CN103466648A - Cleaner production method for preparing superfine powder through self-propagating metallurgy method - Google Patents
Cleaner production method for preparing superfine powder through self-propagating metallurgy method Download PDFInfo
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Abstract
A cleaner production method for preparing superfine powder through a self-propagating metallurgy method is carried out according to the following steps: (1) mixing and conducting ball-milling on the powdery oxide and magnesium powder, then compacting into a blank, putting the blank into a self-propagating reaction furnace to cause a self-propagating reaction, and naturally cooling to the room temperature to obtain a coarse product; (2) using hydrochloric acid to leach and separate magnesium oxide in the coarse product after breaking, and filtering to obtain a solid phase and a leaching agent; (3) washing and drying the solid phase and making the solid phase into ultrafine powder; (4) processing the leaching agent through a spray-pyrolysis mode to obtain a nanoscale magnesium oxide and pyrolysis tail gas, wherein the hydrogen chloride in the pyrolysis tail gas is absorbed to form hydrochloric acid and is circularly used back in the leaching process. The cleaner production method producing the ultrafine powder through the self-propagating metallurgy mode has the characteristics of low material cost, low energy consumption, simple operation, low requirement on process conditions and the like, and the product is high in purity, small in particle size and high in powder activity.
Description
Technical field
The invention belongs to metallurgical technology field, particularly the clean preparation method of the standby superfine powder of a kind of self-spreading metallurgical legal system.
Background technology
The superfine powder technology of preparing is to follow modern high technology and new material industry, the new engineering grown up as microelectronics and information technology, high-performance ceramics and refractory materials, polymer composites materials, biochemical industry, aerospace, new forms of energy etc. and conventional industries technical progress and comprehensive utilization of resources and deep processing etc., be an emerging integrated technology science, significant to the development of modern high technology industry.
The technology of preparing of superfine powder from large scope can be divided into the current industrial use of vapor phase process, liquid phase method and solid phase method maximum be comminuting method, use aforesaid method to prepare superfine powder and exist energy consumption high more, the shortcomings such as cost is high, complex process.With aforementioned production method, compare, adopt the self-spreading metallurgical method to produce the superfine powders such as refractory metal powder, amorphous boron powder or boride ceramics powder to have that raw materials cost is low, energy consumption is low, simple to operate, processing condition are required to the characteristics such as low, and the purity of product is high, granularity is little, powder activity is high.Northeastern University combines Self-propagating High-temperature Synthesis Process and metallurgical extract technology, (patent No. is respectively ZL200510047297.8 to have invented the new technology of the standby superfine powder of self-spreading metallurgical legal system, ZL200510047308.2, ZL201010233471.9, ZL201010233478.0, ZL200810011972.5), being about to the raw materials such as oxide compound and reductive agent magnesium powder mixes, after being pressed into the base sample, be placed in the self-propagating reaction stove, cause self-propagating reaction with means such as part igniting or constant temperature detonate, the cooling thick product of product disperse in spongiform magnesium oxide matrix that obtain, then the diluted acid of at room temperature take leaches thick product as leaching agent is direct, filtering separation obtains superfine powder, produced a large amount of acid magnesium-containing waste solutions owing to having introduced acid leaching process at leaching process.
Summary of the invention
The problems referred to above that exist for the standby superfine powder of self-spreading metallurgical legal system, the invention provides the clean preparation method of the standby superfine powder of a kind of self-spreading metallurgical legal system, adopting hydrochloric acid is that leaching agent leaches the synthetic thick product obtained of self propagating high temperature, remove magnesium oxide wherein, filtering separation obtains superfine powder and magnesium chloride solution, then the thermolysis of magnesium chloride solution directly being sprayed obtains the nano level magnesium oxide powder, obtain hydrogen chloride gas simultaneously, hydrogen chloride gas can return to the leaching process recycle after absorbing, and realizes the cleaner production of this process.
