CN110387480B - Particle refining agent for magnesium alloy and preparation method thereof - Google Patents
Particle refining agent for magnesium alloy and preparation method thereof Download PDFInfo
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- C22C1/00—Making non-ferrous alloys
- C22C1/06—Making non-ferrous alloys with the use of special agents for refining or deoxidising
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Abstract
The invention relates to the technical field of refining agent preparation, and particularly discloses a particle refining agent for magnesium alloy and a preparation method thereof, wherein raw materials are mixed and then put into a melting furnace for melting, and the melting temperature is more than or equal to 700 ℃; the melting material is condensed to a solid state after heat preservation and is crushed; crushing the mixture condensed to a solid state into a powdery material; the powder material is extruded by a granulator to obtain a particle refining agent with the particle size of 0.83-3.15 mm, and the raw materials of the refining agent comprise 47-55 parts by weight of MgCl25-8 parts of NaCl and 35-40 parts of KCl, and the balance of magnesium fluoride and magnesium oxide, wherein the particle size of the particle refining agent is 0.83-3.15 mm, and the density is 1.17-1.21 g/cm3The melting point is 440-480 ℃. The technical scheme of the invention solves the problem that the existing refining agent has poor refining effect due to the density close to that of the magnesium alloy melt.
Description
Technical Field
The invention relates to the technical field of refining agent preparation, and particularly relates to a particle refining agent for magnesium alloy and a preparation method thereof.
Background
Magnesium and magnesium alloys have a low melting point and a small heat capacity, are rapidly oxidized when heated in air, are easily burned when overheated, and are vigorously burned when not protected with a refining agent in a molten state. The surface oxide film of the magnesium alloy melt is loose, and magnesium is an active element and has strong bonding force with oxygen, so that MgO and Mg can be generated by reaction with oxygen, water vapor and nitrogen in the atmosphere during smelting3N2And H2And the like. Therefore, magnesium and magnesium alloy must be always refined in a refining agent and under a protective atmosphere during smelting. Meanwhile, various tools also need to be washed and protected during the transfer of magnesium alloys and the casting process, which all involve the use of refining agents.
The refining agent prepared by the process has high melting point and density which is often close to that of a magnesium alloy melt, so that the refining agent cannot quickly float upwards in the magnesium alloy melt and takes away slag in the magnesium alloy melt, the refining effect of the magnesium alloy melt is influenced, meanwhile, the refining agent covering the surface of the magnesium alloy melt can sink, the heat loss on the surface of the magnesium alloy melt is fast, and meanwhile, the surface of the magnesium alloy melt is further oxidized, so that the burning loss of the magnesium alloy melt is increased.
Disclosure of Invention
The invention provides a particle refining agent for magnesium alloy and a preparation method thereof, aiming at solving the problems that the existing refining agent can not quickly float upwards due to the density being close to that of a magnesium alloy melt, slag inclusion in the magnesium alloy melt is taken away, and the refining effect is poor, and simultaneously, the refining agent covering the surface of the magnesium alloy melt can sink, so that the surface of the magnesium alloy melt is further oxidized.
In order to achieve the purpose, the technical scheme of the invention is as follows:
a particle refining agent for magnesium alloy comprises 47-55 parts by weight of MgCl25-8 parts of NaCl and 35-40 parts of KCl, and the balance of magnesium fluoride and magnesium oxide, wherein the particle size of the particle refining agent is 0.83-3.15 mm, and the density is 1.17-1.21 g/cm3The melting point is 440-480 ℃.
The technical principle and the effect of the technical scheme are as follows:
the melting point of the particle refining agent is low (440-480 ℃), so that the refining agent can be quickly melted after entering the magnesium alloy melt, and the slag groups are adsorbed and wrapped, thereby being beneficial to discharging the slag groups in the magnesium alloy melt, and the density of the particle refining agent is small (1.17-1.21 g/cm)3) And the density of the magnesium alloy solution is about 1.8 g/cm3Therefore, the density of the refining agent in the scheme is far less than that of the magnesium alloy melt, so that the refining agent enters the magnesium alloy melt to wrap slag groups to float upwards quickly and discharge magnesium when being applied to the magnesium alloy melt refining processThe alloy melt further improves the refining effect of the magnesium alloy melt.
