CN105152652A - Plate-shaped Cr with ferrochrome slag as main material7C3And method for preparing the same - Google Patents
Plate-shaped Cr with ferrochrome slag as main material7C3And method for preparing the same Download PDFInfo
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- CN105152652A CN105152652A CN201510647704.2A CN201510647704A CN105152652A CN 105152652 A CN105152652 A CN 105152652A CN 201510647704 A CN201510647704 A CN 201510647704A CN 105152652 A CN105152652 A CN 105152652A
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- ferrochrome
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Abstract
The invention relates to a plate-shaped Cr using ferrochromium slag as a main material7C3And a method for preparing the same. The technical scheme is as follows: mixing materials according to the mass ratio of the ferrochrome slag to the silicon carbide of 100: 0.5-1, and ball-milling the materials in a ball mill until the particle size is less than or equal to 100 mu m to obtain ferrochrome slag powder; mixing the materials according to the mass ratio of the ferrochrome slag powder to the carbon powder of 100: 2.5-4, and mixing for 0.3-0.5 hours to obtain mixed powder; adding the mixed powder into a vacuum arc furnace, heating to 1580-1760 ℃, and preserving heat for 3-5 hours; removing the upper slag layer, cooling to room temperature, and crushing to obtain plate-shaped Cr with ferrochrome slag as main material7C3. The invention has the characteristics of simple process, low production cost and no special requirement on equipment, and the plate-shaped Cr prepared by the method7C3Not only has high purity and good crystallization, but also has complete growth and development of crystal grains and excellent densification degree.
Description
Technical field
The invention belongs to Cr
7c
3technical field.Be specifically related to a kind of tabular Cr being major ingredient with ferrochrome slag
7c
3and preparation method thereof.
Background technology
The slag that namely ferrochrome slag is smelted " chromium-iron alloy " produces.Take chromite as main raw material, employing metallic aluminium powder is reductive agent, and (generally at 1850 ~ 1900 DEG C) is widely use at present and the industrial technology means of maturation by thermite reaction preparation " chromium-iron alloy " under the high temperature conditions.Because slag is different from the proportion of ferrochrome, ferrochrome slag floats on " chromium-iron alloy " upper strata, therefore the two is easy to be separated.But discarded ferrochrome slag is only used for the exploitation of low product fire resistive material product by most enterprises after industrial refuse process or simple classification at present, not only causes the waste of resource, and Cr
6+formation and the also severe contamination environment that runs off.
Cr
7c
3that (by the impact of the changeable valence state of chromium element, the carbonized product of chromium also comprises Cr to one of carbonized product of chromium
3c
2and Cr
23c
6), have that fusing point is high, hardness is large, wear resistance is good, resistance to chemical attack is excellent and the feature such as high-temperature oxidation resistance is strong, the work-ing life of machine, parts can be improved, aerospace (engine) and petrochemical industry can be widely used in.But mainly Cr is concentrated on to the carbonized product preparation research of chromium
3c
2, this is in the carbonized product due to chromium, Cr
3c
2not only modulus of volume expansion is maximum, non-deformability is the strongest and hardness is the highest, and mechanics and thermodynamic stability best; Comparatively speaking, Cr
7c
3cr-C bonding strength maximum, and the anisotropy of crystal elasticity constant is the strongest, therefore Cr
7c
3toughness better.
At present, chromium carbide (Cr is prepared
3c
2, Cr
7c
3and Cr
23c
6) method be mainly direct carborization and carbothermic method.
Direct carborization prepares chromium carbide, mainly with carbon black carbon sources such as (or) nano carbon blacks and Cr powder for raw material, through mixing, compacting and shaping after, high temperature cabonization under the condition of reducing atmosphere or shielding gas.But adopt carbon black carbon sources such as (or) nano carbon blacks and Cr powder to be that chromium carbide prepared by raw material, the temperature of its solid state reaction is higher, and the conditional request such as control climate and conversion unit is higher; In addition, in the carbonation reaction of Cr powder, need to introduce other additive (Ti powder, Zr powder etc.) toward contact, easily produce new impurity phase (TiC or ZrC etc.) in the chromium carbide of preparation, reduce the purity of chromium carbide.
Carbothermic method prepares chromium carbide, mainly with carbon black (or the carbon source such as nano carbon black, resin) and Cr
2o
3for raw material, under vacuum in certain temperature thermal treatment after premix (or pre-burning).But adopt carbothermic method to prepare chromium carbide, its reaction product (Cr
3c
2, Cr
7c
3and Cr
23c
6) wayward, be difficult to prepare the chromium carbide that purity is high, thing phase composite is single; And carbon black carbon sources such as (or) nano carbon blacks, Cr
2o
3the cost of the raw material such as (or Cr powder) and other additive is higher, further increases the preparation cost of chromium carbide.
