CN101643227A - Preparation method of special magnesium oxide for grain-oriented silicon steel sheet - Google Patents

Preparation method of special magnesium oxide for grain-oriented silicon steel sheet Download PDF

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CN101643227A
CN101643227A CN200910194732A CN200910194732A CN101643227A CN 101643227 A CN101643227 A CN 101643227A CN 200910194732 A CN200910194732 A CN 200910194732A CN 200910194732 A CN200910194732 A CN 200910194732A CN 101643227 A CN101643227 A CN 101643227A
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magnesium
magnesium oxide
steel sheet
silicon steel
oriented silicon
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CN101643227B (en
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宗俊
宗巍
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Shanghai Industrial Zhentai Chemical Industrial Co., Ltd.
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SHANGHAI ZONGWEI TECHNOLOGY DEVELOPMENT Co Ltd
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Abstract

The invention relates to a preparation method of special magnesium oxide for grain-oriented silicon steel sheet, belonging to the technical field of the preparation special magnesium oxide. The methodcomprises the following steps: reacting magnesium compound solution with the mixed solution of sodium carbonate and sodium hydroxide at a temperature to prepare a mixture of intermediate product containing magnesium carbonate and magnesium hydroxide, filtrating, washing, drying, calcining at high temperature, and grinding to obtain the special magnesium oxide for grain-oriented silicon steel sheet. The method has the advantages that the raw material is accessible, the cost is low, the production process is simple, the facility request is low, the method is applicable to industrialized production; the intermediate product is easy for separation and purification and is easy to wash, the washing loss of the product is low, the product yield is high; the product is special magnesium oxide powder, the powder has high purity, the grain size is small, and the average grain size is 1-2mu m and has a certain distribution range. The method is especially suitable for the preparation of special magnesium oxide for grain-oriented silicon steel sheet.

