CN106115702A - The method of preparation solid-state carbide - Google Patents
The method of preparation solid-state carbide Download PDFInfo
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- CN106115702A CN106115702A CN201610430256.5A CN201610430256A CN106115702A CN 106115702 A CN106115702 A CN 106115702A CN 201610430256 A CN201610430256 A CN 201610430256A CN 106115702 A CN106115702 A CN 106115702A
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- bituminous coal
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- calcium fluoride
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Abstract
The method that the invention discloses preparation solid-state carbide.The method includes: bituminous coal, calcic raw material and additive are carried out fine grinding process respectively, in order to obtaining bituminous coal granule, calcic feed particles and calcium fluoride particles, wherein, described bituminous coal is high volatile, low ash bituminous coal；Described bituminous coal granule, described calcic feed particles and described calcium fluoride particles carry out mix pressure ball process, in order to obtain mixed material agglomerate；Described mixed material agglomerate is carried out pyrolysis processing, in order to the pelletizing after being pyrolyzed and the flue gas containing volatile matter；And the pelletizing after described pyrolysis is carried out calcination process, in order to obtain solid-state carbide.The method is by adding containing lithium carbonate and the additive of calcium fluoride in smelting process, achieve to smelt under cryogenic and produce carbide, simultaneously, raw material is carried out fine grinding process, improve raw material specific surface area and contact area, improve raw material mass transfer and heat transfer efficiency, improve reaction rate, reduce carbide smelting temperature and energy consumption.
Description
Technical field
The method that the present invention relates to prepare solid-state carbide.
Background technology
Carbide is important Coal Chemical Industry product and basic chemical industry raw material, mainly for the production of acetylene and acetenyl chemical industry
Product, is particularly useful for producing polrvinyl chloride, was once described as " mother of organic synthesis industry ", and it is mainly composed of CaC2, current work
Produce carbide in industry and all use electrothermal way.
Electrothermal way technique mainly use electric furnace to produce carbonaceous material and calcic thing that carbide, specially granularity are 5～30mm
Material in electric furnace by electric arc heated to 2000 DEG C more than, under hot environment carbon reduction-oxidation calcium generate CaC2Product, liquid
Carbide material from furnace bottom be interrupted discharge.Though this production technology experience the updating and optimize of many decades, still suffer from
Lower problem: 1) use high-quality carbon raw (coke, anthracite etc.), production cost is higher；2) use block carbon former in producing
Material and Calx, mass transfer and heat transfer efficiency are low, and reaction rate is relatively low；3) electric arc heated, the conversion efficiency of thermoelectric of power generation process are used
Being only about 40%, general power consumption is 3200～3600kwh/t carbides, and smelting cycle is long, and energy consumption is higher；4) carbide produced produces
Product are liquid, and the erosion for stove, electrode is serious；In addition the process of liquid carbide needs the cooling of carbide crucible, the demoulding, crushes
Operation, complex process, environmental pollution is serious.
Thus, the method for preparation solid-state carbide haves much room for improvement.
Summary of the invention
It is contemplated that at least solve one of technical problem present in prior art.To this end, one object of the present invention
Being the method that carbide is prepared in proposition, the method contains lithium carbonate and the additive of calcium fluoride by adding in smelting process,
Achieving to smelt under cryogenic and produce carbide, and the energy consumption of the method is little, production capacity is high.
It should be noted that the present invention is following work based on inventor and completes:
The fusing point of calcium fluoride is relatively low, is 1423 DEG C, is also liquid under test temperature, former at carbon raw and calcio equally
Form liquid phase diffusion admittance between material, accelerate carbon and CaO diffusion to each other.Additionally, calcium fluoride is possible not only to provide calcium source, simultaneously
F-As anion, the ionic radius of its ionic radius and oxygen is more or less the same, and can enter CaO lattice, makes lattice activate, and is conducive to
Carbon and the diffusion inside of CaO, reduce the activation energy producing carbide reaction simultaneously, make carbide to produce at a lower temperature.
The studies above based on inventor, inventor adds calcium fluoride in the reaction prepare carbide, can effectively facilitate electricity
Stone reaction is carried out at low ambient temperatures, improves carbide quality.
