CN107857267B - A kind of method that vacuum low-pressure prepares calcium carbide - Google Patents
A kind of method that vacuum low-pressure prepares calcium carbide Download PDFInfo
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Abstract
The invention discloses a kind of methods that vacuum low-pressure prepares calcium carbide.This method are as follows: carbon-based raw material and calcium based raw material synthesize calcium carbide under lower pressure, and two sections of heatings, respectively middle low-temperature heat stage and pyroreaction stage are used in reaction process.The temperature in the middle low-temperature heat stage is 500~900 DEG C, and the time is 0.5~3h, and absolute pressure is 0.5~105Kpa.The temperature in the pyroreaction stage is 1550~1900 DEG C, and the time is 0.2~4h, absolute pressure 50-2000pa.The present invention produces calcium carbide using low pressure or vacuum condition, can reduce reaction temperature, shortens the reaction time, and the direction for promoting reaction to generate to calcium carbide carries out, and reduces energy consumption.Using the method for segmentally heating, energy consumption can be reduced, when using coal as carbon source, when calcium carbonate or calcium hydroxide are calcium source, while may make carbon source that can utmostly be converted into calcium carbide, also obtains gas (CO, H of high added value2、CH4) and tar, greatly reduction CO2Discharge, improves the whole effective rate of utilization of material.
Description
Technical field
The present invention relates to calcium carbide preparation technical fields, and in particular to a kind of method that vacuum low-pressure prepares calcium carbide.
Background technique
Calcium carbide is commonly called as calcium carbide, is a kind of important coal chemical industry intermediate product, production acetylene is reacted with water.Calcium carbide at present
Industrial production is all made of arc process, i.e., using the blocky calcium oxide of certain partial size and blocky coke at a high temperature of electric arc generates
(2000~2200 DEG C) reactions generate calcium carbide (CaC2), while the gases such as carbon monoxide, carbon dioxide are discharged.This calcium carbide is raw
Production process temperature is high, energy consumption is high, ingredient requirement is high, and dust pollution is serious.The shortcomings that " high investment, high energy consumption, high pollution ",
The requirement of coal chemical industry energy-saving and emission-reduction and sustainable development is not met, the development of calcium carbide industry is seriously limited.
In recent years, industrial calcium carbide production technology improves, the type of furnace of furnace of calcium carbide from original opening furnace, semi-hermetic furnace by
Gradually develop into sealed furnace, dust pollution and energy consumption problem all improve to some extent, but calcium carbide production temperature still 2000 DEG C with
On, the energy consumption of calcium carbide product per ton is in 3250KW/h or more.
Application No. is the Chinese patents of CN201611141009.X " system and method for preparing calcium carbide " to disclose a kind of surpass
The system and method for thin carbon-based calcium based raw material production calcium carbide, propose to use producing calcium carbide by using powder raw materials through, reduce calcium carbide and be produced into
This, improves calcium carbide production efficiency;It is " a kind of to utilize microwave energy low temperature preparation electricity that application No. is 201610020462.9 Chinese patents
The method of stone " discloses a kind of method using microwave synthesis calcium carbide, strengthens the Mass and heat transfer mistake between raw material using microwave heating
Journey reduces the generation temperature of calcium carbide.Some scholars propose to use the excessive source C and O2Reaction mass is heated in situ combustion heat release
Oxygen thermal method next life produce electricity stone.These new methods all provide to reduce calcium carbide production energy consumption and cost, improving calcium carbide production technology
New thinking.