Furthermore, the water content in the particle refining agent is less than or equal to 0.5 percent.
Has the advantages that: because the existence of the moisture can have strong oxidation effect on the magnesium alloy melt, the moisture is reduced, so that the burning loss of the magnesium alloy melt can be avoided.
Further, the refining agent is irregularly shaped particles.
Has the advantages that: irregular particles can increase the contact area of the particle refining agent and the magnesium alloy melt, thereby improving the slag removal capability of the magnesium alloy melt.
A preparation method of a particle refining agent for magnesium alloy comprises the following steps:
step 1: mixing magnesium chloride, sodium chloride, potassium chloride, magnesium fluoride and magnesium oxide, and then putting the mixture into a melting furnace for melting, wherein the melting temperature is more than or equal to 700 ℃;
step 2: preserving the heat of the molten material in the step 1 for more than 70min, and then condensing the molten material to a solid state;
and step 3: crushing the mixture condensed to be solid in the step 2 to obtain a powdery material;
and 4, step 4: and (4) granulating the powdery material obtained in the step (3) by adopting an extrusion granulator to obtain a granule refining agent with the particle size of 0.83-3.15 mm.
Has the advantages that: in the scheme, MgCl is added2Raw materials such as NaCl, KCl and the like are melted, solidified and crushed to be extruded and granulated into a particle refining agent with the thickness of 0.83-3.15 mm, and the industrial production data statistics shows that after the particle refining agent in the scheme is adopted to refine the magnesium alloy melt, the removal rate of alkali metal in the magnesium alloy melt can reach 70-80%, the removal rate of oxide inclusion in the magnesium alloy melt is more than 70%, and the subsequent filtering pressure of the magnesium alloy melt is greatly reduced.
1. Mixing MgCl2The raw materials of NaCl, KCl and the like are melted to form a stable binary eutectic compound (MgKCl)3And NaKCl2) The melting point of the compound is much lower than that of MgCl2NaCl, KCl and other raw materials, so that the refining agent can be quickly dissolved in the magnesium alloy melt to achieve refiningThe effect of (1).
2. Through powder material extrusion after will smashing in this scheme for finished product granule refining agent, such effect lies in, owing to through powder extrusion's granule, its inside small hole that has not only can reduce the density of granule refining agent, and the existence in hole makes the granule can absorb the heat in the magnesium alloy melt fast simultaneously to melt fast.
For the particle refining agent entering the magnesium alloy melt, the surface adsorption force is large due to the existence of pores in the refining agent, the wrapping capacity of the particle refining agent on slag clusters in the magnesium alloy melt is improved, the deslagging efficiency is improved, and the separation of the magnesium alloy melt and the slag clusters is better realized.
In addition, the particle refining agent covered on the surface of the magnesium alloy melt has loose air holes in the particles, has small particle density, can float on the surface of the magnesium alloy melt and cannot sink, so that the magnesium alloy melt is protected from further oxidation, and the surface heat loss of the magnesium alloy melt can be prevented, thereby effectively avoiding the problems of aluminum melt oxidation aggravation and loss caused by heat release of the refining agent in the internal refining process of the magnesium alloy melt.
Compared with the prior art, the solidified material is directly crushed into particles, the particles formed in the way have no loose air holes inside, the density of the particles is high, the particles are not easy to float upwards in the magnesium alloy melt, meanwhile, the adsorption force on the surfaces of the particles is reduced, and the wrapping capacity of the particles on the slag clusters in the magnesium alloy melt is reduced.
Further, when smelting is carried out in the step 1, heating is carried out step by step, the mixture is heated to 445-480 ℃ at a speed of less than or equal to 3 ℃/min, the temperature is kept for 20-25 min, and then the mixture is heated to a temperature of more than or equal to 700 ℃.