The clean preparation method of the standby superfine powder of self-spreading metallurgical legal system of the present invention carries out according to the following steps:
1, by after the oxide compound of powdery and the mixing of magnesium powder, being milled to granularity≤0.5 μ m, then be pressed into blank, put into the self-propagating reaction stove and cause self-propagating reaction; Described oxide compound is boron oxide, Tungsten oxide 99.999 or zirconium white;
After self-propagating reaction finishes, reaction product naturally cools to normal temperature, obtains thick product, and the boron in thick product or metal disperse are in spongy magnesium oxide matrix;
2, by thick product after fragmentation, adopt the mode of Leaching in Hydrochloric Acid to separate magnesium oxide wherein; Leaching the concentration of hydrochloric acid adopted is 1 ~ 5mol/L; Hydrochloric acid is (4 ~ 20): 1ml/g with the liquid-solid ratio of thick product, leaches the mode that adopts normal temperature to leach or the mode that high temperature leaches in confined conditions; When normal temperature leaches, extraction temperature is that 25 ~ 90 ℃, extraction time are 10 ~ 40h; When high temperature leaches, extraction temperature is that 100 ~ 150 ℃, extraction time are 30 ~ 180min; Filter after leaching and obtain solid phase and leach liquor;
3, impurity is removed in the solid phase washing that leaching obtains, then dries removal moisture, makes the superfine powder of weight purity >=99%;
4, adopt the mode of spraying thermolysis to process leach liquor; The spraying thermolysis is by atomizing nozzle, leach liquor to be carried out to the atomization winding-up in the high temperature pyrolysis stove under the pressure of 0.13 ~ 0.6MPa, then pyrolysis obtains nano level magnesium oxide and pyrolysis tail gas; Hydrogenchloride in pyrolysis tail gas forms hydrochloric acid after absorbing, and returns to leaching process and recycles; Pyrolysis temperature in the high temperature pyrolysis stove is that 200 ~ 700 ℃, pyrolysis time are 0.5 ~ 60min.
In aforesaid method, the pressure while being pressed into blank is 40 ~ 70MPa.
In aforesaid method, when oxide compound is boron oxide, blending ratio is boron oxide in mass ratio: magnesium powder=100:(110 ~ 128), when oxide compound is Tungsten oxide 99.999, blending ratio is Tungsten oxide 99.999 in mass ratio: magnesium powder=100:(33 ~ 40), when oxide compound is zirconium white, blending ratio is pressed zirconium white: magnesium powder=100:(105 ~ 122).
Above-mentioned self-propagating reaction general formula is as follows:
MeO
x+xMg=xMgO+Me+△H
Wherein Me is B, W or Zr, and △ H represents the reaction heat that the reaction of self-propagating reaction generating process discharges;
In aforesaid method, the leaching process reaction is as follows:
MgO+2HCl=MgCl
2+H
2O；
In aforesaid method, the reaction of thermal decomposition process is as follows:
MgCl
2+H
2O=MgO+2HCl。
The boron powder that above-mentioned superfine powder is granularity≤tungsten powder of 1 μ m, the zirconium powder of granularity≤400nm or granularity≤200nm.
In above-mentioned leach liquor, the mass concentration of magnesium chloride is 50 ~ 300g/L.
The magnesian granularity of above-mentioned nano level is 80 ~ 390 nm.
The concentration of the hydrochloric acid that above-mentioned hydrogenchloride forms after absorbing is 1 ~ 5mol/L.
In aforesaid method, self-propagating reaction is divided into direct initiation and constant temperature detonates two kinds; Direct initiation is direct heating blank under air atmosphere, until self-propagating reaction occurs, now can form dazzling flame, and have a large amount of cigarettes to volatilize, and the temperature of reaction system raises rapidly; Constant temperature detonates and refers under air atmosphere, the heating blank, and temperature is controlled between 720 ~ 950 ℃, until self-propagating reaction occurs, now can form dazzling flame, and have a large amount of cigarettes to volatilize, and the temperature of reaction system raises rapidly.
Because self-propagating reaction is to occur under unlimited air atmosphere, and the self-propagating reaction temperature is very high, and in reaction process, the gasification of MAGNESIUM METAL amount, can cause a large amount of volatilization loss of Mg, and Mg will be not enough like this; In order to make up the volatilization loss of Mg, the present invention when batching MAGNESIUM METAL than reaction theory requirement excessive 5 ~ 25%; In order to make the self-propagating reaction operation simpler, self-propagating reaction also can adopt the partial points pyrogenic process to cause.