Thus, according to an aspect of the present invention, the invention provides a kind of method preparing solid-state carbide.According to this
Bright embodiment, the method includes: bituminous coal, calcic raw material and additive are carried out fine grinding process, in order to obtains bituminous coal granule, contain
Calcium feed particles and calcium fluoride particles, wherein, described bituminous coal is high volatile, low ash bituminous coal；By described bituminous coal granule, described
Calcic feed particles and described calcium fluoride particles carry out mixing pressure ball and process, in order to obtain mixed material agglomerate；By described mixing
Material agglomerate carries out pyrolysis processing, in order to the pelletizing after being pyrolyzed and the flue gas containing volatile matter；And by after described pyrolysis
Pelletizing carry out calcination process, in order to obtain solid-state carbide.
The method preparing carbide according to embodiments of the present invention, on the one hand by adding calcium fluoride in smelting process, real
Show to smelt under cryogenic and produced carbide, on the other hand, raw material has been carried out fine grinding process, improve raw material specific surface area, increase
The contact area of big two kinds of raw materials, improves raw material mass transfer and heat transfer efficiency, improves reaction rate, reduces carbide and smelts reaction temperature
Degree and process energy consumption.Additionally, smelting reaction temperature is low, the requirement to equipment thermostability reduces further, thus reduces equipment and throw
Money cost.
It addition, the method preparing carbide according to the above embodiment of the present invention can also have following additional technology spy
Levy:
According to embodiments of the invention, the mean diameter of described bituminous coal granule is 70～120 μm；Described calcic feed particles
Mean diameter be 10～30 μm；The mean diameter of described calcium fluoride particles is 30～50 μm.
According to embodiments of the invention, described bituminous coal, described calcic raw material and described calcium fluoride particles in mass ratio 100:
(100～200): (3～15) carry out described mixing pressure ball and process.
According to embodiments of the invention, described calcic raw material is limestone.
According to embodiments of the invention, the calcium oxide content of described calcic raw material is not less than 50 mass %.
According to embodiments of the invention, the volatile matter content of described bituminous coal is 25%～35%, content of ashes be 4%～
8%
According to embodiments of the invention, the temperature of described pyrolysis processing is 1000～1200 DEG C.
According to embodiments of the invention, the temperature of described calcination process is 1500 DEG C～1800 DEG C, and the time is 30～90 points
Clock.
According to embodiments of the invention, described calcination process is carried out under an argon atmosphere.
According to embodiments of the invention, the method farther includes: before described fine grinding processes, to described bituminous coal and described
Calcic raw material is dried process, in order to obtain dried bituminous coal and calcic raw material.
According to embodiments of the invention, utilize the described flue gas containing volatile matter as the combustion needed for described pyrolysis processing
Material.
The additional aspect of the present invention and advantage will part be given in the following description, and part will become from the following description
Obtain substantially, or recognized by the practice of the present invention.
Accompanying drawing explanation
Above-mentioned and/or the additional aspect of the present invention and advantage are from combining the accompanying drawings below description to embodiment and will become
Substantially with easy to understand, wherein:
Fig. 1 shows the schematic flow sheet of the method preparing solid-state carbide according to an embodiment of the invention.
Detailed description of the invention
Embodiments of the invention are described below in detail, and the example of described embodiment is shown in the drawings.Below with reference to
The embodiment that accompanying drawing describes is exemplary, is only used for explaining the present invention, and is not considered as limiting the invention.
According to an aspect of the present invention, the invention provides a kind of method preparing solid-state carbide.Reference Fig. 1, according to
Embodiments of the invention, explain this method preparing carbide, and the method includes:
S100 fine grinding processes
According to embodiments of the invention, bituminous coal, calcic raw material and calcium fluoride are carried out fine grinding process, obtain bituminous coal granule,
Calcic feed particles and calcium fluoride particles, wherein, bituminous coal is high volatile, low ash bituminous coal, and in coal, volatile matter is subject to when pyrolysis
Heat is volatized in flue gas, makes to there is a large amount of imflammable gas in flue gas, and flue gas can return to pyrolysis oven and uses as fuel, reduces
The use of other fuel.Meanwhile, at this, the effect to calcium fluoride is specifically described, and the fusing point of calcium fluoride is relatively low, is 1423 DEG C,
Also be liquid under test temperature, between carbon raw and calcio raw material, form liquid phase diffusion admittance equally, accelerate carbon and CaO that
Diffusion around here.Additionally, calcium fluoride is possible not only to provide calcium source, simultaneously F-As anion, its ionic radius and the ion of oxygen
Radius is more or less the same, and can enter CaO lattice, makes lattice activate, beneficially carbon and the diffusion inside of CaO, reduces producing electricity simultaneously
The activation energy of stone reaction, makes carbide to produce at a lower temperature.Thus, on the one hand pass through to add in raw materials for metallurgy to contain
Additive with calcium fluoride, it is achieved that smelt under cryogenic and produce carbide, on the other hand, by raw material is carried out at fine grinding
Reason, improves raw material specific surface area, increases the contact area of two kinds of raw materials, improves raw material mass transfer and heat transfer efficiency, improves reaction speed
Rate, reduces carbide reaction temperature and process energy consumption.Additionally, smelting reaction temperature is low, the requirement to equipment thermostability further
Reduce, thus reduce equipment investment cost.Meanwhile, raw material particle size is little, make raw material be obtained by the most completely, it is to avoid traditional work
Skill is less than the problem that the raw material of 5mm cannot be applied, reduces cost of material.