Application No. is the 201620591766.6 Chinese utility model patent system of solid-state calcium carbide " preparation " disclose by
The calcium carbide preparation system that fine mill, mixing device, molding machine and vacuum furnace form, can anti-blocking sintering and improvement
In addition dynamic conditions.But since this patented technology only carries out vacuumizing in 1200 DEG C of non-stages of reaction below, and
The operation of totally-enclosed, a large amount of carbon monoxide that cannot will be generated in reaction process are carried out at (1700~1800 DEG C) of the stage of reaction
Reaction system is excluded in time, thus will cause carbon monoxide and accumulate in reactor and rise with pressure, according in patent Example
Calcium carbide gas forming amount reach 290L/kg and calculated, the CO that reaction process generates can will at least make the pressure of reaction system
1.2atm or so, completely positive pressure are risen to, is not had in reaction process and the sealed furnace in reaction principle with existing industry
The difference of essence is extremely difficult to improve the effect of reacting dynamics condition proposed in patent.
Summary of the invention
The purpose of the present invention is " high pollution of high temperature high energy consumption " problems for calcium carbide production, propose one kind in vacuum low-pressure
Under the conditions of prepare the new solution of calcium carbide.
The industrial production technology of calcium carbide and oxygen thermal method etc. are all that electricity is synthesized under conditions of normal pressure or micro-positive pressure at present
Stone.Calcium carbide generates the reaction equation of reaction are as follows: CaO+3C=CaC2+CO.From reaction equation as can be seen that this chemistry is anti-
The characteristics of answering is that 3 molecular carbons restore 1 molecular oxidation calcium generation, 1 molecule calcium carbide, 1 molecular carbon monoxide gas of by-product simultaneously.From anti-
It answers thermodynamic analysis to know, removes carbon monoxide in time, reduces carbon monoxide pressure of tension, can promote to react to generation calcium carbide
Direction carries out.Therefore, the present invention provides a kind of vacuum to prepare calcium carbide new method, reduces energy consumption and production costs, and increases economical
Benefit, this method can be not only used for the furnace of calcium carbide of electric arc heated, can be used for the furnace of calcium carbide of microwave heating.
Present invention technical solution used for the above purpose is as follows:
The method that vacuum low-pressure of the present invention prepares calcium carbide is as follows:
1) pretreatment of raw material: mainly the calcium based raw materials such as the carbon-based raw material such as coal, coke and calcite, lime stone or lime are pressed
Broken fine is carried out after certain ratio uniform mixing, obtains the first uniformly mixed mixture;Tar, binder are mixed
Uniformly obtain the second mixture;
2) compression moulding after being mixed the first mixture according to 100:0-5% with the second mixture obtains molding
Reactant feed;Alternatively, the block carbon based raw material of certain partial size and blocky calcium based raw material are directly mixed according to a certain percentage
Obtain reactant feed;
3) forvacuum: ready reactant feed being added in the closed calcium carbide reactor with vacuum system,
Start vacuum pump, the air etc. in extraction device and material.After the absolute pressure in reactor is lower than 500Pa, it is believed that
Air in reactor excludes completely substantially;
4) the low-temperature heat stage in: the heating period is divided into two stages of two middle low-temperature heats and pyroreaction.First rank
Duan Weizhong low-temperature heat, heating temperature are 500~900 DEG C, 0.5~3h of constant temperature.This stage can release gas, exchanged heat, separated
After purification, the product (such as tar, synthesis gas, methane) of high added value can be obtained, at this time the pressure in reactor be 0.5~
105KPa, i.e. this stage can heat for negative pressure, or micro-positive pressure heating;
5) the pyroreaction stage: after the middle low-temperature heat stage, increasing temperature to 1550~1900 DEG C makes material reaction
Generate calcium carbide calcium carbide.Absolute pressure in this stage control reactor is 50-2000Pa, and in this reaction temperature and reaction pressure
0.2~4h of reaction is maintained under the conditions of power, so that material reaction is complete.The CO gas generated in reaction process through heat exchange,
It can be used in subsequent reactions process after isolating and purifying;
6) calcium carbide discharges: after reaction, stopping heating and vacuumizes, when reaction temperature is lower than 450 DEG C, opens reaction
Device takes out solid product calcium carbide.
