CN105439147A - Method of utilizing microwave energy to prepare calcium carbide at low temperature - Google Patents
Method of utilizing microwave energy to prepare calcium carbide at low temperature Download PDFInfo
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- CN105439147A CN105439147A CN201610020462.9A CN201610020462A CN105439147A CN 105439147 A CN105439147 A CN 105439147A CN 201610020462 A CN201610020462 A CN 201610020462A CN 105439147 A CN105439147 A CN 105439147A
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Abstract
The invention discloses a method of utilizing microwave energy to prepare calcium carbide at low temperature. The method comprises the following steps of using coal as a carbon source, using limestone or lime as a calcium source, heating by the microwave energy, and reacting and synthesizing to form the calcium carbide, wherein the reaction temperature of the synthesized calcium carbide is 1300-2000 DEG C, the reaction pressure is 0.3-1.1atm, and the reaction time is 3-120min; primarily grinding the carbon source and the calcium source, mixing according to a ratio, and performing ultrafine treatment to obtain an ultrafine mixed material; heating to react and synthesizing to form the calcium carbide by utilizing the microwave energy. The method has the advantages that the coal and the limestone are directly used as the raw materials, are subjected to ultrafine crushing, and are heated and synthesized to form the calcium carbide by the microwave energy; by utilizing various coal types, two steps of the coking of raw coal and the high-temperature decomposing of the calcium carbonate to prepare the limestone are not needed, the synthesizing temperature of the calcium carbide is lowered, the production efficiency and mechanical degree of the calcium carbide are improved, and a byproduct of carbon monoxide can be used as a chemical raw material to produce other chemical products.
Description
Technical field
The present invention relates to calcium carbide preparing technical field, be specifically related to a kind of method utilizing micro-wave energy low-temperature growth calcium carbide.
Background technology
Carbide of calcium, is commonly called as calcium carbide, is obtained through pyroreaction by coke (C) and lime (CaO), is a kind of important Coal Chemical Industry intermediate product, is the key compound of being produced clean chemical product except methyl alcohol by coal.Current industrial calcium carbide production technology was invented in 1892, (more than 2000 DEG C) reaction generation molten state carbide of calcium (CaC under the high temperature that to be calcium oxide and coke produces at electric arc
2).Although electric heating process is with a long history, but still there is the shortcoming of high energy consumption, high pollution.Calcium carbide building-up reactions is a solid phase thermo-negative reaction, and raw material mass transfer, heat transfer efficiency are low, and the chemical dynamics process time is long, thus needs heat and highly active coke as raw material.The heating condition of 2000 ~ 2200 DEG C needs a large amount of energy, and the energy consumption of calcium carbide product per ton is 3250 ~ 3600KW/h, requires high, add cost of investment and energy consumption to the resistance toheat of equipment.Coke is generally obtained by the coking of coal, and this process flow is long, and organic carbon loss is high, power consumption is high, environmental pollution is serious.Because traditional calcium carbide production technology exists the shortcoming of " high investment, high energy consumption, high pollution ", do not meet the requirement of energy-saving and emission-reduction and Sustainable development, seriously limit the development of calcium carbide industry.
Micro-wave energy is a kind of clean energy, and microwave heating is the dielectric properties conversion microwave energy relying on material self, produces heat.A large amount of research work has been carried out both at home and abroad in microwave calcination, and by this Technology in modern nonferrous metallurgy and field of new material preparation widespread use.Microwave heating is as a kind of heating means of green high-efficient, and compared with the heating means of routine, microwave heating has selectivity heating, temperature rise rate is fast, the reaction times is short, be easy to automatic control, can reduce the advantages such as chemical reaction temperature.
Summary of the invention
The object of the invention is to, a kind of method utilizing micro-wave energy low-temperature growth calcium carbide is provided, solve the technical problem that calcium carbide production technology traditional in prior art exists " high investment, high energy consumption, high pollution ".
The technical scheme that the present invention is adopted for achieving the above object is as follows:
Utilize a method for micro-wave energy low-temperature growth calcium carbide, the method is: take coal as carbon source, Wingdale or lime be calcium source, under Microwave Heating, and Reactive Synthesis calcium carbide.The main component of described Wingdale is calcium carbonate, and the main component of lime is calcium oxide.
Preferably, the temperature of reaction of described synthesis calcium carbide is 1300 ~ 2000 DEG C, and reaction pressure is 0.3 ~ 1.1atm, and the reaction times is 3 ~ 120min.
Further preferably, the temperature of reaction of described synthesis calcium carbide is 1550 ~ 1750 DEG C, and reaction pressure is 0.7 ~ 1.0atm, and the reaction times is 20 ~ 40min.
Preferably, described coal is selected from hard coal, brown coal, long-flame coal, one or more in semicoke, coking coal.
Preferably, when described calcium source is lime, the mol ratio of carbon and calcium oxide is 4.5 ~ 3.5:1.More preferably 4.1 ~ 3.8:1.
Preferably, when described calcium source is Wingdale, the mol ratio of carbon and calcium carbonate is 3.5 ~ 2.7:1.More preferably 3.1 ~ 2.8:1.
Preferably, be mixed in proportion after described carbon source and the preliminary grinding of calcium source, then carry out the mixture that super-refinement obtains super-refinement, recycling Microwave Heating Reactive Synthesis calcium carbide.The particle diameter of described preliminary grinding is 0.1 ~ 10mm, and the particle diameter of super-refinement is 5 μm ~ 0.1mm, more preferably 10 ~ 50 μm.