Wherein it is desired to explanation, the calcium fluoride of the embodiment of the present invention, can be i.e. pure calcium fluoride, it is also possible to contain
Other compound.
According to a particular embodiment of the invention, the mean diameter of bituminous coal granule is 70～120 μm；Putting down of calcic feed particles
All particle diameters are 10～30 μm；The mean diameter of described calcium fluoride particles is 30～50 μm.Inventor finds through numerous studies, when
The mean diameter of reaction raw materials is little, and raw material specific surface area is high, and the contact area of two kinds of raw materials is big, raw material mass transfer and heat transfer efficiency
Height, reaction rate is fast.Meanwhile, the mean diameter of bituminous coal granule is 70～120 μm, is easy to the discharge of volatile matter when pyrolysis, with
Time reduce carbon scaling loss.The mean diameter of calcic feed particles is 10～30 μm, is easy to the fast decoupled of limestone when pyrolysis
Become quick lime.Additionally, bituminous coal granule is different with the granule size of calcic feed particles, formed grade poor, beneficially molding with become
The raising of material strength after type.
According to embodiments of the invention, in mixed material, the ratio of each component is not particularly limited, as long as system can be reacted
Standby carbide.According to a preferred embodiment of the invention, bituminous coal, calcic raw material and calcium fluoride 100:(100 in mass ratio～
200): (3～15) carry out described mixing pressure ball and process.Thus, carbide is smelted the excellent catalytic effect of reaction by calcium fluoride, smelts temperature
Spending low, the time is short, and bituminous coal and calcic raw material fully react, it is to avoid the reactant waste that reactant excess causes, carbide
Quality better.
According to a particular embodiment of the invention, calcic raw material is limestone.Thus, the reactant activity of carbide reaction is high,
Promote the carrying out of carbide reaction, carbide quality better.
According to a particular embodiment of the invention, the calcium oxide content of calcic raw material is not less than 50 mass %.Thus, containing oxidation
The calcium oxide content of calcium raw material is high, and impurity is few, carbide quality better.
According to some embodiments of the present invention, the volatile matter content of bituminous coal is 25%～35%, content of ashes be 4%～
8%.Owing in bituminous coal, volatile matter content is high, and then the volatile matter being volatilized to enter in flue gas that is heated when pyrolysis is more so that
Imflammable gas content in flue gas is high, and therefore, flue gas can return to pyrolysis oven and uses as fuel, reduces making of other fuel
With, it is achieved the high-efficiency comprehensive utilization of resource, save the energy.
According to some embodiments of the present invention, the method farther includes: before fine grinding processes, to bituminous coal and calcic raw material
It is dried process, obtains dried bituminous coal and calcic raw material.Thus, reducing the water content of raw material, pyrolysis processing energy consumption is low.
S200 mixing pressure ball processes
According to embodiments of the invention, carry out bituminous coal granule, calcic feed particles and calcium fluoride particles mixing at pressure ball
Reason, obtains mixed material agglomerate.Thus, reaction raw materials is dispersed, and the particle diameter of mixed material agglomerate is suitable, it is simple to follow-up
Carry out metallurgy.
S300 pyrolysis processing
According to embodiments of the invention, mixed material agglomerate is carried out pyrolysis processing, pelletizing after being pyrolyzed and containing
The flue gas of volatile matter.Utilize this mixed material, it is only necessary to low temperature smelting can prepare the carbide of high-quality.In pyrolytic process,
Limestone is decomposed reaction (r-1), can react (r-2) with the C in coal simultaneously, produces CO and enters flue gas and cause the damage of carbon
Lose.In coal, volatile matter is heated when pyrolysis and is volatized in flue gas, therefore, there is a large amount of imflammable gas, can return in flue gas
Pyrolysis oven uses as fuel, reduces the use of other fuel.