Preferably, the carbon-based material in the present invention is anthracite, lignite, jet coal, one of semicoke or coke or one
Kind or more.Calcium-based materials are calcite, lime stone, calcium hydroxide, lime (calcium oxide) etc..
Preferably, the molar ratio of the carbon in step 1) and calcium oxide is 3.5~2.0:1, preferably 3.0~2.2:1;Carbon with
The molar ratio of calcium carbonate is 4.2~2.7:1, preferably 3.6~2.6:1.
Preferably, the molding raw mixture in step 2) its it is ultra-fine after granularity be 10~300 μm, preferably 30~
150μm;Not ultra-fine its partial size of block stock directly reacted that forms is 0.1~10cm, preferably 0.5~2.5cm.
Preferably, the calcium carbide reactor (furnace of calcium carbide) in step 3) is closed reactor, is circumscribed with vacuum system, vacuum
Degree can regulate and control.
Preferably, the calcium carbide reactor (furnace of calcium carbide) in step 3) is in electric arc furnaces, resistance furnace, graphite furnace or micro-wave oven
One kind;Heating method can be electric heating, electric arc heated, induction heating and microwave heating.
Preferably, the calcium carbide reactor in step 3) is batch reactor, and reactor is built-in with crucible, and material is placed in earthenware
It is reacted in crucible.
Preferably, the calcium carbide reactor in step 3) is more reactor combinations;The high temperature of reactor by-product when combination
Gas can be used as the supplemental heat source of other reactors first stage heating.
Preferably, the middle low-temperature heat phase temperature in step 4) is 500~900 DEG C, and pressure is 0.5~105KPa.It is excellent
Choosing, when calcium based raw material is lime stone, calcite, heating temperature is 700~850 DEG C;When calcium based raw material be quick lime or
When white lime, heating temperature is 500~750 DEG C;The gas that this stage generates can preheat reaction mass, then separate
Purification, obtains the CO or synthesis gas of high-purity, can be directly used for next section of reaction process.
Preferably, in step 4), when the carbon-based raw material of reactant is coal, first stage heating temperature is 600~900
DEG C, the gas that this stage generates is gas mixture, through with the heat exchange of other reactors it is cooling after tar and pyrolysis gas can be obtained, heat
It vents one's spleen after isolating and purifying, obtains the synthesis gas and methane of high added value.
Preferably, it in step 4), when reactant feed is coke and calcium oxide, can directly be warming up to needed for pyroreaction
Temperature.
Preferably, in step 5), the temperature of pyroreaction is 1550~1900 DEG C, and reaction absolute pressure is 50-2000Pa,
Preferred temperature is 1600~1800 DEG C, and preferred absolute pressure is 500-1000Pa.
Preferably, in step 5), the high-temperature gas of pyroreaction stage by-product can be used as the supplemental heat source of first stage.
Compared with prior art, beneficial effects of the present invention are as follows:
1, the thermodynamics feature of reaction is generated according to calcium carbide, calcium carbide generates the critical reaction temperature of reaction with carbon monoxide point
Pressure drop is low and reduces.It, can be with when carrying out calcium carbide production, especially absolute pressure using low pressure or vacuum condition and being lower than 2000Pa
Reaction temperature is reduced, the reaction time is shortened, the direction for promoting reaction to generate to calcium carbide carries out, and significantly improves the production for generating calcium carbide
Rate reduces energy consumption.