With traditional superfine powder technology of preparing, compare, characteristics of the present invention and beneficial effect are:
(1) adopt the mode of self-spreading metallurgical to produce superfine powder, have that raw materials cost is low, energy consumption is low, simple to operate, processing condition are required to the characteristics such as low, and the purity of product is high, granularity is little, powder activity is high;
(2) adopt the mode of spraying thermolysis to process magnesium chloride solution, reaction efficiency is high, can obtain the nano level magnesium oxide product, has improved added value of product;
(3) production process produces acid and water can be realized recycle by thermal decomposition process, have realized that whole process is without useless cleaner production.
The accompanying drawing explanation
The clean preparation method process flow diagram that Fig. 1 is the standby superfine powder of self-spreading metallurgical legal system of the present invention.
Embodiment
Magnesium powder, boron oxide, Tungsten oxide 99.999 and the zirconium white adopted in the embodiment of the present invention is technical grade product, granularity all≤0.5mm.
The self-propagating reaction stove adopted in the embodiment of the present invention is the disclosed self-propagating reaction stove of patent " ZL200510047308.2 ", and this Reaktionsofen consists of reaction vessel, well heater, sight glass, transformer, function recording instrument, thermopair, gas valve.
In the embodiment of the present invention, the time of self-propagating reaction is 5 ~ 90s.
In the embodiment of the present invention, washing is that the solid phase water is filtered to washing, and the acid wash water of acquisition is for the moisture of Leaching in Hydrochloric Acid process replenish loss.
In the embodiment of the present invention, drying time is 24h at least.
The high temperature pyrolysis stove adopted in the embodiment of the present invention is the formula stove.
In the embodiment of the present invention be pressed into blank the time equipment that adopts be the pressure-like machine, the blank be pressed into is that diameter 5-10cm is cylindric.
The equipment that in the embodiment of the present invention, ball milling adopts is high energy ball mill.
Embodiment 1
By after the boron oxide of powdery and the mixing of magnesium powder, being milled to granularity≤0.5 μ m, then under 40MPa pressure, be pressed into blank, put into the self-propagating reaction stove and cause self-propagating reaction; Blending ratio is boron oxide in mass ratio: magnesium powder=100:110,
After self-propagating reaction finishes, reaction product naturally cools to normal temperature, obtains thick product, and the boron disperse in thick product is in spongy magnesium oxide matrix;
After fragmentation, adopt the mode of Leaching in Hydrochloric Acid to separate magnesium oxide wherein thick product; Leaching the concentration of hydrochloric acid adopted is 1mol/L; Hydrochloric acid is 20:1ml/g with the liquid-solid ratio of thick product, leaches the mode that adopts normal temperature to leach, and extraction temperature is that 90 ℃, extraction time are 10h; Filter after leaching and obtain solid phase and leach liquor; In leach liquor, the mass concentration of magnesium chloride is 50g/L;
Impurity is removed in the solid phase washing that leaching obtains, then dries removal moisture, makes the Superfine Boron Powder of weight purity >=99%, and granularity is between 120 ~ 200nm;
Adopt the mode of spraying thermolysis to process leach liquor; The spraying thermolysis is by atomizing nozzle, leach liquor to be carried out to the atomization winding-up in the high temperature pyrolysis stove under the pressure of 0.13MPa, then pyrolysis obtains nano level magnesium oxide and pyrolysis tail gas; Pyrolysis tail gas comprises water vapour and hydrogen chloride gas; Hydrogenchloride wherein forms hydrochloric acid after absorbing, and returns to leaching process and recycles; Pyrolysis temperature in the high temperature pyrolysis stove is that 700 ℃, pyrolysis time are 0.5min; The magnesian granularity of nano level is 180 ~ 230 nm; The concentration of the hydrochloric acid that hydrogenchloride forms after absorbing is 1mol/L.
Embodiment 2
The preparation method is with embodiment 1, and difference is:
(1) be pressed into blank under 60MPa pressure; Blending ratio is boron oxide in mass ratio: magnesium powder=100:120;
(2) leaching the concentration of hydrochloric acid adopted is 3mol/L; Hydrochloric acid is 10:1ml/g with the liquid-solid ratio of thick product; The mode extraction temperature that leach to adopt normal temperature to leach is that 25 ℃, extraction time are 40h; Obtain solid phase and leach liquor after leaching; In leach liquor, the mass concentration of magnesium chloride is 180g/L;
(3) the spraying thermolysis is by atomizing nozzle, leach liquor to be carried out to the atomization winding-up in the high temperature pyrolysis stove under the pressure of 0.32MPa, and the pyrolysis temperature in the high temperature pyrolysis stove is that 400 ℃, pyrolysis time are 10min; The magnesian granularity of nano level is 80 ~ 100 nm; The concentration of the hydrochloric acid that hydrogenchloride forms after absorbing is 3mol/L.