Description

A kind of preparation method of special magnesium oxide for grain-oriented silicon steel sheet
Technical field
The present invention relates to a kind of preparation method of special magnesium oxide for grain-oriented silicon steel sheet, belong to the technical field of extraordinary magnesium oxide preparation.
Background technology
The oriented silicon steel sheet is to be exclusively used in the production of oriented silicon steel sheet, as the high temperature annealing separant with extraordinary magnesium oxide.The main effect of described magnesium oxide in oriented silicon steel sheet high temperature annealing:
1, (the thick 0.35mm of sheet～0.25mm) is sintering in high temperature (1250 ℃, 24 * 7 hours) annealing to prevent the siliconized plate coil of strip.
2, remove impurity such as S, P in the siliconized plate coil of strip.
In high temperature annealing, the SiO on described magnesium oxide and siliconized plate surface 2Reaction generates Mg 2SiO 4Film gives siliconized plate surface insulation resistance layer and magnetic properties (coercive force), thereby has improved the quality of siliconized plate.
Described magnesian part key property:
1, described magnesian activity
In order to improve described magnesium oxide and SiO 2Between response capacity, described magnesium oxide must possess activity.Ultra tiny level magnesium oxide has very big reactive behavior, therefore utilizes production technology to introduce ultra tiny level magnesium oxide particle in described magnesium oxide, has just improved described magnesian activity.
2, described magnesian particle structure
In order to improve the accumulation density between siliconized plate surface oxidation magnesium granules, it is spherical that described magnesian particle structure must tend to.Because spheroid has the closestpacking advantage.Magnesium oxide particle can be tending towards closestpacking after coating the siliconized plate surface, reduces between magnesia particle and the voidage between magnesia particle and siliconized plate surface silica dioxide, improves Mg 2SiO 4The density of film.
3, the size distribution of described magnesia particle
Because after described magnesian slurries are coated on the siliconized plate, must after super-dry, be curled into the coil-like secondary high temperature annealing that carries out, must progressively drive the magnesium hydroxide (Mg (OH) that described magnesium oxide generates away in the temperature-rise period in pulping process in annealing before the stage entering high temperature annealing 2) in water molecules, in implementing this process, the magnesium oxide layer that necessarily requires to be coated with has air permeability and good, and the water molecules in the described magnesium oxide can be overflowed in the coil of strip slit of rolling-in, in order to avoid the Mg that the aqueous vapor influence generates 2SiO 4The quality of film.Therefore, described magnesium oxide should not be the aggregate of single ultra tiny level magnesia particle, and should be the aggregate of the magnesia particle of various different-grain diameters, promptly should make the magnesia particle of various different-grain diameters respectively occupy certain allocation proportion.
Described magnesium oxide is to be exclusively used in the production of oriented silicon steel sheet, as the high temperature annealing separant, belongs to the fine inorganic chemical materials, and its preparation has unique method.The precipitator method such as bittern soda ash method, rhombspar carborization, bittern ammonium carbonate method are arranged about described preparation method of magnesia at present both at home and abroad.Although the described magnesium oxide with method for preparing has the advantage that purity is higher, particle size distribution is narrow, aforesaid method can not satisfy the requirement that high name oriented siliconized plate is produced.Adopt the oriented silicon steel sheet of aforesaid method production to influence oriented silicon steel sheet surface Mg because of producing high name oriented siliconized plate with extraordinary magnesium oxide 2SiO 4The formation of film, Mg 2SiO 4The reason that film does not form is to lack part high reactivity, fine magnesium oxide powder, and speed of response is slow, influences the quality of oriented silicon steel sheet.
Precipitator method MgCl 26H 2O and NH 4HCO 3Or Na 2CO 3Be the described magnesium oxide of feedstock production.With NH 4HCO 3Be raw material, the discharging of ammonia has pollution to environment; With Na 2CO 3Be raw material, preparation cost is too high; Sluggish precipitation is with MgCl 26H 2O and NH 3H 2O is a raw material, forms Mg (OH) 2Colloid, calcination at a certain temperature obtains described magnesium oxide, but in the whole technological process of synthetic magnesium oxide powder, colloid has the shortcoming that is difficult to filter, separate the removal of impurities difficulty.Thereby above-mentioned method is unsuitable for the described magnesium oxide of suitability for industrialized production.