2, using the method for segmentally heating, energy consumption can be reduced, when using coal as carbon source, calcium carbonate or calcium hydroxide are calcium source
When, while may make carbon source that can utmostly be converted into calcium carbide, also obtain gas (CO, H of high added value2、CH4) and it is burnt
Oil, greatly reduction CO2Discharge, improves the whole effective rate of utilization of material.In this approach, the change under two sections of heating temperatures
Reaction is learned to be respectively as follows:
First segment: CaCO3+ C=CaO+2CO or Ca (OH)2+ C=CaO+CO+H2Second stage: CaO+3C=CaC2+
CO
But first lime stone etc. is fired into after calcium oxide in limekiln in traditional calcium carbide production technology and carries out broken sieve
It is used as reaction raw materials after point, generates a large amount of carbon dioxide at this time and increases carbon emission, and calcium oxide cools to preservation temperature from high temperature
Degree, wastes a large amount of latent heat.Its reaction equation is CaCO3=CaO+CO2。
3, this method raw material and type of furnace strong applicability.This method can be tried out in electric arc furnaces, resistance furnace, can be used for microwave
Calcium carbide is produced in furnace.Meanwhile the fitness of raw material is high, can use with calcium carbonate calcite as main component and lime stone,
It can also be using quick lime, white lime etc.;Carbon source can use block-like coke, can also use coke breeze fine coal.In short, this work
Skill production calcium carbide process is short, CO2 emission is few, reaction temperature is low, energy conservation and environmental protection.
Specific embodiment
Illustrate technical solution of the present invention below by way of specific embodiment.The equal city of raw materials and reagents used in the present invention
Selling can obtain.
Embodiment 1
It according to molar ratio is C:Ca=by metallurgical coke (being shown in Table one) and lime stone (calcium carbonate mass content is greater than 98.0%)
Extra-fine grinding is carried out after 3.7:1 mixing, obtains the ultra-fine mixed material that less than 80 μm particles of granularity account for 90% or more.To roll-in
Ultra-fine mixture diameter is pressed on piece machine to be 0.5~1cm, be highly the cylindrical particle of 0.2~1cm.By above-mentioned compacting
Good material is placed in boron nitride crucible and is reacted in the vacuum microwave reactor that microwave frequency is 0.915GHz.Instead
Answer air in device forvacuum discharge reactor and material.Microwave power supply is opened after system absolute pressure is lower than 1000Pa,
Adjusting microwave power makes material be warming up to 900 DEG C, simultaneously regulating system pressure to 0.9atm and with this condition maintenance temperature pressure
Power 0.5h.Gas (CO about 75%, CH that this stage generates4About 3%, CO2The CO gas about 22%) isolated and purified after exchanging heat
Body is sent into carbon monoxide basin.After the completion of middle low-temperature zone heating, low-voltage high-temperature heating reaction is carried out to material.Heating temperature is
1720 DEG C, system absolute pressure maintains 1000Pa or so, and insulation reaction 90min, and (CO is about for the gas generated in reaction process
For 96%, CO2It is 4% or so) purifies and separates after heat exchange is cooling, it is sent into carbon monoxide basin.Reaction terminates to cool to 400 DEG C
After take out material.It is got angry detection, gas forming amount reaches 306L/Kg.
One smelter coke ingredient of table
Project | Mc | Aw | Va | Wv |
Content | 87.34 | 0.27 | 7.79 | 4.60 |
Comparative example 1-1
It according to molar ratio is C:Ca=by metallurgical coke (being shown in Table one) and lime stone (calcium carbonate mass content is greater than 98.0%)
Extra-fine grinding is carried out after 3.7:1 mixing, obtains the ultra-fine mixed material that less than 80 μm particles of granularity account for 90% or more.To roll-in
Ultra-fine mixture diameter is pressed on piece machine to be 0.5~1cm, be highly the cylindrical particle of 0.2~1cm.By above-mentioned compacting
Good material is placed in boron nitride crucible and is reacted in the vacuum microwave reactor that microwave frequency is 0.915GHz.Instead
Answer air in device forvacuum discharge reactor and material.Microwave power supply is opened after system absolute pressure is lower than 1000Pa,
Adjusting microwave power makes material be warming up to 900 DEG C, simultaneously regulating system pressure to 0.9atm and with this condition maintenance temperature pressure
Power 0.5h.Gas (CO about 75%, CH generated in this phase process4About 3%, CO2It about 22%) isolates and purifies, obtains after exchanging heat
The CO gas arrived is sent into carbon monoxide basin.After the completion of middle low-temperature zone heating, constant-pressure and high-temperature heating reaction is carried out to material.It is passed through
Argon gas stops being passed through argon gas and opens microwave power supply after so that system pressure is reached 1.1atm, and adjusting microwave power is warming up to material
1720 DEG C, and the insulation reaction 120min in the case where system pressure maintains positive pressure 1.1atm.(CO is about for the gas generated in reaction process
For 98%, CO2Etc. other components be purifies and separates after heat transfer of mixture gas 2%) is cooling, obtain pure carbon monoxide gas, send
Enter carbon monoxide basin.Material is taken out after cooling to 400 DEG C after reaction.It is got angry detection, gas forming amount reaches 143L/Kg.