Has the advantages that: firstly, heating the mixture to 420-465 ℃ at a speed of less than or equal to 3 ℃/min, and preserving the heat for 20-25 min, because MgCl2NaCl and KCl are used as main raw materials, when the main raw materials are melted, a plurality of binary eutectic compounds can be formed when the temperature reaches above 420 ℃, and the two compounds can be more fully formed into the binary eutectic compounds by slow heating.
Further, after heating to a temperature of more than or equal to 700 ℃, heat preservation is carried out for 50-65 min.
Has the advantages that: the temperature is kept at the temperature of more than or equal to 700 ℃ for 50-65 min, so that some unstable binary eutectic compounds in the eutectic system can be prepared, for example: MgKCl4、NaKCl3、NaKCl4To form a stable eutectic compound.
Further, the crushing in the step 2 is completed in multiple steps, firstly, a jaw crusher is adopted to crush the materials into blocks, and then, a hammer crusher is adopted to crush the blocks into powder.
Has the advantages that: the crushing is completed step by step, so that the loss of the crusher can be reduced, and the service life of the crusher is prolonged.
And further, screening the powdery material obtained in the step 3 to obtain granular material and powdery material, wherein the adopted mesh is 200-300 meshes.
Has the advantages that: the granularity of the powdery material can be ensured after screening, and the large granular material is screened out, so that the bad influence of the granular material on the subsequent granulation is avoided.
Further, the screened granular materials are returned to the step 3 for crushing or are returned to the step 1 for smelting again.
Has the advantages that: the recovery of the granular materials is realized, and the loss of the materials is reduced.
Further, a binder is added to the powdery material before extrusion granulation in the step 4.
Has the advantages that: the use of the binder can improve the bonding strength between the powdery materials, so that the formed particles are not easy to break.
Drawings
FIG. 1 is a schematic view showing the structure of a granulating drum in an extrusion granulator used in example 1 of the present invention;
FIG. 2 is an enlarged view of portion A of FIG. 1 according to the present invention.
Detailed Description
The following is further detailed by way of specific embodiments:
reference numerals in the drawings of the specification include: the device comprises an outer layer cylinder 10, an inner layer cylinder 11, reinforcing ribs 12, a channel interlayer 13, a granulation groove 14, an elastic layer 15, an air cavity 16, an air flow hole 17 and a protrusion 18.
A particle refining agent for magnesium alloy comprises 47-55 parts by weight of MgCl25-8 parts of NaCl and 35-40 parts of KCl, and the balance of magnesium fluoride and magnesium oxide, wherein the particle size of the particle refining agent is 0.83-3.15 mm, and the density is 1.17-1.21 g/cm3The melting point is 440-480 ℃, the water content in the particle refining agent is less than or equal to 0.5%, and the shape of the refining agent particles is irregular.
The preparation method of the particle refining agent for reducing the burning loss of the aluminum alloy is illustrated by examples 1 to 5, and the process parameters of the examples 1 to 5 are shown in the following table 1:
table 1 shows the process parameters of examples 1 to 5 of a method for preparing a grain refining agent for magnesium alloy
| Example parameters | Example 1 | Example 2 | Example 3 | Example 4 | Example 5 |
| First heating temperature (. degree. C.) | 420 | 430 | 440 | 455 | 465 |
| Heating Rate (. degree. C./min) | 3 | 2.5 | 2.5 | 2 | 2 |
| First heat preservation time (min) | 20 | 20 | 22 | 22 | 25 |
| Second heating temperature (. degree. C.) | 700 | 710 | 750 | 750 | 770 |
| Second heat preservation time (min) | 50 | 55 | 60 | 60 | 65 |
| Mesh of sieving | 200 | 230 | 260 | 260 | 300 |
| Binder | Epoxy resin | Epoxy resin | Phenolic resin | Phenolic resin | Phenolic resin |
The following will explain in detail a method for producing a grain refining agent for magnesium alloy by taking example 1 as an example, comprising the steps of:
step 1: the mixture of the raw materials of magnesium chloride, sodium chloride, potassium chloride, magnesium fluoride and magnesium oxide is put into a melting furnace for melting, the first heating temperature is 420 ℃, the heating rate is 3 ℃/min, the temperature is kept for 20min, and then the mixture is heated to 700 ℃ to obtain molten material.