Summary of the invention
The purpose of this invention is to provide a kind of preparation method of special magnesium oxide for grain-oriented silicon steel sheet.For realizing this purpose, the present invention adopts following technical scheme: under certain temperature condition, and the reaction of the mixture solution of magnesium compound solution and soda ash and caustic soda, generate the mixture of intermediate product magnesiumcarbonate and magnesium hydroxide, after filtration, washing, the drying, high-temperature calcination, pulverize, make
The extraordinary magnesium oxide of oriented silicon steel sheet.
Now describe technical scheme of the present invention in detail.A kind of preparation method of special magnesium oxide for grain-oriented silicon steel sheet is characterized in that, the concrete operations step:
The first step preparation contains the intermediate product of magnesiumcarbonate and magnesium hydroxide
Preparation soda ash and the caustic soda mixture aqueous solution and the magnesium compound aqueous solution, Na in soda ash and the caustic soda mixture aqueous solution + 1Concentration be 4mol/L, Mg in the magnesium compound aqueous solution + 2Concentration be 2mol/L, the Mg in the magnesium compound aqueous solution + 2With soda ash and the mol ratio of caustic soda, the i.e. Mg in soda ash and the caustic soda mixture aqueous solution + 2: soda ash: the mol ratio of caustic soda is 6.0: 5.0: 2.0, and soda ash and caustic soda mixture aqueous solution are added in the magnesium compound aqueous solution, stirs, and 20 ℃～80 ℃ were reacted 15 minutes～30 minutes down, obtain containing the intermediate product of magnesiumcarbonate and magnesium hydroxide;
The intermediate product of the second step filtration, washing, dried carbonaceous acid magnesium and magnesium hydroxide
The intermediate product that contains magnesiumcarbonate and magnesium hydroxide that the first step is made carries out vacuum suction filter, deionized water wash is gone into oven drying after vacuum suction filter is drained, and drying temperature is 80 ℃～120 ℃, be 1 hour～2 hours time of drying, obtains the intermediate product that exsiccant contains magnesiumcarbonate and magnesium hydroxide;
The 3rd step calcining exsiccant contains the intermediate product of magnesiumcarbonate and magnesium hydroxide, generates the extraordinary magnesium oxide of oriented silicon steel sheet
Calcine second down for 800 ℃～1000 ℃ and go on foot the intermediate product that the exsiccant that makes contains magnesiumcarbonate and magnesium hydroxide, calcination time is 2 hours～4 hours, pulverize calcinate, obtain the extraordinary magnesium oxide powder of product oriented silicon steel sheet, product yield is 95%, and the median size of product is between 1 μ m～2 μ m.
Technical scheme of the present invention is further characterized in that described magnesium compound is bittern magnesium chloride, solid-state magnesium chloride or sal epsom.
The advantage that the present invention has:
1, raw material used in the present invention is easy to get, and cost is low, and production technique is simple, and equipment requirements is low, is easy to realize industrialization.
2, the invention solves the separation impurities removal that generally prepares complexity in the extraordinary magnesium oxide process, also solved the easily problem of washing of intermediate product simultaneously by the liquid phase homogeneous precipitation method.
3, preparation technology is simple, the production efficiency height, in the production process product washing loss few, product yield is up to 95%.
4, the oriented silicon steel sheet of method of the present invention preparation is with the powder purity height of extraordinary magnesium oxide powder, and particle diameter is little, and median size has certain distribution range between 1 μ m～2 μ m.This advantage makes product of the present invention be particularly suitable for making slurries, is coated on oriented silicon steel sheet surface, and drying, high temperature annealing form Mg on oriented silicon steel sheet surface 2SiO 4Film.The purity height of product of the present invention, particle diameter is little, median size between 1 μ m～2 μ m, the chemically reactive height, guarantee when high temperature annealing product of the present invention can with the silicon dioxde reaction on oriented silicon steel sheet surface, form Mg 2SiO 4Film.The particle diameter of product of the present invention has certain distribution range, guarantees that the carbonic acid gas and the water vapour that produce when high temperature annealing can discharge smoothly, makes the Mg of formation 2SiO 4Film can be attached to the surface of oriented silicon steel sheet securely.
Embodiment
All embodiment all operate by the concrete operations step of technique scheme.Each embodiment is only enumerated the gordian technique data of each step.
Embodiment 1