Comparative example 1-2
It according to molar ratio is C:Ca=by metallurgical coke (being shown in Table one) and lime stone (calcium carbonate mass content is greater than 98.0%)
Extra-fine grinding is carried out after 3.7:1 mixing, obtains the ultra-fine mixed material that less than 80 μm particles of granularity account for 90% or more.To roll-in
Ultra-fine mixture diameter is pressed on piece machine to be 0.5~1cm, be highly the cylindrical particle of 0.2~1cm.By above-mentioned compacting
Good material is placed in boron nitride crucible and is reacted in the vacuum microwave reactor that microwave frequency is 0.915GHz.Instead
Answer air in device forvacuum discharge reactor and material.Microwave power supply is opened after system absolute pressure is lower than 1000Pa,
Adjusting microwave power makes material be warming up to 1720 DEG C, and system absolute pressure maintains 1000Pa or so, and insulation reaction 120min,
The gas generated in reaction process purifies and separates after heat exchange is cooling, obtained mixed gas composition are as follows: CO content about 70% is left
The right side, CO2Content is about 30%).Material is taken out after cooling to 400 DEG C after reaction.It is got angry detection, gas forming amount reaches 297L/
Kg。
Embodiment 2
Using the coke (being shown in Table one) and white lime (Ca (OH) in embodiment one2Content is greater than
The ultra-fine mixed material that less than 80 μm particles of granularity account for 90% or more is obtained after C:Ca=4:1 mixing and fine.To roll-in
Above-mentioned ultra-fine mixture is pressed into diameter 5mm on piece machine, is highly the cylindrical particle of 10mm.By above-mentioned molding particulate matter
Material is placed in the electrothermal furnace of Si-Mo rod heating, opens the air in vacuum pump extraction system.It opens and adds after pressure is lower than 500Pa
Hot button is heated, and 40min is kept the temperature when temperature is increased to 550 DEG C, while maintenance system pressure is normal pressure, this reaction process
Gas (the H of middle generation2Molar content is about 46%, CO 52%, CO2And other components are 2%) to isolate and purify after exchanging heat,
Synthesis gas (the H of obtained high-purity2And CO) be sent into synthesis gas basin or enter next section of reaction process.Middle low-temperature zone heating knot
Shu Hou, regulation system absolute pressure is 800Pa or so, while continuing heated material to 1650 DEG C and maintaining 90min, reaction system
Absolute pressure maintains 800Pa or so, and the gas (CO content is about 98% or more) generated in this reaction process divides after exchanging heat
Carbon monoxide basin is sent into from the high-purity CO gas after purification, obtained or enters next section of synthesis procedure.End cools to 400
Material is taken out after DEG C.It is got angry detection, gas forming amount reaches 264L/Kg.