Embodiment 3
The preparation method is with embodiment 1, and difference is:
(1) be pressed into blank under 70MPa pressure; Blending ratio is boron oxide in mass ratio: magnesium powder=100:128;
(2) leaching the concentration of hydrochloric acid adopted is 5mol/L; Hydrochloric acid is 4:1ml/g with the liquid-solid ratio of thick product; The mode extraction temperature that leach to adopt normal temperature to leach is that 50 ℃, extraction time are 20h; Obtain solid phase and leach liquor after leaching; In leach liquor, the mass concentration of magnesium chloride is 300g/L;
(3) the spraying thermolysis is by atomizing nozzle, leach liquor to be carried out to the atomization winding-up in the high temperature pyrolysis stove under the pressure of 0.6MPa, and the pyrolysis temperature in the high temperature pyrolysis stove is that 200 ℃, pyrolysis time are 60min; The magnesian granularity of nano level is 330 ~ 390 nm; The concentration of the hydrochloric acid that hydrogenchloride forms after absorbing is 5mol/L.
Embodiment 4
By after the Tungsten oxide 99.999 of powdery and the mixing of magnesium powder, being milled to granularity≤0.5 μ m, then under 40MPa pressure, be pressed into blank, put into the self-propagating reaction stove and cause self-propagating reaction; Blending ratio is Tungsten oxide 99.999 in mass ratio: magnesium powder=100:33,
After self-propagating reaction finishes, reaction product naturally cools to normal temperature, obtains thick product, and the tungsten disperse in thick product is in spongy magnesium oxide matrix;
After fragmentation, adopt the mode of Leaching in Hydrochloric Acid to separate magnesium oxide wherein thick product; Leaching the concentration of hydrochloric acid adopted is 1mol/L; Hydrochloric acid is 20:1ml/g with the liquid-solid ratio of thick product, and leaching and adopting the mode that high temperature leaches in confined conditions, extraction temperature is that 100 ~ 150 ℃, extraction time are 180min; Filter after leaching and obtain solid phase and leach liquor; In leach liquor, the mass concentration of magnesium chloride is 50g/L;
Impurity is removed in the solid phase washing that leaching obtains, then dries removal moisture, makes the ultrafine tungsten powder of weight purity >=99%, and granularity is between 0.5 ~ 1 μ m;
Adopt the mode of spraying thermolysis to process leach liquor; The spraying thermolysis is by atomizing nozzle, leach liquor to be carried out to the atomization winding-up in the high temperature pyrolysis stove under the pressure of 0.13MPa, then pyrolysis obtains nano level magnesium oxide and pyrolysis tail gas; Pyrolysis tail gas comprises water vapour and hydrogen chloride gas; Hydrogenchloride wherein forms hydrochloric acid after absorbing, and returns to leaching process and recycles; Pyrolysis temperature in the high temperature pyrolysis stove is that 700 ℃, pyrolysis time are 0.5min; The magnesian granularity of nano level is 300 ~ 360 nm; The concentration of the hydrochloric acid that hydrogenchloride forms after absorbing is 1mol/L.
Embodiment 5
The preparation method is with embodiment 4, and difference is:
(1) be pressed into blank under 60MPa pressure; Blending ratio is Tungsten oxide 99.999 in mass ratio: magnesium powder=100:36;
(2) leaching the concentration of hydrochloric acid adopted is 5mol/L; Hydrochloric acid is 4:1ml/g with the liquid-solid ratio of thick product; The mode that leaching adopts high temperature in confined conditions to leach, extraction temperature is that 100 ~ 150 ℃, extraction time are 30min; Obtain solid phase and leach liquor after leaching; In leach liquor, the mass concentration of magnesium chloride is 300g/L;
(3) the spraying thermolysis is by atomizing nozzle, leach liquor to be carried out to the atomization winding-up in the high temperature pyrolysis stove under the pressure of 0.6MPa, and the pyrolysis temperature in the high temperature pyrolysis stove is that 200 ℃, pyrolysis time are 60min; The magnesian granularity of nano level is 100 ~ 190 nm; The concentration of the hydrochloric acid that hydrogenchloride forms after absorbing is 5mol/L.