Summary of the invention
The present invention is intended to overcome prior art defect, and object is to provide that a kind of technique is simple, production cost is low and to the tabular Cr that with ferrochrome slag be major ingredient of equipment without particular requirement
7c
3preparation method.With prepared by the method with the tabular Cr that ferrochrome slag is major ingredient
7c
3not only purity is high and advantages of good crystallization, and Grain growth is complete and densification degree is excellent.
For achieving the above object, the step of the technical solution used in the present invention is:
Step one, be 100 ︰ (0.5 ~ 1) batchings by the mass ratio of ferrochrome Zha ︰ silicon carbide, then in ball mill, be milled to granularity≤100 μm, obtain ferrochrome ground-slag end.
Step 2, be 100 ︰ (2.5 ~ 4) batchings by the mass ratio of described ferrochrome ground-slag Mo ︰ carbon dust, mix 0.3 ~ 0.5 hour, obtain mixed powder.
Step 3, described mixed powder is added in vacuum arc fumace, be warming up to 1580 ~ 1760 DEG C, be incubated 3 ~ 5 hours; Remove upper strata scum layer again, cool to room temperature, fragmentation with the furnace, be namely able to the tabular Cr that ferrochrome slag is major ingredient
7c
3.
The slag that described ferrochrome slag produces for smelting chromium irons, the dominant of ferrochrome slag is corundum and aluminium picotite mutually; The main chemical compositions of ferrochrome slag is: Al
2o
3content is 80 ~ 85wt%, Cr
2o
3content is 10 ~ 15wt%, Fe
2o
3content≤1wt%.
SiC content >=the 99wt% of described silicon carbide.
Described carbon dust is carbon black or is coke, the C content >=95wt% of carbon dust.
Owing to adopting technique scheme, the present invention compared with prior art has following positively effect:
The present invention for main raw material, adds in vacuum arc fumace with solid waste-ferrochrome slag after ball milling and mixing, and to equipment without particular requirement, not only preparation technology is simple, and significantly can reduce production cost, is suitable for industrial production application.Low melt-phase in ferrochrome slag forms liquid phase under the high temperature conditions, changes " Gu solid-" carburizing reagent into " solid-liquid " carburizing reagent, increases speed of reaction, promotion Cr
7c
3crystallization and Grain growth.In addition, in " solid-liquid " system, due to Cr
7c
3proportion maximum and be sunken to furnace bottom, reduce and the contact of other component or reaction, improve Cr
7c
3purity, the prepared tabular Cr being major ingredient with ferrochrome slag
7c
3, true density is 6.28 ~ 6.58g/cm
3, therefore densification degree is excellent.
Therefore, the present invention has that technique is simple, production cost is low and to the feature of equipment without particular requirement, the tabular Cr being major ingredient with ferrochrome slag prepared by the method
7c
3not only purity is high and advantages of good crystallization, and Grain growth is complete and densification degree is excellent.
Embodiment
Below in conjunction with embodiment, the invention will be further described, the restriction not to its protection domain:
For avoiding repetition, first by as follows for the raw material Unify legislation involved by this embodiment, repeat no more in embodiment:
The slag that described ferrochrome slag produces for smelting chromium irons, the dominant of ferrochrome slag is corundum and aluminium picotite mutually; The main chemical compositions of ferrochrome slag is: Al
2o
3content is 80 ~ 85wt%, Cr
2o
3content is 10 ~ 15wt%, Fe
2o
3content≤1wt%.
SiC content >=the 99wt% of described silicon carbide.
Described carbon dust is carbon black or is coke, the C content >=95wt% of carbon black and coke.
embodiment 1
A kind of tabular Cr that is major ingredient with ferrochrome slag
7c
3and preparation method thereof.Described in the present embodiment, the concrete steps of preparation method are:
Step one, be 100 ︰ (0.5 ~ 0.7) batchings by the mass ratio of ferrochrome Zha ︰ silicon carbide, then in ball mill, be milled to granularity≤100 μm, obtain ferrochrome ground-slag end.
Step 2, be 100 ︰ (2.5 ~ 3.1) batchings by the mass ratio of described ferrochrome ground-slag Mo ︰ carbon black, mix 0.3 ~ 0.5 hour, obtain mixed powder.
Step 3, described mixed powder is added in vacuum arc fumace, be warming up to 1688 ~ 1760 DEG C, be incubated 3.0 ~ 3.8 hours; Remove upper strata scum layer again, cool to room temperature, fragmentation with the furnace, be namely able to the tabular Cr that ferrochrome slag is major ingredient
7c
3.