In the first step, magnesium compound is the solid magnesium chloride, and 80 ℃ were reacted 15 minutes down; In second step, drying temperature is 80 ℃, and be 2 hours time of drying; In the 3rd step, 1000 ℃ of down the exsiccant magnesiumcarbonate that makes of second step of calcining and intermediate products of magnesium hydroxide, calcination time is 2 hours.
The product oriented silicon steel sheet of present embodiment with the median size of extraordinary magnesium oxide powder between 1 μ m～2 μ m.
The chemical reaction skeleton symbol relevant with present embodiment:
5MgCl 2+5Na 2CO 3+5H 2O＝4MgCO 3·Mg(OH) 2·4H 2O+CO 2+10NaCl
5Mg 2++5CO 3 2-+5H 2O→4MgCO 3·Mg(OH) 2·4H 2O+CO 2
MgCl 2+2NaOH＝Mg(OH) 2+2NaCl
Mg 2++2OH -→Mg(OH) 2
The left side explanation of following formula, the Mg in the magnesium compound aqueous solution + 2With the soda ash in soda ash and the caustic soda mixture aqueous solution and the mol ratio of caustic soda be 6.0: 5.0: 2.0;
(calcining)
4MgCO 3·Mg(OH) 2·4H 2O＝5MgO+4CO 2+5H 2O
(calcining)
Mg(OH) 2＝MgO+H 2O
Embodiment 2
Except for the following differences, all the other are all identical with embodiment 1.
In the first step, 50 ℃ were reacted 22 minutes down; In second step, drying temperature is 100 ℃, and be 1.5 hours time of drying; In the 3rd step, 900 ℃ of down the exsiccant magnesiumcarbonate that makes of second step of calcining and intermediate products of magnesium hydroxide, calcination time is 3 hours.
Embodiment 3
Except for the following differences, all the other are all identical with embodiment 1.
In the first step, 20 ℃ were reacted 30 minutes down; In second step, drying temperature is 120 ℃, and be 1 hour time of drying; In the 3rd step, 800 ℃ of down the exsiccant magnesiumcarbonate that makes of second step of calcining and intermediate products of magnesium hydroxide, calcination time is 4 hours.
Embodiment 4
Implementation process except for the following differences, all the other are all identical with embodiment 1.
In the first step, magnesium compound is the bittern magnesium chloride.
Embodiment 5
Implementation process except for the following differences, all the other are all identical with embodiment 2.
In the first step, magnesium compound is the bittern magnesium chloride.
Embodiment 6
Implementation process except for the following differences, all the other are all identical with embodiment 3.All the other are all with embodiment 3.
In the first step, magnesium compound is the bittern magnesium chloride.
Embodiment 7
Implementation process except for the following differences, all the other are all identical with embodiment 1.
In the first step, magnesium compound is a solid magnesium sulfate.
The chemical equation relevant with present embodiment:
5MgSO 4+5Na 2CO 3+5H 2O＝4MgCO 3·Mg(OH) 2·4H 2O+CO 2+5Na 2SO 4
MgSO 4+2NaOH＝Mg(OH) 2+Na 2SO 4，
The left side explanation of following formula, the Mg in the magnesium compound aqueous solution + 2With the soda ash in soda ash and the caustic soda mixture aqueous solution and the mol ratio of caustic soda be 6.0: 5.0: 2.0;
(calcining)
4MgCO 3·Mg(OH) 2·4H 2O＝5MgO+4CO 2+5H 2O。
(calcining)
Mg(OH) 2＝MgO+H 2O。
Embodiment 8
Implementation process except for the following differences, and is all identical with embodiment 2.
In the first step, magnesium compound is a solid magnesium sulfate.
Embodiment 9
Implementation process except for the following differences, and is all identical with embodiment 3.
In the first step, magnesium compound is a solid magnesium sulfate.
More than the using method of product of nine embodiment: earlier product is added the water making beating, make slurries, with coating machine slurries are coated on oriented silicon steel sheet surface, drying, high temperature annealing form Mg on oriented silicon steel sheet surface 2SiO 4Film.Because of in nine above-mentioned embodiment, the extraordinary magnesium oxide that magnesium compound and soda ash and caustic soda reaction generate contains the magnesian particle diameter more tiny particle of particle diameter ratio with existing precipitator method preparation, median size is between 1 μ m～2 μ m, certain distribution range is arranged, the magnesian high reactivity of small particle size guarantee when high temperature annealing magnesium oxide can with the silicon dioxde reaction on oriented silicon steel sheet surface, form Mg 2SiO 4Film, particle diameter have the extraordinary magnesium oxide of certain distribution range to guarantee that the carbonic acid gas and the water vapour that produce can discharge smoothly when high temperature annealing, make the Mg of formation 2SiO 4Film can be attached to the surface of oriented silicon steel sheet securely, has eliminated the thicker because of generating magnesian particle diameter of the existing precipitator method, and activity is not high, easily the Mg that produces 2SiO 4The shortcoming that film does not form.
Method of the present invention is particularly suitable for being used for preparing the extraordinary magnesium oxide that the oriented silicon steel sheet is used.

