CN113753898A - Method for improving purity of calcium carbide - Google Patents

Method for improving purity of calcium carbide Download PDF

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Publication number
CN113753898A
CN113753898A CN202110957646.9A CN202110957646A CN113753898A CN 113753898 A CN113753898 A CN 113753898A CN 202110957646 A CN202110957646 A CN 202110957646A CN 113753898 A CN113753898 A CN 113753898A
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calcium carbide
vacuum
liquid
purity
vacuum equipment
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张曦东
李涛
杨卫中
魏昭峰
卢伟
白京磊
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Shougang Group Co Ltd
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Shougang Group Co Ltd
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    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01BNON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B32/00Carbon; Compounds thereof
    • C01B32/90Carbides
    • C01B32/914Carbides of single elements
    • C01B32/942Calcium carbide
    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01PINDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2006/00Physical properties of inorganic compounds
    • C01P2006/80Compositional purity

Abstract

The invention provides a method for improving the purity of calcium carbide, belonging to the technical field of calcium carbide production, and the method comprises the following steps: injecting calcium carbide liquid into vacuum equipment, wherein the vacuum equipment heats the calcium carbide liquid under a vacuum condition; after the liquid level of the calcium carbide liquid in the vacuum equipment is stable, pouring the calcium carbide liquid under a vacuum condition, and then cooling to obtain calcium carbide; the gas pressure in the vacuum equipment is controlled to be 1.3-47 kPa, the heating temperature of the vacuum equipment is 1950-2000 ℃, and the vacuum heat preservation time of the calcium carbide liquid in the vacuum equipment is 20-40 min. The method can obviously improve the purity of the calcium carbide, does not influence the production efficiency of the calcium carbide furnace, and does not improve the energy consumption and the carbon material consumption of the calcium carbide furnace.