The tabular Cr being major ingredient with ferrochrome slag prepared by the present embodiment
7c
3, true density is 6.46 ~ 6.58g/cm
3, densification degree is excellent.
embodiment 2
A kind of tabular Cr that is major ingredient with ferrochrome slag
7c
3and preparation method thereof.Described in the present embodiment, the concrete steps of preparation method are:
Step one, be 100 ︰ (0.6 ~ 0.8) batchings by the mass ratio of ferrochrome Zha ︰ silicon carbide, then in ball mill, be milled to granularity≤100 μm, obtain ferrochrome ground-slag end.
Step 2, be 100 ︰ (2.8 ~ 3.4) batchings by the mass ratio of described ferrochrome ground-slag Mo ︰ carbon black, mix 0.3 ~ 0.5 hour, obtain mixed powder.
Step 3, described mixed powder is added in vacuum arc fumace, be warming up to 1652 ~ 1724 DEG C, be incubated 3.4 ~ 4.2 hours; Remove upper strata scum layer again, cool to room temperature, fragmentation with the furnace, be namely able to the tabular Cr that ferrochrome slag is major ingredient
7c
3.
The tabular Cr being major ingredient with ferrochrome slag prepared by the present embodiment
7c
3, true density is 6.40 ~ 6.52g/cm
3, densification degree is excellent.
embodiment 3
A kind of tabular Cr that is major ingredient with ferrochrome slag
7c
3and preparation method thereof.Described in the present embodiment, the concrete steps of preparation method are:
Step one, be 100 ︰ (0.7 ~ 0.9) batchings by the mass ratio of ferrochrome Zha ︰ silicon carbide, then in ball mill, be milled to granularity≤100 μm, obtain ferrochrome ground-slag end.
Step 2, be 100 ︰ (3.1 ~ 3.7) batchings by the mass ratio of described ferrochrome ground-slag Mo ︰ coke, mix 0.3 ~ 0.5 hour, obtain mixed powder.
Step 3, described mixed powder is added in vacuum arc fumace, be warming up to 1616 ~ 1688 DEG C, be incubated 3.8 ~ 4.6 hours; Remove upper strata scum layer again, cool to room temperature, fragmentation with the furnace, be namely able to the tabular Cr that ferrochrome slag is major ingredient
7c
3.
The tabular Cr being major ingredient with ferrochrome slag prepared by the present embodiment
7c
3, true density is 6.34 ~ 6.46g/cm
3, densification degree is excellent.
embodiment 4
A kind of tabular Cr that is major ingredient with ferrochrome slag
7c
3and preparation method thereof.Described in the present embodiment, the concrete steps of preparation method are:
Step one, be 100 ︰ (0.8 ~ 1.0) batchings by the mass ratio of ferrochrome Zha ︰ silicon carbide, then in ball mill, be milled to granularity≤100 μm, obtain ferrochrome ground-slag end.
Step 2, be 100 ︰ (3.4 ~ 4.0) batchings by the mass ratio of described ferrochrome ground-slag Mo ︰ coke, mix 0.3 ~ 0.5 hour, obtain mixed powder.
Step 3, described mixed powder is added in vacuum arc fumace, be warming up to 1580 ~ 1652 DEG C, be incubated 4.2 ~ 5.0 hours; Remove upper strata scum layer again, cool to room temperature, fragmentation with the furnace, be namely able to the tabular Cr that ferrochrome slag is major ingredient
7c
3.
The tabular Cr being major ingredient with ferrochrome slag prepared by the present embodiment
7c
3, true density is 6.28 ~ 6.40g/cm
3, therefore densification degree is excellent.
This embodiment compared with prior art has following positively effect:
This embodiment for main raw material, adds in vacuum arc fumace with solid waste-ferrochrome slag after ball milling and mixing, and to equipment without particular requirement, not only preparation technology is simple, and significantly can reduce production cost, is suitable for industrial production application.Low melt-phase in ferrochrome slag forms liquid phase under the high temperature conditions, changes " Gu solid-" carburizing reagent into " solid-liquid " carburizing reagent, increases speed of reaction, promotion Cr
7c
3crystallization and Grain growth.In addition, in " solid-liquid " system, due to Cr
7c
3proportion maximum and be sunken to furnace bottom, reduce and the contact of other component or reaction, improve Cr
7c
3purity, the prepared tabular Cr being major ingredient with ferrochrome slag
7c
3true density be 6.28 ~ 6.58g/cm
3, therefore densification degree is excellent.
Therefore, this embodiment has that technique is simple, production cost is low and to the feature of equipment without particular requirement, the tabular Cr being major ingredient with ferrochrome slag prepared by the method
7c
3not only purity is high and advantages of good crystallization, and Grain growth is complete and densification degree is excellent.
