CN101891219B - Method for preparing special magnesium borate for oriented silicon steel - Google Patents
Method for preparing special magnesium borate for oriented silicon steel Download PDFInfo
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- CN101891219B CN101891219B CN2010102592405A CN201010259240A CN101891219B CN 101891219 B CN101891219 B CN 101891219B CN 2010102592405 A CN2010102592405 A CN 2010102592405A CN 201010259240 A CN201010259240 A CN 201010259240A CN 101891219 B CN101891219 B CN 101891219B
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Abstract
The invention relates to the field of oriented silicon steel plate manufacture, in particular to a method for preparing special magnesium borate for oriented silicon steel. The method solves the problems of poor adhesion, dispersibility and electromagnetic performance and the like of the conventional boron aid. The method comprises the following steps of: (1) pouring aqueous solution of magnesium bicarbonate and boric acid in a ratio into a reaction kettle; (2) performing sedimentation treatment on the mixed solution; (3) then conveying the sediment into a pyrolysis tank, adding finished magnesium borate crystal seeds and silane coupling agent into the pyrolysis tank, and producing a mixture of nano magnesium carbonate and metaboric acid by using a liquid phase precipitation method; (4) filter-pressing the pyrolysis product to obtain filter cakes; (5) treating the filter cakes in a high-temperature crystal oven to form nano magnesium borate powder with complete crystal; and (6) grading the material discharged out of the high-temperature crystal oven with jet milling to obtain a screened substance of less than or equal to 320 meshes. All indexes of the special magnesium borate are superior to that of the primary product, and in particular, the adhesion, dispersibility and electromagnetic performance are remarkably improved, and the quality of the oriented silicon steel plate is improved; and the method has the advantages of simple production process, lower cost and no three-waste pollution.
Description
Technical field
The present invention relates to the oriented silicon steel sheet and make the field, be specially a kind of preparation method of special magnesium borate for oriented silicon steel.
Background technology
The oriented silicon steel sheet in order to increase the synthesising reacting speed of silicon-dioxide and silicon-steel magnesium oxide in the steel plate, improves the sticking power and the electromagnetic performance of underlayer insulating film layer Magnesium Silicate q-agent in manufacturing processed.Oriented silicon steel sheet manufacturing firm generally adopts boron additive both at home and abroad at present; The boron ion can suppress the conduction of iron atom in the oriented silicon steel sheet; And then insulation resistance, the electromagnetic performance of raising siliconized plate; Can effectively reduce the fusing point of silicon-dioxide and silicon steel level Natural manganese dioxide high temperature synthetic magnesium silicate insulating film layer in the siliconized plate, can generate the volatility salt with harmful ion such as sodium ion reaction.At present; Boron be introduced as two types: a boron content for self containing in the silicon-steel magnesium oxide; Two for adding the boron magnesium compound, and both all exist, and the boron ion is soluble in water, enhancing Magnesium Silicate q-agent insulation book film properties is poor, become the key subjects of present raising oriented silicon steel tablet quality.
The current domestic and international method for preparing nano boric acid magnesium mainly contains high temperature solid-state method, microwave solid phase method and sol-gel method.The raw material that adopts is magnesium chloride and boric acid, or magnesium nitrate, boric acid and Hydrocerol A are raw material.As everyone knows, nano boric acid magnesium is mainly at aerospace material, building, machinery, automobile, aluminium, magnesium, and alloy in and use as enhancement additive in the engineering plastics.This product is as being applied to the oriented silicon steel sheet, also has shortcomings such as poor adhesive force, dispersing property are poor, electromagnetic performance difference.Current domestic oriented silicon steel sheet top coat sticking power is generally in the C-E level, and insulation resistance is about 50 Ω, and the trade mark is basically at 30QG120.Along with the requirement of end product X-former improves constantly, conventional oriented steel can not be used in some engineering field therefore.From oriented silicon steel sheet manufacturing processed, through adding extraordinary boron additive, improving the siliconized plate quality and the trade mark is the major issue that needs to be resolved hurrily at present.
Summary of the invention
There are problems such as poor adhesive force, dispersing property are poor, electromagnetic performance difference in the present invention in order to solve in the existing oriented silicon steel manufacturing boron additive product in practical application, a kind of preparation method of special magnesium borate for oriented silicon steel is provided.