Claims (2)

1, a kind of preparation method of special magnesium oxide for grain-oriented silicon steel sheet is characterized in that, the concrete operations step:
The first step preparation contains the intermediate product of magnesiumcarbonate and magnesium hydroxide
Preparation soda ash and the caustic soda mixture aqueous solution and the magnesium compound aqueous solution, Na in soda ash and the caustic soda mixture aqueous solution + 1Concentration be 4mol/L, Mg in the magnesium compound aqueous solution + 2Concentration be 2mol/L, the Mg in the magnesium compound aqueous solution + 2With soda ash and the mol ratio of caustic soda, the i.e. Mg in soda ash and the caustic soda mixture aqueous solution + 2: soda ash: the mol ratio of caustic soda is 6.0: 5.0: 2.0, and soda ash and caustic soda mixture aqueous solution are added in the magnesium compound aqueous solution, stirs, and 20 ℃～80 ℃ were reacted 15 minutes～30 minutes down, obtain containing the intermediate product of magnesiumcarbonate and magnesium hydroxide;
The intermediate product of the second step filtration, washing, dried carbonaceous acid magnesium and magnesium hydroxide
The intermediate product that contains magnesiumcarbonate and magnesium hydroxide that the first step is made carries out vacuum suction filter, deionized water wash is gone into oven drying after vacuum suction filter is drained, and drying temperature is 80 ℃～120 ℃, be 1 hour～2 hours time of drying, obtains the intermediate product that exsiccant contains magnesiumcarbonate and magnesium hydroxide;
The 3rd step calcining exsiccant contains the intermediate product of magnesiumcarbonate and magnesium hydroxide, generates the extraordinary magnesium oxide of oriented silicon steel sheet
Calcine second down for 800 ℃～1000 ℃ and go on foot the intermediate product that the exsiccant that makes contains magnesiumcarbonate and magnesium hydroxide, calcination time is 2 hours～4 hours, pulverize calcinate, obtain the extraordinary magnesium oxide powder of product oriented silicon steel sheet, product yield is 95%, and the median size of product is between 1 μ m～2 μ m.
2, preparation method of special magnesium oxide for grain-oriented silicon steel sheet according to claim 1 is characterized in that, described magnesium compound is bittern magnesium chloride, solid-state magnesium chloride or sal epsom.
CN2009101947328A 2009-08-28 2009-08-28 Preparation method of special magnesium oxide for grain-oriented silicon steel sheet Active CN101643227B (en)

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Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102407210A (en) * 2010-09-21 2012-04-11 鞍钢股份有限公司 MgO coating control method and device for medium and small oriented silicon steel decarburization annealing line
CN104528776A (en) * 2014-12-16 2015-04-22 中国科学院青海盐湖研究所 Preparation method of active magnesium oxide
CN107032373A (en) * 2017-05-22 2017-08-11 河北镁神科技有限公司 A kind of tooth family alginate impression material combined oxidation magnesium raw powder's production technology

Cited By (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102407210A (en) * 2010-09-21 2012-04-11 鞍钢股份有限公司 MgO coating control method and device for medium and small oriented silicon steel decarburization annealing line
CN102407210B (en) * 2010-09-21 2013-10-16 鞍钢股份有限公司 MgO coating control method and device for medium and small oriented silicon steel decarburization annealing line
CN104528776A (en) * 2014-12-16 2015-04-22 中国科学院青海盐湖研究所 Preparation method of active magnesium oxide
CN107032373A (en) * 2017-05-22 2017-08-11 河北镁神科技有限公司 A kind of tooth family alginate impression material combined oxidation magnesium raw powder's production technology
CN107032373B (en) * 2017-05-22 2019-03-01 河北镁神科技股份有限公司 A kind of tooth family alginate impression material combined oxidation magnesium raw powder's production technology

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