Embodiment 6
The preparation method is with embodiment 4, and difference is:
(1) be pressed into blank under 70MPa pressure; Blending ratio is Tungsten oxide 99.999 in mass ratio: magnesium powder=100:40;
(2) leaching the concentration of hydrochloric acid adopted is 3mol/L; Hydrochloric acid is 10:1ml/g with the liquid-solid ratio of thick product; The mode that leaching adopts high temperature in confined conditions to leach, extraction temperature is that 100 ~ 150 ℃, extraction time are 100min; Obtain solid phase and leach liquor after leaching; In leach liquor, the mass concentration of magnesium chloride is 200g/L;
(3) the spraying thermolysis is by atomizing nozzle, leach liquor to be carried out to the atomization winding-up in the high temperature pyrolysis stove under the pressure of 0.3MPa, and the pyrolysis temperature in the high temperature pyrolysis stove is that 500 ℃, pyrolysis time are 20min; The magnesian granularity of nano level is 200 ~ 290 nm; The concentration of the hydrochloric acid that hydrogenchloride forms after absorbing is 3mol/L.
Embodiment 7
By after the zirconium white of powdery and the mixing of magnesium powder, being milled to granularity≤0.5 μ m, then under 40MPa pressure, be pressed into blank, put into the self-propagating reaction stove and cause self-propagating reaction; Blending ratio is zirconium white in mass ratio: magnesium powder=100:105,
After self-propagating reaction finishes, reaction product naturally cools to normal temperature, obtains thick product, and the zirconium disperse in thick product is in spongy magnesium oxide matrix;
After fragmentation, adopt the mode of Leaching in Hydrochloric Acid to separate magnesium oxide wherein thick product; Leaching the concentration of hydrochloric acid adopted is 1mol/L; Hydrochloric acid is 20:1ml/g with the liquid-solid ratio of thick product, and leaching and adopting the mode that high temperature leaches in confined conditions, extraction temperature is that 100 ~ 150 ℃, extraction time are 180min; Filter after leaching and obtain solid phase and leach liquor; In leach liquor, the mass concentration of magnesium chloride is 50g/L;
Impurity is removed in the solid phase washing that leaching obtains, then dries removal moisture, makes the ultra-fine zirconium powder of weight purity >=99%, and granularity is between 220 ~ 400nm;
Adopt the mode of spraying thermolysis to process leach liquor; The spraying thermolysis is by atomizing nozzle, leach liquor to be carried out to the atomization winding-up in the high temperature pyrolysis stove under the pressure of 0.13MPa, then pyrolysis obtains nano level magnesium oxide and pyrolysis tail gas; Pyrolysis tail gas comprises water vapour and hydrogen chloride gas; Hydrogenchloride wherein forms hydrochloric acid after absorbing, and returns to leaching process and recycles; Pyrolysis temperature in the high temperature pyrolysis stove is that 700 ℃, pyrolysis time are 0.5min; The magnesian granularity of nano level is 310 ~ 360 nm; The concentration of the hydrochloric acid that hydrogenchloride forms after absorbing is 1mol/L.
Embodiment 8
The preparation method is with embodiment 7, and difference is:
(1) be pressed into blank under 50MPa pressure; Blending ratio is zirconium white in mass ratio: magnesium powder=100:122;
(2) leaching the concentration of hydrochloric acid adopted is 5mol/L; Hydrochloric acid is 4:1ml/g with the liquid-solid ratio of thick product; The mode that leaching adopts high temperature in confined conditions to leach, extraction temperature is that 100 ~ 150 ℃, extraction time are 30min; Obtain solid phase and leach liquor after leaching; In leach liquor, the mass concentration of magnesium chloride is 300g/L;
(3) the spraying thermolysis is by atomizing nozzle, leach liquor to be carried out to the atomization winding-up in the high temperature pyrolysis stove under the pressure of 0.6MPa, and the pyrolysis temperature in the high temperature pyrolysis stove is that 200 ℃, pyrolysis time are 60min; The magnesian granularity of nano level is 160 ~ 200 nm; The concentration of the hydrochloric acid that hydrogenchloride forms after absorbing is 5mol/L.