CaCO3=CaO+CO2(r-1)
CO2+ C=2CO (r-2)
According to embodiments of the invention, the temperature of pyrolysis processing is 1000～1200 DEG C.Thus, limestone fully decomposes,
Be conducive to improving carbide productivity.
According to embodiments of the invention, the flue gas containing volatile matter is used as the fuel needed for pyrolysis processing.Use
High volatile, low-ash bituminous coal are raw material, and in coal, volatile matter is heated when pyrolysis and is volatized in flue gas, therefore, in flue gas
There is a large amount of imflammable gas, can return to pyrolysis oven and use as fuel, reduce the use of other fuel, save the energy, effectively
Achieve the comprehensive utilization of the energy.
S 400 calcination process
According to embodiments of the invention, the pelletizing after pyrolysis is carried out calcination process, it is thus achieved that solid-state carbide.Thus, pyrolysis
The calcium oxide obtained and the carbon in bituminous coal react generation solid-state carbide.
According to embodiments of the invention, the temperature of metallurgy is 1500～1800 DEG C, and the time is 30～90 minutes.By
This, the temperature of reaction is low, the time is short, and energy consumption cost is few.Meanwhile, the requirement to smelting equipment thermostability also reduce further,
Thus the cost of investment of smelting equipment is lower.
According to embodiments of the invention, metallurgy is carried out under an argon atmosphere so that smelts atmosphere in stove and keeps
For nonoxidizing atmosphere, reduce the scaling loss of cigarette carbon content in coal, simultaneously facilitate generation carbide.According to a preferred embodiment of the invention, smelt
Process is carried out under high-purity argon gas atmosphere.Thus, the scaling loss of cigarette carbon content in coal is less, the beneficially preparation of carbide.
According to embodiments of the invention, the pelletizing after pyrolysis, it is directly loadable into time hot in refractory material crucible, places into high temperature
In roaster.Thus, the hot pelletizing after pyrolysis directly carries out roasting, makes full use of the heat of pyrolysis.
Below with reference to specific embodiment, the present invention will be described, it should be noted that these embodiments are only explanation
Property, and be not considered as limiting the invention.
Embodiment 1
Be divided into 29% with volatilization, ash be 8% bituminous coal and limestone that CaO content is 50.77% for raw material preparation electricity
Stone, concrete grammar is as follows:
(1) coal, limestone and calcium fluoride are dried and levigate process respectively, respectively obtain coal fine powder, limestone thin
Powder and fine calcium fluoride powder, wherein, the Task-size Controlling of coal dust is in 70 μm～120 μm, and the Task-size Controlling of agstone is at 10 μm～30 μ
M, the Task-size Controlling of fine calcium fluoride powder is in 30 μm～50 μ m.
(2) take coal fine powder 100 parts, limestone fines 125 parts and fine calcium fluoride powder 8 parts, after batch mixing is uniform, be pressed into ellipsoid
Shape.
(3) pelletizing pressed is distributed in solution stove and is pyrolyzed at 1050 DEG C, is directly accessed in refractory material crucible after pyrolysis,
It is then placed in high-temperature roasting furnace, roasting 80min at 1600 DEG C, roasting process is passed through high-purity argon gas and carries out atmosphere protection,
Obtain solid-state carbide.Smelting is taken out carbide after terminating and is carried out gas forming amount mensuration, and result is 235L/kg.
Embodiment 2
Be divided into 32% with volatilization, ash be 6% bituminous coal and limestone that CaO content is 52.41% for raw material preparation electricity
Stone, concrete grammar is as follows:
(1) coal, limestone and calcium fluoride are dried and levigate process respectively, respectively obtain coal fine powder, limestone thin
Powder and fine calcium fluoride powder, wherein, the Task-size Controlling of coal dust is in 70 μm～120 μm, and the Task-size Controlling of agstone is at 10 μm～30 μ
M, the Task-size Controlling of fine calcium fluoride powder is in 30 μm～50 μ m.
(2) take coal fine powder 100 parts, limestone fines 180 parts and fine calcium fluoride powder 10 parts, after batch mixing is uniform, be pressed into ellipsoid
Shape.