Comparative example 2
Using the coke (being shown in Table one) and white lime (Ca (OH) in embodiment one2Content is greater than
The ultra-fine mixed material that less than 80 μm particles of granularity account for 90% or more is obtained after C:Ca=4:1 mixing and fine.To roll-in
Above-mentioned ultra-fine mixture is pressed into diameter 5mm on piece machine, is highly the cylindrical particle of 10mm.By above-mentioned molding particulate matter
Material is placed in the electrothermal furnace of Si-Mo rod heating, opens the air in vacuum pump extraction system.It opens and adds after pressure is lower than 500Pa
Hot button carries out heated material and to 1650 DEG C and maintains 130min, and reaction system absolute pressure maintains 8000Pa or so, this is anti-
After the gas (CO content is about 98% or more) that should be generated in the process isolates and purifies after exchanging heat, obtained high-purity CO gas is sent
Enter carbon monoxide basin or enters next section of synthesis procedure.End takes out material after cooling to 400 DEG C.It is got angry detection, hair
Tolerance reaches 88L/Kg.
Embodiment 3
Using in table two lignite and quick lime (calcium oxide content > 98.0%) reacted.It is according to carbon calcium molar ratio
Material is mixed and is obtained after fine the ultra-fine mixed material that less than 40 μm particles of granularity account for 90% or more by the ratio of 2.9:1.
With the method in embodiment one to mixing superfine-material tabletting.Above-mentioned material is taken to be placed in the electrothermal furnace of Si-Mo rod heating,
Open the air in vacuum pump extraction system.It opens heat button after pressure is lower than 500Pa to be heated, when temperature is increased to
40min is kept the temperature at 550 DEG C, while maintenance system pressure is normal pressure, the gas generated in this reaction process obtains after heat exchange separation
To tar and gaseous product (gas composition: H2+ CO is 44.7%, CH4For 32.3%, CO2For 20.8%, it is other 2.2%), gas
Body product obtains the synthesis gas and methane of high-purity after separation, can respectively enter next section of reaction process.Middle low-temperature zone heating
After, regulation system absolute pressure is 800Pa or so, while continuing heated material to 1650 DEG C and maintaining 90min, this reaction
After the gas generated in the process isolates and purifies after exchanging heat, under obtained high-purity CO gas is sent into carbon monoxide basin or is entered
One section of synthesis procedure.Reaction terminates to take out material after cooling to 400 DEG C.It is got angry detection, gas forming amount reaches 263L/Kg.
Two lignite ingredient of table
Project | Mad | Aad | Vdaf | FCdaf | Elemental analysis Cad |
Content | 24.79 | 7.88 | 45.50 | 54.50 | 71.33 |
Embodiment 4
By partial size after preliminary grinding be 0.5~5mm coke (ingredient is shown in Table three) and lime (calcium oxide mass content is greater than
99%) be to carry out extra-fine grinding after C:Ca=2.4:1 mixing according to molar ratio, obtain particle of the granularity less than 25 μm account for 90% with
On ultra-fine mixed material, depressing to diameter in the hydraulic press that pressure is 50MPa is 5cm, with a thickness of the disk of 1cm.It will be above-mentioned
Mixed raw material is placed in the microwave reactor that microwave frequency is 0.915GHz, is opened vacuum pump and is pumped the air in system.When
After system absolute pressure is lower than 1000Pa, adjusting microwave power makes reaction temperature rise to 1750 DEG C simultaneously from room temperature in 30min
1750 DEG C of reaction 120min are kept, and keeping absolute pressure in reactor is 1500Pa or so.Reaction terminates after cooling to 400 DEG C
Take out material.Surface of material is white, and internal structure densification has sintering, calcium carbide product as obtained.Product is got angry detection,
Its gas forming amount reaches 325L/Kg.