Step 2: and (3) preserving the heat of the molten material in the step (1) for 50min, condensing to a solid state, crushing the solid material into blocks by using a jaw crusher, ensuring the particle size of the block material to be below 15cm, crushing the block material into powder by using a hammer crusher, sieving by using a 200-mesh sieve, and obtaining the powder material and the granular material after sieving.
And (3) crushing the screened granular materials again by using a hammer crusher, or returning the granular materials to the melting furnace in the step 1 for smelting again.
And step 3: and (3) adding epoxy resin into the powder material sieved in the step (2), wherein the mass of the added epoxy resin accounts for 8-10% of that of the powder material, and performing extrusion granulation by using an extrusion granulator to obtain a granule refining agent with the particle size of 0.83-3.15 mm.
The structure of the granulation roller in the extrusion granulator adopted in the step 3 is shown in fig. 1, and comprises an outer layer cylinder 10 and an inner layer cylinder 11, wherein a reinforcing rib 12 is fixed between the inner layer cylinder 11 and the outer layer cylinder 10, a channel interlayer 13 is formed between the outer layer cylinder 10 and the inner layer cylinder 11, two ends of the outer layer cylinder 10 are coaxially connected with pipelines, the pipelines are communicated with the channel interlayer 13, a plurality of granulation grooves 14 are uniformly distributed on the outer layer cylinder 10, an elastic layer 15 is bonded in each granulation groove 14, an air cavity 16 is formed between each elastic layer 15 and each granulation groove 14 in combination with the structure shown in fig. 2, an air flow hole 17 communicated with the air cavity 16 and the channel interlayer 13 is formed at the bottom of each granulation groove 14, a plurality of protrusions 18 are uniformly distributed on the outer wall of the inner layer cylinder 11, the protrusions 18 are opposite to the granulation grooves 14 on the outer layer cylinder 10, the heights of the protrusions 18 are different, and therefore, the distances between the channels between, meanwhile, the positions of the airflow holes 17 in the granulation tanks 14 are different, and the sizes of the airflow holes 17 are different.
During granulation, a group of granulation rollers with attached side walls rotate relatively, the tangential directions of adjacent parts of the two granulation rollers are downward, during granulation, a powdery material and a binder are mixed and then fall between the two granulation rollers from top to bottom, the arrow in figure 1 indicates the direction of cold air flow, during granulation, high-pressure cold air (with the temperature not higher than 18 ℃) enters the channel interlayer 13 from the left end of the granulation roller and then flows out from the right end of the granulation roller along the channel interlayer 13, when the cold air flow flows between the bulge 18 and the granulation groove 14, the distance between the channel between the bulge 18 and the granulation groove 14 is reduced, the gas flow velocity is increased, the air pressure is reduced, therefore, the gas in the air cavity 16 enters the channel interlayer 13 through the airflow hole 17, meanwhile, the elastic layer 15 deforms towards the airflow hole 17, and the powdery material entering the granulation groove 14 is extruded during deformation of the elastic layer 15, thereby forming a particle discharge.
Because the channel spacing between each protrusion 18 and the granulation tank 14 is different, and the size of the airflow hole 17 is different, the pressure between each protrusion 18 and the granulation tank 14 is different, so that the elastic layers 15 are deformed in different sizes, and different granular refining agents with irregular shapes are formed. It should be noted that in the present application, the flow rate of the high-pressure gas introduced into the granulation cylinder is not constant, but is in a variable state, so that the elastic layer 15 has the opportunity to recover its deformation, thereby completing the granulation.
By adopting the granulation roller, not only can the granular refining agents with different shapes be obtained, but also the high-pressure cold air introduced can cool the granular refining agents and the granulation roller, the service life of the granulation roller is prolonged, and meanwhile, the temperature of the granular refining agents is not too high.