The present invention adopts following technical scheme to realize: a kind of preparation method of special magnesium borate for oriented silicon steel comprises following process step:
(1) raw materials mix: will contain the magnesian Magnesium hydrogen carbonate aqueous solution input of 7.0 ~ 7.5g/L reaction kettle; Open and stir; Then with boric acid according to magnesian part by weight be that the ratio of 1.8 ~ 2.0 : 1 is poured reaction kettle into, stirring velocity is that PM 120 ~ 140 changes, temperature of reaction kettle is 5 ~ 30 ℃; Churning time is 1.0 ~ 2.0h, obtains raw materials mix liquid;
(2) deposition: raw materials mix liquid is carried out precipitation process, and the ST is 30 ~ 60 minutes; After two kinds of raw materials mix, possibly have few portion water insolubles or Magnesium hydrogen carbonate crystal and separate out, so be removed through post precipitation;
(3) pyrolysis: with the mixed solution input pyrolytic tank of post precipitation; Add the magnesium borate finished product crystal seed that accounts for raw materials mix liquid gross weight 2 ~ 5%; And then interpolation accounts for raw materials mix liquid gross weight 0.2 ~ 0.5%KH-570 silane coupling agent; In 95 ~ 100 ℃, the liquid-phase precipitation method processing condition of 15 ~ 20 minutes time are produced sodium rice magnesiumcarbonate and metaboric acid mixture with steam; The effect of adding a small amount of magnesium borate finished product crystal seed is the complete in crystal formation that guarantees the finished product; The KH-570 silane coupling agent is existing known products, and chemical name is the 3-methacryloxypropyl trimethoxy silane, trade(brand)name: KH-570; Main effect is the physical strength that can significantly improve matrix material; Increase electric property, above-mentioned liquid-phase precipitation method is existing public technology, and liquid phase method is to select one or more suitable soluble metal salts; Form metering by prepared material and be mixed with solution; Make each element be the lewis' acid attitude, select a kind of suitable precipitation agent again or, make the metals ion precipitation from homogeneous solution or crystallize out with operations such as evaporation, distillation, hydrolysis; To precipitate at last or crystalline dehydration or thermal degradation and obtain the material requested powder, those of ordinary skills can become the nanometer grade powder that contains little water with the solution that contains Magnesium hydrogen carbonate and boric acid fully;
(4) filter: pyrolysis product is carried out press filtration in pressure filter, obtain water cut and be 65 ~ 80% filter cake (water cut according to the invention is a mass percent), the softening water flushing is adopted in press filtration, and filter cake reacts synthetic through transfer roller to the high temperature crystallization stove; Waste water is through settling tank, neutralization tank, and circulation is used for the press filtration wash water after the IX, reduces pollutant emission;
(5) high temperature crystallization: the filter cake that will contain nano-calcium carbonate magnesium and metaboric acid is handled in the high temperature crystallization stove, and treatment step is as follows: the first step: temperature section is at 250 ~ 300 ℃, metaboric acid HBO
2Resolve into boron trioxide B
2O
3, magnesiumcarbonate is undecomposed, and becoming water cut is the powder shaped below 1%; Second step: temperature section is at 450 ~ 500 ℃, boron trioxide B
2O
3Begin fusing; The 3rd step: temperature section is at 800 ~ 850 ℃, and magnesiumcarbonate resolves into Natural manganese dioxide, is evenly dispersed in fused boron trioxide B
2O
3In the drop, form the intact sodium rice magnesium borate powder of crystal, generated time is 2.0h ~ 4.0h; This step main chemical reactions formula is as follows:
Mg（HCO
3）
2→MgCO
3+H
2O+CO
2↑ （1）
MgCO
3→MgO+?CO
2↑ （2）
H
3BO
3→B
2O
3+3H
2O （3）
2MgO+B
2O
3→Mg
2B
2O
5 （4）
(6) powder handling: the material that the high temperature crystallization stove is come out is handled with grading machine under airflow milling, obtains≤320 purpose screen underflows, is special magnesium borate for oriented silicon steel of the present invention.Usually control screenings≤0.1% is promptly qualified.