Description

Method for improving purity of calcium carbide
Technical Field
The invention belongs to the technical field of calcium carbide production, and particularly relates to a method for improving the purity of calcium carbide.
Background
The main component of the calcium carbide is CaC2,CaC2The higher the content, the better the quality. The industrial production method of calcium carbide is to heat carbon material (coke, blue) in calcium carbide furnaceCharcoal and anthracite) and lime, the calcium carbide furnace reaches the high temperature of 1800-2200 ℃, and the chemical reaction CaO + C → CaC occurs2+ CO ℃, (d) generating liquid calcium carbide, namely calcium carbide liquid. The prepared calcium carbide contains unreacted impurities such as free CaO, carbon particles and the like, and the purity of the calcium carbide is influenced.
The specific forming process of the calcium carbide comprises the following steps:
(1) lime blocks in the raw materials are firstly melted into liquid, and lime liquid permeates into capillary pores of the carbon material and reacts with carbon to generate CaC2
(2) Generated CaC2Quickly diluted by lime liquor to form eutectic body with low melting point, and most easily formed into CaC269-70% of low-melting-point eutectic.
(3) And discharging the calcium carbide liquid from the furnace at 1900-2000 ℃, and flowing into a cast steel or cast iron calcium carbide pot.
(4) Cooling and solidifying the calcium carbide liquid in the calcium carbide pot. Although the temperature of the calcium carbide liquid is higher than the melting point of the calcium carbide pot, the calcium carbide liquid can be rapidly cooled and cannot melt the calcium carbide pot due to the fact that the heat dissipation of the calcium carbide pot is fast and the heat absorption capacity is large.
(5) The condensed calcium carbide is lifted out by a hoisting machine, and then is crushed and packaged to form the calcium carbide product.
From the above process, when CaC is used2When the content is 69-70%, the melting point of the calcium carbide is lowest, and the low-purity calcium carbide is easy to form. In order to increase CaC in calcium carbide2The content is increased to 70-80%. The method commonly adopted in the calcium carbide industry is as follows:
(1) the furnace temperature is increased by prolonging the residence time of calcium carbide liquid in the furnace, and the generation of calcium carbide is promoted;
(2) the carbon material proportion in the raw materials is improved.
The problems with these two methods are:
(1) the scheme of increasing the furnace temperature by prolonging the residence time of the calcium carbide liquid in the calcium carbide furnace increases the power consumption and reduces the production efficiency of the calcium carbide furnace.
(2) The scheme of improving the carbon material ratio in the raw materials is beneficial to reducing the dilution of the calcium carbide liquid by the lime liquid, but increases the carbon material consumption, and causes the reduction of the specific resistance of the furnace charge, the increase of the material layer current and the increase of the material surface temperature. The surface temperature is increased, the specific resistance of the furnace charge is reduced, and vicious circle is formed. If the height of the electrode is increased to reduce the current, the open arc operation is easy to be caused, the electric energy loss is increased, and the service life of the refractory material is shortened.
(3) Even though the purity of the calcium carbide liquid can be improved by the two schemes, the melting point of the calcium carbide liquid is increased, the fluidity is poor, and the calcium carbide liquid is difficult to discharge.
How to improve the purity of the calcium carbide without reducing the production efficiency of the calcium carbide furnace, increasing the power consumption of the calcium carbide furnace and increasing the consumption of carbon materials is always a problem for technical personnel in the industry.
Disclosure of Invention
In order to solve the technical problems, the invention provides a method for improving the purity of calcium carbide, which can obviously improve the purity of the calcium carbide, does not influence the production efficiency of a calcium carbide furnace, and does not improve the energy consumption and carbon material consumption of the calcium carbide furnace.
The invention is realized by the following technical scheme:
the embodiment of the invention provides a method for improving calcium carbide purity, which comprises the following steps:
injecting calcium carbide liquid into vacuum equipment, wherein the vacuum equipment heats the calcium carbide liquid under a vacuum condition;
after the liquid level of the calcium carbide liquid in the vacuum equipment is stable, pouring the calcium carbide liquid under a vacuum condition, and then cooling to obtain calcium carbide;
the gas pressure in the vacuum equipment is controlled to be 1.3-47 kPa, the heating temperature of the vacuum equipment is 1950-2000 ℃, and the vacuum heat preservation time of the calcium carbide liquid in the vacuum equipment is 20-40 min.
Further, before the calcium carbide liquid is injected into the vacuum equipment, CaC2The content is 69-80%.
Further, the temperature of the calcium carbide liquid when being injected into the vacuum equipment is 1850-.
Further, before the calcium carbide liquid is injected into the vacuum equipment, the calcium carbide liquid is prepared by a calcium carbide furnace.
Further, before the calcium carbide liquid is injected into the vacuum equipment, the calcium carbide liquid is prepared through a calcium carbide furnace and then enters a refractory container, and the calcium carbide liquid is injected into the vacuum equipment through the refractory container.
Furthermore, the refractory container is lined with alumina bricks.
Further, the vacuum equipment is a vacuum induction furnace.
Further, the calcium carbide liquid is heated in a graphite crucible of the vacuum induction furnace.
Further, the calcium carbide liquid is poured under a vacuum condition and then cooled to obtain the calcium carbide, and the method specifically comprises the following steps:
and pouring the calcium carbide liquid under a vacuum condition, and cooling to obtain the calcium carbide, wherein the cooling adopts vacuum cooling or air cooling after the calcium carbide liquid is discharged from a furnace.
Further, the casting mould for casting the calcium carbide liquid under the vacuum condition is an iron mould.
One or more technical solutions in the embodiments of the present invention have at least the following technical effects or advantages:
according to the method for improving the purity of the calcium carbide provided by the embodiment of the invention, calcium carbide liquid produced by the calcium carbide furnace is injected into vacuum equipment for external refining, the partial pressure of CO is reduced by creating a vacuum environment, and CaO and C which do not participate in the reaction in the calcium carbide are promoted to continuously generate CaC by combining reasonable negative pressure, reaction temperature and reaction time control2Further improve the purity of the calcium carbide, does not increase the energy consumption and the raw material consumption for manufacturing the calcium carbide, improves the production efficiency and overcomes the defect of CaC2The increase of the concentration causes the increase of the melting point of the calcium carbide liquid, the deterioration of the fluidity and the difficulty in discharging.