Claims (5)
1. the tabular Cr that is major ingredient with ferrochrome slag
7c
3preparation method, it is characterized in that the step of described preparation method is:
Step one, be 100 ︰ (0.5 ~ 1) batchings by the mass ratio of ferrochrome Zha ︰ silicon carbide, then in ball mill, be milled to granularity≤100 μm, obtain ferrochrome ground-slag end;
Step 2, be 100 ︰ (2.5 ~ 4) batchings by the mass ratio of described ferrochrome ground-slag Mo ︰ carbon dust, mix 0.3 ~ 0.5 hour, obtain mixed powder;
Step 3, described mixed powder is added in vacuum arc fumace, be warming up to 1580 ~ 1760 DEG C, be incubated 3 ~ 5 hours; Remove upper strata scum layer again, cool to room temperature, fragmentation with the furnace, be namely able to the tabular Cr that ferrochrome slag is major ingredient
7c
3.
2. the tabular Cr that is major ingredient with ferrochrome slag according to claim 1
7c
3preparation method, it is characterized in that the slag that described ferrochrome slag produces for smelting chromium irons, the dominant of ferrochrome slag is corundum and aluminium picotite mutually; The main chemical compositions of ferrochrome slag is: Al
2o
3content is 80 ~ 85wt%, Cr
2o
3content is 10 ~ 15wt%, Fe
2o
3content≤1wt%.
3. the tabular Cr that is major ingredient with ferrochrome slag according to claim 1
7c
3preparation method, it is characterized in that the SiC content>=99wt% of described silicon carbide.
4. the tabular Cr that is major ingredient with ferrochrome slag according to claim 1
7c
3preparation method, it is characterized in that described carbon dust is carbon black or for coke, the C content>=95wt% of carbon dust.
5. the tabular Cr that is major ingredient with ferrochrome slag
7c
3, it is characterized in that the described tabular Cr being major ingredient with ferrochrome slag
7c
3the tabular Cr being major ingredient with ferrochrome slag according to any one of claim 1 ~ 4
7c
3the tabular Cr being major ingredient with ferrochrome slag prepared by preparation method
7c
3.
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Cited By (6)
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CN106083094A (en) * | 2016-06-27 | 2016-11-09 | 武汉科技大学 | A kind of copper converter tuyere brick and preparation method thereof |
CN106966730A (en) * | 2017-03-24 | 2017-07-21 | 武汉科技大学 | A kind of fine and close TiC materials and preparation method thereof |
CN105541359B (en) * | 2016-01-18 | 2018-01-12 | 武汉科技大学 | A kind of ladle splash guard castable refractory and preparation method thereof |
CN107759207A (en) * | 2017-11-20 | 2018-03-06 | 武汉科技大学 | Using aluminium chromium slag as blast furnace iron outlet groove castable of major ingredient and preparation method thereof |
CN111500878A (en) * | 2020-04-30 | 2020-08-07 | 渤海大学 | Method for preparing chromium metal by using chromium carbide |
CN111500921A (en) * | 2020-04-29 | 2020-08-07 | 辽宁工业大学 | Method for preparing ferrochromium nitride from aluminum-chromium waste residues |
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JPH0523848A (en) * | 1991-07-19 | 1993-02-02 | Toyota Motor Corp | Cladding method for engine valve |
CN203751141U (en) * | 2014-03-14 | 2014-08-06 | 宁波甬抚机械有限公司 | Cold-punching mold with repairable surface |
-
2015
- 2015-10-09 CN CN201510647704.2A patent/CN105152652B/en active Active
Patent Citations (2)
Publication number | Priority date | Publication date | Assignee | Title |
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JPH0523848A (en) * | 1991-07-19 | 1993-02-02 | Toyota Motor Corp | Cladding method for engine valve |
CN203751141U (en) * | 2014-03-14 | 2014-08-06 | 宁波甬抚机械有限公司 | Cold-punching mold with repairable surface |
Cited By (7)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN105541359B (en) * | 2016-01-18 | 2018-01-12 | 武汉科技大学 | A kind of ladle splash guard castable refractory and preparation method thereof |
CN106083094A (en) * | 2016-06-27 | 2016-11-09 | 武汉科技大学 | A kind of copper converter tuyere brick and preparation method thereof |
CN106083094B (en) * | 2016-06-27 | 2019-03-19 | 武汉科技大学 | A kind of copper converter tuyere brick and preparation method thereof |
CN106966730A (en) * | 2017-03-24 | 2017-07-21 | 武汉科技大学 | A kind of fine and close TiC materials and preparation method thereof |
CN107759207A (en) * | 2017-11-20 | 2018-03-06 | 武汉科技大学 | Using aluminium chromium slag as blast furnace iron outlet groove castable of major ingredient and preparation method thereof |
CN111500921A (en) * | 2020-04-29 | 2020-08-07 | 辽宁工业大学 | Method for preparing ferrochromium nitride from aluminum-chromium waste residues |
CN111500878A (en) * | 2020-04-30 | 2020-08-07 | 渤海大学 | Method for preparing chromium metal by using chromium carbide |
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