Examples 2 to 5 are the same as example 1 except for the process parameters.
Two groups of comparative examples and the grain refining agents prepared in examples 1 to 5 were additionally arranged for comparative experiments:
comparative example 1: the difference from the example 1 is that the step 3 is not performed in the comparative example 1, and the solid material is crushed into particles with the particle size of 1-4 mm only by using a crusher.
Comparative example 2: the difference from example 1 is that the pellets obtained in comparative example 2 were spherical pellets of about 2 mm.
Now, the particle refining agents prepared in examples 1 to 5 and comparative examples 1 to 2 were subjected to powder injection refining experiments:
according to production requirements, the refining agents prepared in the examples 1-5 and the comparative examples 1-2 are added into a powder spraying refining tank, the refining tank is opened when the temperature of the magnesium liquid is 660-690 ℃, and inert gas (the pressure of the inert gas is 1.2-1.8 kg/cm) is introduced into the refining tank2) And spraying the particle refining agent into the magnesium alloy melt by using inert gas, and removing oxidation inclusions, alkali metal, hydrogen and the like in the magnesium liquid under the combined action of the small dispersive bubbles and the particle refining agent, wherein the refining time is 15-20 minutes each time.
And (3) after the refined magnesium alloy melt is solidified, detecting the cast structure of the magnesium alloy melt, measuring the removal rate of alkali metal and oxide inclusions in the magnesium alloy melt, and averaging.
The experimental results of examples 1 to 5 and comparative examples 1 to 2 are shown in the following table 2:
table 2 shows the removal rates of alkali metal and oxide inclusions in the refining agents prepared in examples 1 to 5 and comparative examples 1 to 2
| Example 1 | Example 2 | Example 3 | Example 4 | Example 5 | Comparative example 1 | Comparative example 2 | |
| Rate of removal of impurities from alkali metal | 71% | 70% | 73% | 76% | 79% | 50% | 61% |
| Removal rate of oxide inclusions | 70% | 71% | 72% | 76% | 78% | 57% | 60% |
From table 2 above, it can be seen that:
1. in the industrial application of the particle refining agent obtained in the embodiment 1-5 in magnesium alloy melt refining, the removal rate of alkali metal in the magnesium alloy melt can reach 70-80%, and the removal rate of oxide inclusions in the magnesium alloy melt is more than 70%, so that the subsequent filtering pressure of the magnesium alloy melt is greatly reduced, the titanium casting structure of the aluminum alloy is greatly improved, and the quality of the aluminum alloy is greatly improved.
2. In comparative example 1, since extrusion granulation molding is not adopted, the density of the granule refining agent prepared in comparative example 1 is detected to be about 1.71-1.79 g/cm3Density and density of magnesium alloy solution (about 1.8 g/cm)3) And the slag groups can not be quickly wrapped and float upwards, so that the removal rate of alkali metal and oxide inclusion is reduced.
3. In comparative example 2, since the pellets were formed into spherical pellets, the contact area with the molten aluminum in the transverse or vertical direction was reduced after the pellets were introduced into the molten aluminum, the adsorption of the slag agglomerates was reduced, and the removal rate of both alkali metal and oxide inclusions was reduced as seen from the results of the examination.
The foregoing is merely an example of the present invention and common general knowledge of known specific structures and features of the embodiments is not described herein in any greater detail. It should be noted that, for those skilled in the art, without departing from the structure of the present invention, several changes and modifications can be made, which should also be regarded as the protection scope of the present invention, and these will not affect the effect of the implementation of the present invention and the practicability of the patent. The scope of the claims of the present application shall be determined by the contents of the claims, and the description of the embodiments and the like in the specification shall be used to explain the contents of the claims.