The foregoing description is only an overview of the technical solutions of the present invention, and the embodiments of the present invention are described below in order to make the technical means of the present invention more clearly understood and to make the above and other objects, features, and advantages of the present invention more clearly understandable.
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In order to more clearly illustrate the technical solutions in the embodiments of the present invention, the drawings needed to be used in the description of the embodiments are briefly introduced below, and it is obvious that the drawings in the following description are some embodiments of the present invention, and it is obvious for those skilled in the art to obtain other drawings based on these drawings without creative efforts.
FIG. 1 is a process flow diagram of an embodiment of the invention.
Detailed Description
The present invention will be described in detail below with reference to specific embodiments and examples, and the advantages and various effects of the present invention will be more clearly apparent therefrom. It will be understood by those skilled in the art that these specific embodiments and examples are for the purpose of illustrating the invention and are not to be construed as limiting the invention.
Throughout the specification, unless otherwise specifically noted, terms used herein should be understood as having meanings as commonly used in the art. Accordingly, unless defined otherwise, all technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art to which this invention belongs. If there is a conflict, the present specification will control.
Unless otherwise specifically stated, various raw materials, reagents, instruments, equipment and the like used in the present invention are commercially available or can be prepared by existing methods.
It should be further noted that the terms "comprises," "comprising," or any other variation thereof, are intended to cover a non-exclusive inclusion, such that a process, method, article, or apparatus that comprises a list of elements does not include only those elements but may include other elements not expressly listed or inherent to such process, method, article, or apparatus.
Meanwhile, the terms "first", "second", etc. in the present invention do not denote any order or order, and these words may be interpreted as names.
In order to solve the technical problems, the embodiment of the invention provides the following general ideas:
in the existing calcium carbide production process, in order to increase the concentration of calcium carbide, the retention time of calcium carbide liquid in a furnace is usually prolonged to increase the furnace temperature or increase the raw material carbon material ratio, so that the consumption of energy and raw materials is increased, the production efficiency of the calcium carbide furnace is reduced, and the CaC is used2The increase of the concentration causes the increase of the melting point of the calcium carbide liquid, the deterioration of the fluidity, the difficulty in discharging the calcium carbide liquid, and the increase of the production difficulty.
Based on the reasons, the calcium carbide liquid produced by the calcium carbide furnace is refined outside the furnace through the vacuum induction furnace, the partial pressure of C0 is reduced by using the vacuum condition, and the CaO and C which do not participate in the reaction in the calcium carbide are promoted to continuously generate CaC2Further improve the purity of the calcium carbide. The essence of the process is the post-treatment of the calcium carbide liquid outside the calcium carbide furnace, so that the production operation of the original calcium carbide furnace is not influenced, for example, the proportion of raw material carbon materials does not need to be improved, the temperature of the calcium carbide furnace does not need to be additionally improved, the retention time of the calcium carbide liquid in the furnace is not prolonged, and the consumption of energy and raw materials is reduced on the basis of improving the purity of the calcium carbide. The discharge of the calcium carbide liquid is carried out by a vacuum induction furnace, thereby overcoming the defect of CaC2The increase of the concentration causes the increase of the melting point of the calcium carbide liquid, the deterioration of the fluidity and the difficulty in discharging.
According to a typical embodiment of the present invention, an embodiment of the present invention provides a method for improving purity of calcium carbide, as shown in fig. 1, the method includes:
s1, injecting calcium carbide liquid into vacuum equipment, wherein the vacuum equipment heats the calcium carbide liquid under a vacuum condition;
s2, after the liquid level of the calcium carbide liquid in the vacuum equipment is stable, pouring the calcium carbide liquid under a vacuum condition, and cooling to obtain calcium carbide;
the gas pressure in the vacuum equipment is controlled to be 1.3-47 kPa, the heating temperature of the vacuum equipment is 1950-2000 ℃, and the vacuum heat preservation time of the calcium carbide liquid in the vacuum equipment is 20-40 min.
If the absolute pressure of the gas in the vacuum equipment is more than 47kPa, the degassing effect is not obvious, and the chemical reaction is slow;
vacuum equipmentIf the absolute pressure of the gas in the calcium carbide is less than 1.3kPa, the calcium carbide liquid is obviously reduced because the CaC is promoted by the too low gas pressure2Decomposing to generate calcium vapor and dissipating.
As an optional implementation mode, before the calcium carbide liquid is injected into the vacuum equipment, CaC is adopted2The content is 69-80%.
As an optional implementation mode, the temperature of the calcium carbide liquid when being injected into the vacuum equipment is 1850-.
As an optional embodiment, before the calcium carbide liquid is injected into the vacuum equipment, the calcium carbide liquid is prepared by a calcium carbide furnace.
As an optional implementation manner, before the calcium carbide liquid is injected into the vacuum equipment, the calcium carbide liquid is prepared through a calcium carbide furnace, and then enters a refractory container, and the calcium carbide liquid is injected into the vacuum equipment through the refractory container, wherein the refractory container is lined with an alumina brick.
As an alternative embodiment, the vacuum apparatus is a vacuum induction furnace, and a vacuum arc furnace may also be used.
As an optional embodiment, the calcium carbide liquid is heated in a graphite crucible of the vacuum induction furnace.
As an optional embodiment, the casting of the calcium carbide liquid under vacuum condition, and then cooling to obtain the calcium carbide specifically include:
and (3) pouring the calcium carbide liquid under a vacuum condition, and then cooling to obtain the calcium carbide, wherein the pouring mold is an iron mold, and the cooling is carried out under the vacuum condition or is carried out in the air after the calcium carbide liquid is discharged from the furnace.
According to the embodiment of the invention, calcium carbide liquid produced by the calcium carbide furnace is injected into the vacuum induction furnace for refining outside the furnace, the partial pressure of CO is reduced by creating a vacuum environment, and reasonable negative pressure, reaction temperature and reaction time control are combined to promote CaO and C which do not participate in the reaction in the calcium carbide to continuously generate CaC2Further improve the purity of the calcium carbide, does not increase the energy consumption and the raw material consumption for manufacturing the calcium carbide, improves the production efficiency and overcomes the defect of CaC2The concentration is increased to cause the calcium carbide liquidThe melting point is increased, the fluidity is poor, and the tapping is difficult.
The method for improving the purity of the calcium carbide according to the present application will be described in detail below with reference to examples, comparative examples and experimental data.
Examples
A method for improving the purity of calcium carbide comprises the following steps:
(1) the initial temperature is 1850-2Allowing 69-80% calcium carbide liquid to flow from a discharge port of the calcium carbide furnace to a baked refractory container;
(2) injecting calcium carbide liquid into a graphite crucible in a vacuum induction furnace through a refractory container, and heating under a vacuum condition, wherein the heating temperature is 1950-2000 ℃, so that the calcium carbide is kept in a liquid state, and the gas pressure in the vacuum induction furnace is controlled to be 1.3-47 kPa;
(3) and (3) heating in vacuum for 20-40 min, after the internal chemical reaction of the calcium carbide liquid is basically completed and the liquid level is stable, pouring the calcium carbide liquid into an iron mold under the vacuum condition, and cooling in the air after the calcium carbide liquid is broken and discharged from the furnace.
The method is provided with 4 embodiments, 100kg of calcium carbide liquid with different purities is respectively injected into a graphite crucible of a vacuum induction furnace with the rated capacity of 500kg for vacuum heat preservation treatment, and the calcium carbide liquid GaC in each embodiment2Concentration, process parameters and calcium carbide CaC after vacuum treatment2The contents are shown in table 1:
in table 1, the purity of calcium carbide was measured using an instrument: the LJD type calcium carbide gas evolution measuring device and the detection method are disclosed in GB 10665. Table 1 examples 1-4 calcium carbide CaC after vacuum treatment2Content (wt.)
Figure BDA0003219916680000051
In the prior art, if a calcium carbide furnace is used for producing CaC2The low-purity calcium carbide with the content of about 70 percent has the power consumption of about 3200-3300 kWh/t, and if the CaC is treated by measures such as increasing the furnace temperature or the reaction time and the like2The content is improved to more than 80 percent, the power consumption is about 3500-3600 kWh/t, and the power consumption is increased by about 300 kWh/t. While the vacuum method of the invention is adopted to treatThe power consumption of the pure calcium carbide liquid is about 100-200 kWh/t.
CaC2When the content is 69-70%, the melting point of the calcium carbide is 1760-1800 ℃. When CaC2When the content is increased to more than 80%, the melting point is close to 2000 ℃. When the calcium carbide furnace discharges materials, the calcium carbide liquid has poor fluidity and discharges materials slowly, and even solidifies to block the discharge hole due to the increase of the melting point of the calcium carbide.
From examples 1-4, it can be seen that the calcium carbide liquid produced by the calcium carbide furnace is injected into the vacuum induction furnace for external refining, the partial pressure of CO is reduced by creating a vacuum environment, and CaO and C which do not participate in the reaction in the calcium carbide are promoted to continuously generate CaC by combining reasonable negative pressure, reaction temperature and reaction time control2The purity of the calcium carbide is obviously improved. The energy consumption and the consumption of carbon raw materials for manufacturing calcium carbide are not increased, the production efficiency is improved, and the defect of CaC2The increase of the concentration causes the increase of the melting point of the calcium carbide liquid, the deterioration of the fluidity and the difficulty in discharging.
One or more technical solutions in the embodiments of the present invention at least have the following technical effects or advantages:
(1) in the embodiment of the invention, calcium carbide liquid produced by the calcium carbide furnace is injected into the vacuum induction furnace for external refining, the partial pressure of CO is reduced by creating a vacuum environment, and reasonable negative pressure, reaction temperature and reaction time control are combined to promote CaO and C which do not participate in the reaction in the calcium carbide to continuously generate CaC2The purity of the calcium carbide is obviously improved.
(2) In the embodiment of the invention, on the basis of ensuring the improvement of the purity of the calcium carbide, the energy consumption and the consumption of carbon raw materials for manufacturing the calcium carbide are not increased, the production efficiency is improved, and the defect of GaC2The increase of the concentration causes the increase of the melting point of the calcium carbide liquid, the deterioration of the fluidity and the difficulty in discharging.
Finally, it should also be noted that the terms "comprises," "comprising," or any other variation thereof, are intended to cover a non-exclusive inclusion, such that a process, method, article, or apparatus that comprises a list of elements does not include only those elements but may include other elements not expressly listed or inherent to such process, method, article, or apparatus.
While preferred embodiments of the present invention have been described, additional variations and modifications in those embodiments may occur to those skilled in the art once they learn of the basic inventive concepts. Therefore, it is intended that the appended claims be interpreted as including preferred embodiments and all such alterations and modifications as fall within the scope of the invention.
It will be apparent to those skilled in the art that various changes and modifications may be made in the present invention without departing from the spirit and scope of the invention. Thus, if such modifications and variations of the present invention fall within the scope of the claims of the present invention and their equivalents, the present invention is also intended to include such modifications and variations.