Optimised process step of the present invention is following:
(1) raw materials mix: will contain the magnesian Magnesium hydrogen carbonate aqueous solution input of 7.3g/L reaction kettle; Open and stir; Then with boric acid according to magnesian part by weight be that the ratio of 1.9 : 1 is poured reaction kettle into, stirring velocity is that PM 120 ~ 140 changes, temperature of reaction kettle is 15 ℃; Churning time is 1.5h, obtains raw materials mix liquid; (2) deposition: raw materials mix liquid is carried out precipitation process, and the ST is 45 minutes; (3) pyrolysis: with the mixed solution input pyrolytic tank of post precipitation; Add the magnesium borate finished product crystal seed that accounts for raw materials mix liquid gross weight 3.5%; And then interpolation accounts for raw materials mix liquid gross weight 0.35%KH-570 silane coupling agent; In 98 ℃, the liquid-phase precipitation method processing condition of 17 minutes time are produced sodium rice magnesiumcarbonate and metaboric acid mixture with steam; (4) filter: pyrolysis product is carried out press filtration in pressure filter, obtain water cut and be 70% filter cake, the softening water flushing is adopted in press filtration, and filter cake reacts synthetic through transfer roller to the high temperature crystallization stove; (5) high temperature crystallization: the filter cake that will contain nano-calcium carbonate magnesium and metaboric acid is handled in the high temperature crystallization stove, and treatment step is as follows: the first step: temperature section is at 280 ℃, metaboric acid HBO
2Resolve into boron trioxide B
2O
3, magnesiumcarbonate is undecomposed, and becoming water cut is the powder shaped below 1%; Second step: temperature section is at 480 ℃, boron trioxide B
2O
3Begin fusing; The 3rd step: temperature section is at 825 ℃, and magnesiumcarbonate resolves into Natural manganese dioxide, is evenly dispersed in fused boron trioxide B
2O
3In the drop, form the intact sodium rice magnesium borate powder of crystal, generated time is 3.0h; (6) powder handling: the material that the high temperature crystallization stove is come out is handled with grading machine under airflow milling, obtains≤320 purpose screen underflows, is special magnesium borate for oriented silicon steel of the present invention.
Used equipment is existing known products in the above-mentioned steps; Wherein reaction kettle, pyrolysis filling, high temperature crystallization stove and airflow milling are the present invention's process test of many times; The equipment that preferably comes out cooperatively interacts with technology according to the invention, can improve performance of products greatly.
Used softening water is a reverse-osmosis treated water in the above-mentioned steps (4), and its specific conductivity≤10 μ s/cm guarantees that with this solubility salt increases solubleness.
Special magnesium borate for oriented silicon steel of the present invention prepares raw material and raising oriented silicon steel quality mechanism is described below:
1, raw material
Magnesium hydrogen carbonate: molecular formula Mg (HCO
3)
2, molecular weight 146.30
Boric acid: molecular formula H
3BO
3, molecular weight 61.84
KH-570 silane coupling agent: chemical name 3-methacryloxypropyl trimethoxy silane
2, improve oriented silicon steel tablet quality mechanism
Because the radius little (being about 0.85～0.90) of boron atom and high ionization energy (the first ionizing potential 8.296eV), determined the covalency of boron atomic bonding, thereby the boron atom can not resemble the atoms metal employing metallic bond when forming simple substance.The covalency of boron atom and valence electron number thereof are less than the characteristics of valency layer track number; Also determined the boron atom forming the monokaryon compound (like BX3; X represents F, Cl, Br, I, OH etc.) in, center boron atom is 6 electronic structures normally, i.e. 2s2,2px2,2py2,2pz0.Belong to " electron-deficient compounds ".Electron-deficient compounds has the very strong ability of accepting electronics, shows on the chemical property it is to form the aggretion type molecule easily, also forms stable coordination compound with the electron pair donor easily, so can effectively constrain iron atom and other ionic conduction; The boric acid characteristic can reduce the fusing point of SiO2 and MgO in addition, promotes synthesising reacting speed; These article are nano-powder, have good dispersiveness; These article granularity is little and viscosity is high, has good tack.