(3) pelletizing pressed is distributed in solution stove and is pyrolyzed at 1100 DEG C, is directly accessed in refractory material crucible after pyrolysis,
It is then placed in high-temperature roasting furnace, roasting 60min at 1700 DEG C, roasting process is passed through high-purity argon gas and carries out atmosphere protection,
Obtain solid-state carbide.Smelting is taken out carbide after terminating and is carried out gas forming amount mensuration, and result is 267L/kg.
Embodiment 3
Be divided into 28% with volatilization, ash be 5% bituminous coal and limestone that CaO content is 52.41% for raw material preparation electricity
Stone, concrete grammar is as follows:
(1) coal, limestone and calcium fluoride are dried and levigate process respectively, respectively obtain coal fine powder, limestone thin
Powder and fine calcium fluoride powder, wherein, the Task-size Controlling of coal dust is in 70 μm～120 μm, and the Task-size Controlling of agstone is at 10 μm～30 μ
M, the Task-size Controlling of fine calcium fluoride powder is in 30 μm～50 μ m.
(2) take coal fine powder 100 parts, limestone fines 120 parts and fine calcium fluoride powder 15 parts, after batch mixing is uniform, be pressed into ellipsoid
Shape.
(3) pelletizing pressed is distributed in solution stove and is pyrolyzed at 1000 DEG C, is directly accessed in refractory material crucible after pyrolysis,
It is then placed in high-temperature roasting furnace, roasting 50min at 1800 DEG C, roasting process is passed through high-purity argon gas and carries out atmosphere protection,
Obtain solid-state carbide.Smelting is taken out carbide after terminating and is carried out gas forming amount mensuration, and result is 278L/kg.
In the description of this specification, reference term " embodiment ", " some embodiments ", " example ", " specifically show
Example " or the description of " some examples " etc. means to combine this embodiment or example describes specific features, structure, material or spy
Point is contained at least one embodiment or the example of the present invention.In this manual, to the schematic representation of above-mentioned term not
Necessarily refer to identical embodiment or example.And, the specific features of description, structure, material or feature can be any
One or more embodiments or example in combine in an appropriate manner.
Although an embodiment of the present invention has been shown and described, it will be understood by those skilled in the art that: not
These embodiments can be carried out multiple change in the case of departing from the principle of the present invention and objective, revise, replace and modification, this
The scope of invention is limited by claim and equivalent thereof.
Claims (9)
1. the method preparing solid-state carbide, it is characterised in that including:
Bituminous coal, calcic raw material and calcium fluoride are carried out fine grinding process, in order to obtain bituminous coal granule, calcic feed particles and calcium fluoride
Granule, wherein, described carbon raw material is high volatile, low ash bituminous coal；Described calcic raw material is limestone；
Described bituminous coal granule, described calcic feed particles and described calcium fluoride particles carry out mix pressure ball process, in order to obtain
Mixed material agglomerate；
Described mixed material agglomerate is carried out pyrolysis processing, in order to the pelletizing after being pyrolyzed and the flue gas containing volatile matter；With
And
Pelletizing after described pyrolysis is carried out calcination process, in order to obtain solid-state carbide.
Method the most according to claim 1, it is characterised in that the mean diameter of described bituminous coal granule is 70～120 μm；
The mean diameter of described calcic feed particles is 10～30 μm；
The mean diameter of described calcium fluoride particles is 30～50 μm.
Method the most according to claim 1, it is characterised in that described bituminous coal, described calcic raw material and described calcium fluoride
Grain 100:(100 in mass ratio～200): (3～15) carry out described mixing pressure ball and process.
Method the most according to claim 1, it is characterised in that the calcium oxide content of described calcic raw material is not less than 50 matter
Amount %.
Method the most according to claim 1, it is characterised in that the volatile matter content of described bituminous coal is 25%～35%, ash
Dividing content is 4%～8%.
Method the most according to claim 1, it is characterised in that the temperature of described pyrolysis processing is 1000～1200 DEG C.
Method the most according to claim 1, it is characterised in that the temperature of described calcination process is 1500 DEG C～1800 DEG C,
Time is 30～90 minutes.
Method the most according to claim 1, it is characterised in that described calcination process is carried out under an argon atmosphere.
Method the most according to claim 1, it is characterised in that utilize the described flue gas containing volatile matter as described pyrolysis
Fuel needed for process.
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Effective date of abandoning: 20190416 |
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