Claims (10)

1. A method for improving the purity of calcium carbide is characterized by comprising the following steps:
injecting calcium carbide liquid into vacuum equipment, wherein the vacuum equipment heats the calcium carbide liquid under a vacuum condition;
after the liquid level of the calcium carbide liquid in the vacuum equipment is stable, pouring the calcium carbide liquid under a vacuum condition, and then cooling to obtain calcium carbide;
the gas pressure in the vacuum equipment is controlled to be 1.3-47 kPa, the heating temperature of the vacuum equipment is 1950-2000 ℃, and the vacuum heat preservation time of the calcium carbide liquid in the vacuum equipment is 20-40 min.
2. The method for improving the purity of calcium carbide according to claim 1, wherein the CaC is added to the calcium carbide liquid before the calcium carbide liquid is injected into the vacuum equipment2The content is 69-80%.
3. The method as claimed in claim 1, wherein the temperature of the calcium carbide liquid during the injection into the vacuum apparatus is 1850-.
4. The method for improving the purity of calcium carbide according to claim 1, wherein the calcium carbide liquid is prepared by a calcium carbide furnace before being injected into the vacuum equipment.
5. The method for improving the purity of calcium carbide according to claim 1, wherein the calcium carbide liquid is prepared by a calcium carbide furnace before being injected into the vacuum equipment, and then enters a refractory container, and the calcium carbide liquid is injected into the vacuum equipment through the refractory container.
6. The method for improving the purity of calcium carbide according to claim 5, wherein the refractory container is lined with alumina bricks.
7. The method for improving the purity of calcium carbide according to claim 1, wherein the vacuum equipment is a vacuum induction furnace.
8. The method for improving the purity of calcium carbide according to claim 7, wherein the calcium carbide liquid is heated in a graphite crucible of the vacuum induction furnace.
9. The method for improving the purity of calcium carbide according to claim 1, wherein the calcium carbide liquid is poured under vacuum and then cooled to obtain the calcium carbide, and the method specifically comprises the following steps:
and pouring the calcium carbide liquid under a vacuum condition, and cooling to obtain the calcium carbide, wherein the cooling adopts vacuum cooling or air cooling after the calcium carbide liquid is discharged from a furnace.
10. The method for improving the purity of calcium carbide according to claim 9, wherein the casting mold for casting the calcium carbide liquid under vacuum is an iron mold.
CN202110957646.9A 2021-08-19 2021-08-19 Method for improving purity of calcium carbide Pending CN113753898A (en)

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CN107857267A (en) * 2017-12-12 2018-03-30 中国科学院上海高等研究院 A kind of method that vacuum low-pressure prepares calcium carbide
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CN106865550A (en) * 2017-03-06 2017-06-20 武汉科技大学 A kind of calcium carbide with ardealite as major ingredient and preparation method thereof
CN107089661A (en) * 2017-06-16 2017-08-25 中国石油大学(华东) A kind of calcium focal sphere group classification hot legal system power taking stone production technology of oxygen
CN107857267A (en) * 2017-12-12 2018-03-30 中国科学院上海高等研究院 A kind of method that vacuum low-pressure prepares calcium carbide
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