Processing condition are analyzed:
A, Magnesium hydrogen carbonate, boric acid, KH-570 weight ratio: the boric acid ratio is big, and then the product yield is low and filtration velocity is slow, and the little crystal (fibrous) that then influences product is intact.In this optimal process Magnesium hydrogen carbonate in Natural manganese dioxide (7-7.5g//L) and boric acid than being 1:1.8 ~ 2.0, KH-570 is 0.2 ~ 0.5% a proportioning optimised process of above-mentioned gross weight.
The selection of B, pyrolytic process condition: the Magnesium hydrogen carbonate pyrolysis temperature is low, and then the product yield is few; Pyrolysis temperature is high more, and then the powder product granularity is thicker.The bonded products characteristic prepares requirement, and in 95 ~ 100 ℃, the pyrolytical condition of time 15 ~ 20min is an optimised process to this optimal process with steam.
C, high temperature crystallization Selection of technological conditions: the high temperature crystallization temperature is high more, and then product granularity becomes big, and viscosity reduces; Temperature is low more, and then chemical purity reduces.800 ~ 850 ℃ of this optimal process temperature, time 2.0h ~ 4.0h is the high temperature crystallization optimised process.
By special magnesium borate for oriented silicon steel metallurgic product quality monitoring testing station check through Hubei Province that preparation method of the present invention makes, the detected result of gained sees shown in the table 1 that its examining report sees Appendix 1, and name is called survey report:
| Sequence number | Interventions Requested | Unit | Assay |
| 1 | Natural manganese dioxide (MgO) content | % | ? 52.98 |
| 2 | Boron trioxide (B 2O 3) content | % | ? 46.35 |
| 3 | Muriate (Cl -) content | % | ?0.03 |
| 4 | Vitriol (SO 4 2-) content | % | ?0.10 |
| 5 | Iron (Fe 3+) content | % | ? 0.05 |
| 6 | Screen underflow (320 order) | % | ? 0.056 |
| 7 | The granularity footpath | nm | 6-30 |
| 8 | Crystalline structure | — | Fibrous |
| 9 | Settling velocity | mm/h | 5 |
In addition the special magnesium borate for oriented silicon steel use properties is also checked, assay shows: sticking power is the B level, and iron loss is less than 1W/Kg, and magneticflux-density is greater than 1.930T, and interlamination resistance is greater than 350 Ω
In addition, the present invention entrusts Wuhan Iron and Steel Plant research institute silicon steel that oriented silicon steel used additives nano boric acid magnesium is tested in order to verify the effect of this special magnesium borate for oriented silicon steel in practical application.Analyze to report and show that in the manufacturing of oriented silicon steel sheet, add special magnesium borate for oriented silicon steel, with the boron magnesium compound auxiliary agent contrast of routine, it is even to generate the bottom appearance color, does not reveal brilliant phenomenon; Tack is good; Magnetic property is superior to the on-the-spot boron magnesium compound that uses.Concrete outcome is seen table 2:
| Project | Unit | This project product index | The online product index of Wuhan Iron and Steel Plant |
| MgO | % | 52.98 | 49.82 |
| B 2O 3 | % | 46.35 | 42.14 |
| Cl | % | 0.03 | 0.06 |
| SO 4 | % | 0.10 | 0.23 |
| Fe | % | 0.05 | 0.08 |
| Screenings (320 order) | % | 0.056 | 0.067 |
| Particle diameter | nm | 6~30 | 50~2000 |
| Crystalline structure | ? | Fibrous | Spherical |
| Settling velocity | mm/h | 5 | 60 |
In a word, compared with prior art, the present invention utilizes Magnesium hydrogen carbonate, boric acid, the KH-570 special magnesium borate for oriented silicon steel for raw material production; Its each item index all is superior to existing product, and especially sticking power, dispersing property, electromagnetic performance are significantly increased, and has improved the quality of oriented silicon steel sheet greatly; And production technique is simple; Cost is lower, and three-waste free pollution meets the national environmental protection policy requirements.