Claims (8)
1. A particle refining agent for magnesium alloy is characterized in that: the refining agent comprises 47-55 parts by weight of MgCl25-8 parts of NaCl and 35-40 parts of KCl, and the balance of magnesium fluoride and magnesium oxide, wherein the particle size of the particle refining agent is 0.83-3.15 mm, and the density is 1.17-1.21 g/cm3The melting point is 440-480 ℃;
the preparation method of the particle refining agent for magnesium alloy comprises the following steps:
step 1: mixing magnesium chloride, sodium chloride, potassium chloride, magnesium fluoride and magnesium oxide, and then putting the mixture into a melting furnace for melting, wherein the melting temperature is more than or equal to 700 ℃;
step 2: preserving the heat of the molten material in the step 1 for more than 70min, and then condensing the molten material to a solid state;
and step 3: crushing the mixture condensed to be solid in the step 2 to obtain a powdery material;
and 4, step 4: granulating the powdery material obtained in the step 3 by adopting an extrusion granulator, and adding a binder into the powdery material before extrusion granulation; obtaining a particle refining agent with the particle size of 0.83-3.15 mm;
the extrusion granulator includes the granulation roller, the granulation roller includes outer section of thick bamboo and inlayer section of thick bamboo, be fixed with the strengthening rib between inlayer section of thick bamboo and the outer section of thick bamboo, be formed with the passageway intermediate layer between outer section of thick bamboo and the inlayer section of thick bamboo, the equal coaxial coupling in both ends of outer section of thick bamboo has the pipeline, pipeline and passageway intermediate layer intercommunication, the equipartition has a plurality of granulation grooves on outer section of thick bamboo, it has the elastic layer to bond in the granulation groove, form the air cavity between elastic layer and the granulation groove, intercommunication air cavity and the interbedded air current hole of passageway have been seted up to the bottom in granulation groove, the equipartition has a plurality of archs on the outer wall of inlayer section of thick bamboo, and each arch all is relative with the granulation groove position on.
2. The refining agent for magnesium alloy particles according to claim 1, characterized in that: the water content in the particle refining agent is less than or equal to 0.5 percent.
3. The refining agent for magnesium alloy particles according to claim 2, characterized in that: the refining agent is irregular-shaped particles.
4. The refining agent for magnesium alloy particles according to claim 3, characterized in that: during smelting in the step 1, heating is carried out step by step, the mixture is heated to 420-465 ℃ at a speed of less than or equal to 3 ℃/min, heat is preserved for 20-25 min, and then the mixture is heated to a temperature of more than or equal to 700 ℃.
5. The refining agent for magnesium alloy particles according to claim 4, characterized in that: heating to a temperature of more than or equal to 700 ℃, and then preserving heat for 50-65 min.
6. The refining agent for magnesium alloy particles according to claim 4, characterized in that: and 3, crushing in multiple steps, namely crushing the materials into blocks by using a jaw crusher, and crushing the blocks into powder by using a hammer crusher.
7. The refining agent for magnesium alloy particles according to claim 5, characterized in that: and (4) screening the powdery material obtained in the step (3) to obtain granular material and powdery material, wherein the adopted meshes are 200-300 meshes.
8. The refining agent for magnesium alloy particles according to claim 6, characterized in that: and (4) after screening, returning the granular materials to the step 3 for crushing or entering the step 1 for smelting again.
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| CN104438422A (en) * | 2014-09-28 | 2015-03-25 | 洛阳镁鑫合金制品有限公司 | Process for rolling ZK61M magnesium alloy sheets |
| CN107083508A (en) * | 2017-04-17 | 2017-08-22 | 扬州峰明光电新材料有限公司 | A kind of polynary enhanced heat-proof corrosion-resistant magnesium alloy and its manufacture method |
| CN107130129A (en) * | 2017-07-18 | 2017-09-05 | 合肥万之景门窗有限公司 | A kind of composite refiner of aluminium alloy and preparation method thereof |
| CN108070763A (en) * | 2017-12-21 | 2018-05-25 | 南京工程学院 | A kind of magnesium alloy with LPSO and/or SFs structures and preparation method thereof |
| CN108311652A (en) * | 2018-02-06 | 2018-07-24 | 洛阳晟雅镁合金科技有限公司 | A kind of preparation process of ME20M magnesium alloys slab ingot |
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