Comparative example 4-1
By partial size after preliminary grinding be 0.5~5mm coke (ingredient is shown in Table three) and lime (calcium oxide mass content is greater than
99%) be to carry out extra-fine grinding after C:Ca=2.4:1 mixing according to molar ratio, obtain particle of the granularity less than 25 μm account for 90% with
On ultra-fine mixed material, depressing to diameter in the hydraulic press that pressure is 50MPa is 5cm, with a thickness of the disk of 1cm.It will be above-mentioned
Mixed raw material is placed in the microwave reactor that microwave frequency is 0.915GHz, is opened vacuum pump and is pumped the air in system.When
After system absolute pressure is lower than 1000Pa, adjusting microwave power makes reaction temperature rise to 1750 DEG C simultaneously from room temperature in 30min
1750 DEG C of reaction 120min are kept, and keeping absolute pressure in reactor is 2000Pa or so.Reaction terminates after cooling to 400 DEG C
Take out material.Surface of material is white, and internal structure densification has sintering, calcium carbide product as obtained.Product is got angry detection,
Its gas forming amount reaches 305L/Kg.
Comparative example 4-2
By partial size after preliminary grinding be 0.5~5mm coke (ingredient is shown in Table three) and lime (calcium oxide mass content is greater than
99%) be to carry out extra-fine grinding after C:Ca=2.4:1 mixing according to molar ratio, obtain particle of the granularity less than 25 μm account for 90% with
On ultra-fine mixed material, depressing to diameter in the hydraulic press that pressure is 50MPa is 5cm, with a thickness of the disk of 1cm.It will be above-mentioned
Mixed raw material is placed in the microwave reactor that microwave frequency is 0.915GHz, is opened vacuum pump and is pumped the air in system.When
After system absolute pressure is lower than 1000Pa, adjusting microwave power makes reaction temperature rise to 1750 DEG C simultaneously from room temperature in 30min
1750 DEG C of reaction 120min are kept, and keeping absolute pressure in reactor is 3500Pa or so.Reaction terminates after cooling to 400 DEG C
Take out material.Surface of material is white, and internal structure densification has sintering, calcium carbide product as obtained.Product is got angry detection,
Its gas forming amount reaches 236L/Kg.
It above are only part preferred embodiment of the invention, the present invention is not limited in the content of embodiment.For ability
For technical staff in domain, can there are various change and change in the conception range of technical solution of the present invention, made
What changes and change, within that scope of the present invention.
Claims (2)
1. a kind of method that vacuum low-pressure prepares calcium carbide, it is characterised in that specific step is as follows for the method:
1) pretreatment of raw material: according to a certain percentage by carbon-based feed coal or coke and calcium based raw material calcite, lime stone or lime
Broken fine is carried out after evenly mixing, obtains the first uniformly mixed mixture;Tar, binder are uniformly mixed and obtain the
Two mixtures;
2) compression moulding after being mixed the first mixture according to 100:0-5% with the second mixture obtains molding reaction
Raw material;Alternatively, by the block carbon based raw material of certain partial size and blocky calcium based raw material, directly mixing is obtained according to a certain percentage
Reactant feed;
3) forvacuum: ready reactant feed being added in the closed calcium carbide reactor with vacuum system, starting
Vacuum pump, the air in extraction device and material make the absolute pressure in reactor lower than 500Pa;
4) the low-temperature heat stage in: heating temperature is 500~900 DEG C, 0.5~3h of constant temperature, the pressure in reactor is 0.5~
105KPa;This stage can release gas, and after being exchanged heat, being isolated and purified, the product of high added value can be obtained;
5) the pyroreaction stage: after the middle low-temperature heat stage, increasing temperature generates material reaction to 1550~1900 DEG C
Calcium carbide calcium carbide;Absolute pressure in this stage control reactor is 50-2000Pa, and in this reaction temperature and reaction pressure item
0.2~4h of reaction is maintained under part, so that material reaction is complete;
6) calcium carbide discharges: after reaction, stop heating and vacuumize, when reaction temperature is lower than 450 DEG C, opens reactor,
Take out solid product calcium carbide.
2. a kind of method that vacuum low-pressure prepares calcium carbide as described in claim 1, it is characterised in that: the carbon-based raw material and calcium
The C:Ca molar ratio of based raw material is (2.4~4): 1.
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