Embodiment
Embodiment 1:
A kind of preparation method of special magnesium borate for oriented silicon steel; Comprise following process step: (1) raw materials mix: will contain the magnesian Magnesium hydrogen carbonate aqueous solution of 7.0g/L input reaction kettle, and open and stir, then with boric acid according to magnesian part by weight be that the ratio of 1.8 : 1 is poured reaction kettle into; Stirring velocity is that PM 120 changes; Temperature of reaction kettle is 5 ℃, and churning time is 1.0h, obtains raw materials mix liquid; (2) deposition: raw materials mix liquid is carried out precipitation process, and the ST is 30 minutes; (3) pyrolysis: with the mixed solution input pyrolytic tank of post precipitation; Add the magnesium borate finished product crystal seed that accounts for raw materials mix liquid gross weight 2%; And then interpolation accounts for raw materials mix liquid gross weight 0.2%KH-570 silane coupling agent; In 95 ℃, the liquid-phase precipitation method processing condition of 15 minutes time are produced sodium rice magnesiumcarbonate and metaboric acid mixture with steam; (4) filter: pyrolysis product is carried out press filtration in pressure filter; Obtain water cut and be 65% filter cake, the softening water flushing is adopted in press filtration, and filter cake reacts synthetic through transfer roller to the high temperature crystallization stove; Used softening water is a reverse-osmosis treated water, its specific conductivity≤10 μ s/cm; (5) high temperature crystallization: the filter cake that will contain nano-calcium carbonate magnesium and metaboric acid is handled in the high temperature crystallization stove, and treatment step is as follows: the first step: temperature section is at 250 ℃, metaboric acid HBO
2Resolve into boron trioxide B
2O
3, magnesiumcarbonate is undecomposed, and becoming water cut is the powder shaped below 1%; Second step: temperature section is at 450 ℃, boron trioxide B
2O
3Begin fusing; The 3rd step: temperature section is at 800 ℃, and magnesiumcarbonate resolves into Natural manganese dioxide, is evenly dispersed in fused boron trioxide B
2O
3In the drop, form the intact sodium rice magnesium borate powder of crystal, generated time is 2.0hh; (6) powder handling: the material that the high temperature crystallization stove is come out is handled with grading machine under airflow milling, obtains≤320 purpose screen underflows, is special magnesium borate for oriented silicon steel of the present invention.
Embodiment 2:
A kind of preparation method of special magnesium borate for oriented silicon steel; Comprise following process step: (1) raw materials mix: will contain the magnesian Magnesium hydrogen carbonate aqueous solution of 7.5g/L input reaction kettle, and open and stir, then with boric acid according to magnesian part by weight be that the ratio of 2.0 : 1 is poured reaction kettle into; Stirring velocity is that PM 140 changes; Temperature of reaction kettle is 30 ℃, and churning time is 2.0h, obtains raw materials mix liquid; (2) deposition: raw materials mix liquid is carried out precipitation process, and the ST is 60 minutes; (3) pyrolysis: with the mixed solution input pyrolytic tank of post precipitation; Add the magnesium borate finished product crystal seed that accounts for raw materials mix liquid gross weight 5%; And then interpolation accounts for raw materials mix liquid gross weight 0.5%KH-570 silane coupling agent; In 100 ℃, the liquid-phase precipitation method processing condition of 20 minutes time are produced sodium rice magnesiumcarbonate and metaboric acid mixture with steam; (4) filter: pyrolysis product is carried out press filtration in pressure filter; Obtain water cut and be 80% filter cake, the softening water flushing is adopted in press filtration, and filter cake reacts synthetic through transfer roller to the high temperature crystallization stove; Used softening water is a reverse-osmosis treated water, its specific conductivity≤10 μ s/cm; (5) high temperature crystallization: the filter cake that will contain nano-calcium carbonate magnesium and metaboric acid is handled in the high temperature crystallization stove, and treatment step is as follows: the first step: temperature section is at 300 ℃, metaboric acid HBO
2Resolve into boron trioxide B
2O
3, magnesiumcarbonate is undecomposed, and becoming water cut is the powder shaped below 1%; Second step: temperature section is at 500 ℃, boron trioxide B
2O
3Begin fusing; The 3rd step: temperature section is at 850 ℃, and magnesiumcarbonate resolves into Natural manganese dioxide, is evenly dispersed in fused boron trioxide B
2O
3In the drop, form the intact sodium rice magnesium borate powder of crystal, generated time is 4.0h; (6) powder handling: the material that the high temperature crystallization stove is come out is handled with grading machine under airflow milling, obtains≤320 purpose screen underflows, is special magnesium borate for oriented silicon steel of the present invention.