Embodiment 9
The preparation method is with embodiment 7, and difference is:
(1) be pressed into blank under 70MPa pressure; Blending ratio is zirconium white in mass ratio: magnesium powder=100:115;
(2) leaching the concentration of hydrochloric acid adopted is 3mol/L; Hydrochloric acid is 10:1ml/g with the liquid-solid ratio of thick product; The mode that leaching adopts high temperature in confined conditions to leach, extraction temperature is that 100 ~ 150 ℃, extraction time are 90min; Obtain solid phase and leach liquor after leaching; In leach liquor, the mass concentration of magnesium chloride is 200g/L;
(3) the spraying thermolysis is by atomizing nozzle, leach liquor to be carried out to the atomization winding-up in the high temperature pyrolysis stove under the pressure of 0.3MPa, and the pyrolysis temperature in the high temperature pyrolysis stove is that 500 ℃, pyrolysis time are 20min; The magnesian granularity of nano level is 200 ~ 280 nm; The concentration of the hydrochloric acid that hydrogenchloride forms after absorbing is 3mol/L.
Claims (6)
1. the clean preparation method of the standby superfine powder of a self-spreading metallurgical legal system is characterized in that carrying out according to the following steps:
(1) by after the oxide compound of powdery and the mixing of magnesium powder, being milled to granularity≤0.5 μ m, then be pressed into blank, put into the self-propagating reaction stove and cause self-propagating reaction; Described oxide compound is boron oxide, Tungsten oxide 99.999 or zirconium white;
After self-propagating reaction finishes, reaction product naturally cools to normal temperature, obtains thick product, and the boron in thick product or metal disperse are in spongy magnesium oxide matrix;
(2) by thick product after fragmentation, adopt the mode of Leaching in Hydrochloric Acid to separate magnesium oxide wherein; Leaching the concentration of hydrochloric acid adopted is 1 ~ 5mol/L; Hydrochloric acid is (4 ~ 20): 1ml/g with the liquid-solid ratio of thick product, leaches the mode that adopts normal temperature to leach or the mode that high temperature leaches in confined conditions; When normal temperature leaches, extraction temperature is that 25 ~ 90 ℃, extraction time are 10 ~ 40h; When high temperature leaches, extraction temperature is that 100 ~ 150 ℃, extraction time are 30 ~ 180min; Filter after leaching and obtain solid phase and leach liquor;
(3) impurity is removed in the solid phase washing that leaching obtains, then dries removal moisture, makes the superfine powder of weight purity >=99%;
(4) adopt the mode of spraying thermolysis to process leach liquor; The spraying thermolysis is by atomizing nozzle, leach liquor to be carried out to the atomization winding-up in the high temperature pyrolysis stove under the pressure of 0.13 ~ 0.6MPa, then pyrolysis obtains nano level magnesium oxide and pyrolysis tail gas; Hydrogenchloride in pyrolysis tail gas forms hydrochloric acid after absorbing, and returns to leaching process and recycles; Pyrolysis temperature in the high temperature pyrolysis stove is that 200 ~ 700 ℃, pyrolysis time are 0.5 ~ 60min.
2. a kind of self-spreading metallurgical legal system according to claim 1 is for the clean preparation method of superfine powder, it is characterized in that when oxide compound is boron oxide, blending ratio is boron oxide in mass ratio: magnesium powder=100:(110 ~ 128), when oxide compound is Tungsten oxide 99.999, blending ratio is Tungsten oxide 99.999 in mass ratio: magnesium powder=100:(33 ~ 40), when oxide compound is zirconium white, blending ratio is zirconium white in mass ratio: magnesium powder=100:(105 ~ 122).
3. the clean preparation method of the standby superfine powder of a kind of self-spreading metallurgical legal system according to claim 1, is characterized in that the boron powder that described superfine powder is granularity≤tungsten powder of 1 μ m, the zirconium powder of granularity≤400nm or granularity≤200nm.
4. a kind of self-spreading metallurgical legal system according to claim 1 is for the clean preparation method of superfine powder, and the mass concentration that it is characterized in that magnesium chloride in described leach liquor is 50 ~ 300g/L.
5. the clean preparation method of the standby superfine powder of a kind of self-spreading metallurgical legal system according to claim 1, is characterized in that the magnesian granularity of described nano level is 80 ~ 390 nm.
6. the clean preparation method of the standby superfine powder of a kind of self-spreading metallurgical legal system according to claim 1, is characterized in that the concentration of the hydrochloric acid that described hydrogenchloride forms after absorbing is 1 ~ 5mol/L.
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