oxide boron additive material, is characterized in that, step 2) in the boron additive that obtains at grain-oriented Si steel sheet solid content total in extraordinary magnesium oxide at 400ppm ~ 800ppm.
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| US4740251A (en) * | 1986-12-22 | 1988-04-26 | Calgon Corporation | Method for improving magnesium oxide steel coatings |
| JPH06192743A (en) * | 1992-12-28 | 1994-07-12 | Kawasaki Steel Corp | Production of grain-oriented silicon steel sheet excellent in film property and magnetic property |
| CN101845582B (en) * | 2009-03-26 | 2011-09-21 | 宝山钢铁股份有限公司 | Production method of high magnetic induction oriented silicon steel |
| CN101891219B (en) * | 2010-08-20 | 2012-05-09 | 山西宏亚科技有限责任公司 | Method for preparing special magnesium borate for oriented silicon steel |
| CN102952931B (en) * | 2011-08-30 | 2014-10-29 | 宝山钢铁股份有限公司 | Glass-film-free oriented silicon steel manufacture method and annealing isolation agent |
| CN103014285B (en) * | 2011-09-28 | 2015-04-01 | 宝山钢铁股份有限公司 | Manufacturing method of mirror surface oriented silicon steel with good magnetic performance and annealing parting agent |
| CN103114181A (en) * | 2013-01-24 | 2013-05-22 | 广东盈泉钢制品有限公司 | Coating formula of oriented silicon steel barrier coat |
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