Embodiment 3:
A kind of preparation method of special magnesium borate for oriented silicon steel; Comprise following process step: (1) raw materials mix: will contain the magnesian Magnesium hydrogen carbonate aqueous solution of 7.3g/L input reaction kettle, and open and stir, then with boric acid according to magnesian part by weight be that the ratio of 1.9 : 1 is poured reaction kettle into; Stirring velocity is that PM 120 ~ 140 changes; Temperature of reaction kettle is 15 ℃, and churning time is 1.5h, obtains raw materials mix liquid; (2) deposition: raw materials mix liquid is carried out precipitation process, and the ST is 45 minutes; (3) pyrolysis: with the mixed solution input pyrolytic tank of post precipitation; Add the magnesium borate finished product crystal seed that accounts for raw materials mix liquid gross weight 3.5%; And then interpolation accounts for raw materials mix liquid gross weight 0.35%KH-570 silane coupling agent; In 98 ℃, the liquid-phase precipitation method processing condition of 17 minutes time are produced sodium rice magnesiumcarbonate and metaboric acid mixture with steam; (4) filter: pyrolysis product is carried out press filtration in pressure filter; Obtain water cut and be 70% filter cake, the softening water flushing is adopted in press filtration, and filter cake reacts synthetic through transfer roller to the high temperature crystallization stove; Used softening water is a reverse-osmosis treated water, its specific conductivity≤10 μ s/cm; (5) high temperature crystallization: the filter cake that will contain nano-calcium carbonate magnesium and metaboric acid is handled in the high temperature crystallization stove, and treatment step is as follows: the first step: temperature section is at 280 ℃, metaboric acid HBO
2Resolve into boron trioxide B
2O
3, magnesiumcarbonate is undecomposed, and becoming water cut is the powder shaped below 1%; Second step: temperature section is at 480 ℃, boron trioxide B
2O
3Begin fusing; The 3rd step: temperature section is at 825 ℃, and magnesiumcarbonate resolves into Natural manganese dioxide, is evenly dispersed in fused boron trioxide B
2O
3In the drop, form the intact sodium rice magnesium borate powder of crystal, generated time is 3.0h; (6) powder handling: the material that the high temperature crystallization stove is come out is handled with grading machine under airflow milling, obtains≤320 purpose screen underflows, is special magnesium borate for oriented silicon steel of the present invention.
Embodiment 4:
A kind of preparation method of special magnesium borate for oriented silicon steel; Comprise following process step: (1) raw materials mix: will contain the magnesian Magnesium hydrogen carbonate aqueous solution of 7.5g/L input reaction kettle, and open and stir, then with boric acid according to magnesian part by weight be that the ratio of 2.0 : 1 is poured reaction kettle into; Stirring velocity is that PM 120 changes; Temperature of reaction kettle is 5 ℃, and churning time is 1.0h, obtains raw materials mix liquid; (2) deposition: raw materials mix liquid is carried out precipitation process, and the ST is 60 minutes; (3) pyrolysis: with the mixed solution input pyrolytic tank of post precipitation; Add the magnesium borate finished product crystal seed that accounts for raw materials mix liquid gross weight 4%; And then interpolation accounts for raw materials mix liquid gross weight 0.4%KH-570 silane coupling agent; In 100 ℃, the liquid-phase precipitation method processing condition of 15 minutes time are produced sodium rice magnesiumcarbonate and metaboric acid mixture with steam; (4) filter: pyrolysis product is carried out press filtration in pressure filter; Obtain water cut and be 68% filter cake, the softening water flushing is adopted in press filtration, and filter cake reacts synthetic through transfer roller to the high temperature crystallization stove; Used softening water is a reverse-osmosis treated water, its specific conductivity≤10 μ s/cm; (5) high temperature crystallization: the filter cake that will contain nano-calcium carbonate magnesium and metaboric acid is handled in the high temperature crystallization stove, and treatment step is as follows: the first step: temperature section is at 300 ℃, metaboric acid HBO
2Resolve into boron trioxide B
2O
3, magnesiumcarbonate is undecomposed, and becoming water cut is the powder shaped below 1%; Second step: temperature section is at 450 ℃, boron trioxide B
2O
3Begin fusing; The 3rd step: temperature section is at 840 ℃, and magnesiumcarbonate resolves into Natural manganese dioxide, is evenly dispersed in fused boron trioxide B
2O
3In the drop, form the intact sodium rice magnesium borate powder of crystal, generated time is 2.5h; (6) powder handling: the material that the high temperature crystallization stove is come out is handled with grading machine under airflow milling, obtains≤320 purpose screen underflows, is special magnesium borate for oriented silicon steel of the present invention.
Embodiment 5:
A kind of preparation method of special magnesium borate for oriented silicon steel; Comprise following process step: (1) raw materials mix: will contain the magnesian Magnesium hydrogen carbonate aqueous solution of 7.2g/L input reaction kettle, and open and stir, then with boric acid according to magnesian part by weight be that the ratio of 1.8 : 1 is poured reaction kettle into; Stirring velocity is that PM 120 ~ 140 changes; Temperature of reaction kettle is 25 ℃, and churning time is 1.8h, obtains raw materials mix liquid; (2) deposition: raw materials mix liquid is carried out precipitation process, and the ST is 40 minutes; (3) pyrolysis: with the mixed solution input pyrolytic tank of post precipitation; Add the magnesium borate finished product crystal seed that accounts for raw materials mix liquid gross weight 3%; And then interpolation accounts for raw materials mix liquid gross weight 0.4%KH-570 silane coupling agent; In 96 ℃, the liquid-phase precipitation method processing condition of 18 minutes time are produced sodium rice magnesiumcarbonate and metaboric acid mixture with steam; (4) filter: pyrolysis product is carried out press filtration in pressure filter; Obtain water cut and be 75% filter cake, the softening water flushing is adopted in press filtration, and filter cake reacts synthetic through transfer roller to the high temperature crystallization stove; Used softening water is a reverse-osmosis treated water, its specific conductivity≤10 μ s/cm; (5) high temperature crystallization: the filter cake that will contain nano-calcium carbonate magnesium and metaboric acid is handled in the high temperature crystallization stove, and treatment step is as follows: the first step: temperature section is at 265 ℃, metaboric acid HBO
2Resolve into boron trioxide B
2O
3, magnesiumcarbonate is undecomposed, and becoming water cut is the powder shaped below 1%; Second step: temperature section is at 470 ℃, boron trioxide B
2O
3Begin fusing; The 3rd step: temperature section is at 830 ℃, and magnesiumcarbonate resolves into Natural manganese dioxide, is evenly dispersed in fused boron trioxide B
2O
3In the drop, form the intact sodium rice magnesium borate powder of crystal, generated time is 2.5h; (6) powder handling: the material that the high temperature crystallization stove is come out is handled with grading machine under airflow milling, obtains≤320 purpose screen underflows, is special magnesium borate for oriented silicon steel of the present invention.
Claims (3)
1. the preparation method of a special magnesium borate for oriented silicon steel is characterized in that comprising following process step:
(1) raw materials mix: will contain the magnesian Magnesium hydrogen carbonate aqueous solution input of 7.0 ~ 7.5g/L reaction kettle; Open and stir; Then with boric acid according to magnesian part by weight be that the ratio of 1.8 ~ 2.0 : 1 is poured reaction kettle into, stirring velocity is that PM 120 ~ 140 changes, temperature of reaction kettle is 5 ~ 30 ℃; Churning time is 1.0 ~ 2.0h, obtains raw materials mix liquid;
(2) deposition: raw materials mix liquid is carried out precipitation process, and the ST is 30 ~ 60 minutes;
(3) pyrolysis: with the mixed solution input pyrolytic tank of post precipitation; Add the magnesium borate finished product crystal seed that accounts for raw materials mix liquid gross weight 2 ~ 5%; And then interpolation accounts for raw materials mix liquid gross weight 0.2 ~ 0.5%KH-570 silane coupling agent; In 95 ~ 100 ℃, the liquid-phase precipitation method processing condition of 15 ~ 20 minutes time are produced sodium rice magnesiumcarbonate and metaboric acid mixture with steam;
(4) filter: pyrolysis product is carried out press filtration in pressure filter, obtain water cut and be 65 ~ 80% filter cake, the softening water flushing is adopted in press filtration, and filter cake reacts synthetic through transfer roller to the high temperature crystallization stove;
(5) high temperature crystallization: the filter cake that will contain nano-calcium carbonate magnesium and metaboric acid is handled in the high temperature crystallization stove, and treatment step is as follows:
The first step: temperature section is at 250 ~ 300 ℃, metaboric acid HBO
2Resolve into boron trioxide B
2O
3, magnesiumcarbonate is undecomposed, and becoming water cut is the powder shaped below 1%;
Second step: temperature section is at 450 ~ 500 ℃, boron trioxide B
2O
3Begin fusing;
The 3rd step: temperature section is at 800 ~ 850 ℃, and magnesiumcarbonate resolves into Natural manganese dioxide, is evenly dispersed in fused boron trioxide B
2O
3In the drop, form the intact sodium rice magnesium borate powder of crystal, generated time is 2.0h ~ 4.0h;
(6) powder handling: the material that the high temperature crystallization stove is come out is handled with grading machine under airflow milling, obtains≤320 purpose screen underflows, is described special magnesium borate for oriented silicon steel.
2. the preparation method of a kind of special magnesium borate for oriented silicon steel according to claim 1 is characterized in that comprising following process step:
(1) raw materials mix: will contain the magnesian Magnesium hydrogen carbonate aqueous solution input of 7.3g/L reaction kettle; Open and stir; Then with boric acid according to magnesian part by weight be that the ratio of 1.9 : 1 is poured reaction kettle into, stirring velocity is that PM 120 ~ 140 changes, temperature of reaction kettle is 15 ℃; Churning time is 1.5h, obtains raw materials mix liquid;
(2) deposition: raw materials mix liquid is carried out precipitation process, and the ST is 45 minutes;
(3) pyrolysis: with the mixed solution input pyrolytic tank of post precipitation; Add the magnesium borate finished product crystal seed that accounts for raw materials mix liquid gross weight 3.5%; And then interpolation accounts for raw materials mix liquid gross weight 0.35%KH-570 silane coupling agent; In 98 ℃, the liquid-phase precipitation method processing condition of 17 minutes time are produced sodium rice magnesiumcarbonate and metaboric acid mixture with steam;
(4) filter: pyrolysis product is carried out press filtration in pressure filter, obtain water cut and be 70% filter cake, the softening water flushing is adopted in press filtration, and filter cake reacts synthetic through transfer roller to the high temperature crystallization stove;
(5) high temperature crystallization: the filter cake that will contain nano-calcium carbonate magnesium and metaboric acid is handled in the high temperature crystallization stove, and treatment step is as follows:
The first step: temperature section is at 280 ℃, metaboric acid HBO
2Resolve into boron trioxide B
2O
3, magnesiumcarbonate is undecomposed, and becoming water cut is the powder shaped below 1%;
Second step: temperature section is at 480 ℃, boron trioxide B
2O
3Begin fusing;
The 3rd step: temperature section is at 825 ℃, and magnesiumcarbonate resolves into Natural manganese dioxide, is evenly dispersed in fused boron trioxide B
2O
3In the drop, form the intact sodium rice magnesium borate powder of crystal, generated time is 3.0h;
(6) powder handling: the material that the high temperature crystallization stove is come out is handled with grading machine under airflow milling, obtains≤320 purpose screen underflows, is described special magnesium borate for oriented silicon steel.
3. the preparation method of a kind of special magnesium borate for oriented silicon steel according to claim 1 and 2 is characterized in that softening water used in the step (4) is a reverse-osmosis treated water, its specific conductivity≤10 μ s/cm.
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| CN101177274A (en) * | 2007-11-20 | 2008-05-14 | 大连理工大学 | Method for hydrothermal synthesis of magnesium borate |
| CN101696017A (en) * | 2009-09-30 | 2010-04-21 | 河南理工大学 | Method for preparing magnesium hexaborate |
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| CN101177274A (en) * | 2007-11-20 | 2008-05-14 | 大连理工大学 | Method for hydrothermal synthesis of magnesium borate |
| CN101696017A (en) * | 2009-09-30 | 2010-04-21 | 河南理工大学 | Method for preparing magnesium hexaborate |
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