Preferably, the mixture of described super-refinement is a granulated into particle rear feeding Reactive Synthesis calcium carbide, or the mixture of super-refinement direct charging Reactive Synthesis calcium carbide.
Preferably, utilize microwave radiation device to provide micro-wave energy, microwave radiation frequencies is the one or more frequencies within the scope of 0.915GHz ~ 140GHz.
Preferably, can adopt boosting mode additional heat as required in calcium carbide building-up process, described boosting mode is selected from the waste heat of electrically heated, microwave heating, excess carbon combustion heating, emission.
Compared with prior art, beneficial effect of the present invention is as follows:
1, adopt Wingdale (calcium carbonate) to be calcium source, eliminate lime high temperature calcining unslaked lime operation processed; Adopt coal to substitute lump coke, low scala media fine coal can be utilized, and save coking link, reduce costs, enhance productivity.
2, adopt microwave heating to substitute electrically heated, utilize microwave to the katalysis of calcium carbide formation reaction, reduce the temperature of reaction generating calcium carbide.
3, by product is the carbon monoxide of a large amount of high density, can be used as industrial chemicals and generates other chemical.This explained hereafter calcium carbide operation is short, Carbon emission is few, temperature of reaction is low, energy-conserving and environment-protective.
Embodiment
Below by way of specific embodiment, technical scheme of the present invention is described.Raw material used in the present invention and reagent are all commercially.
The technical process that the present invention prepares calcium carbide is:
Adopt fine coal as carbon source, Wingdale or lime are as calcium source, and superfine grinding is carried out after mixing by a certain percentage in carbon source and calcium source after corase grind; The ultra-fine mixture obtained directly can enter Reaktionsofen and carry out calcium carbide reaction, enters Reaktionsofen again and carry out calcium carbide reaction after also caning be passed through granulation, and reaction generates calcium carbide and CO gas.
The microwave reactor adopted in following embodiment 1-7 is High-Power Microwave reactor prepared by this laboratory designed, designed, and microwave frequency is 2.45GHz, and microwave power is at 0 ~ 4KW continuously adjustabe, and the gas produced in reaction process is extracted out by vapor pipe.In embodiment 8, the microwave frequency of microwave reactor is 0.915GHz, and other conditions are consistent with precedent.
Embodiment 1
Be the Fujian Anthracite (hard coal composition is in table 1) of 0.5 ~ 5mm and Wingdale (calcium carbonate mass content is greater than 98%) by particle diameter after preliminary grinding according to mol ratio be carry out extra-fine grinding after C:Ca=4:1 mixing, obtain granularity and be less than the ultra-fine mixture that 40 μm of particles account for more than 90%.Depress at the pressure hydropress that is 50MPa that diameter is 5cm, thickness is the disk of 1cm.The weight of every sheet is about 20g.Above-mentioned 3 mixing raw materials are positioned in the crucible of microwave reactor, regulate microwave power to make temperature of reaction in 45mins, rise to 1700 DEG C from room temperature and keep 1700 DEG C to react 30min.Material is taken out after reaction end cools to 400 DEG C.Material surface is grey black, and whole contraction is lumpd, and is obtained calcium carbide product.Product is through detection of getting angry, and its gas forming amount reaches 300L/Kg.
Table 1 Fujian Anthracite composition
Embodiment 2
Mol ratio in employing embodiment 1 is the ultra-fine mixture direct reaction of C:Ca=4:1.Taking above-mentioned powder 60.0g is placed in the crucible of microwave reactor, regulates microwave power to make temperature of reaction in 45mins, rise to 1700 DEG C from room temperature and keep 1700 DEG C to react 30min.Material is taken out after reaction end cools to 400 DEG C.Material surface is canescence, and inside is grey black, loose without sintering, is obtained calcium carbide product.Product is through detection of getting angry, and its gas forming amount reaches 277L/Kg.
Embodiment 3
Mol ratio in employing embodiment 1 is the mixed powder direct reaction of C:Ca=4:1.Taking above-mentioned powder 60.0g is placed in the crucible of microwave reactor, regulates microwave power to make temperature of reaction in 30mins, rise to 1400 DEG C from room temperature and keep 1400 DEG C to react 20min.Material is taken out after reaction end cools to 400 DEG C.Material surface is grey black, and inside is black, loose without sintering, is obtained calcium carbide product.Product is through detection of getting angry, and its gas forming amount reaches 129L/Kg.
Embodiment 4
Adopt the Fujian Anthracite in embodiment 1 and Wingdale.Be that mixing of materials is obtained granularity and is less than the ultra-fine mixture that 40 μm of particles account for more than 90% by the ratio of 3.8:1 after super-refinement according to carbon calcium mol ratio.With the method in embodiment 1 to mixing superfine-material compressing tablet.Getting above-mentioned sheet stock 3 is placed in the crucible of microwave reactor, regulates microwave power to make temperature of reaction in 30mins, rise to 1650 DEG C from room temperature and keep 1650 DEG C to react 10min.Material is taken out after reaction end cools to 400 DEG C.Material surface is canescence, and have contraction, internal structure is compacted sintering, is obtained calcium carbide product.Product is through detection of getting angry, and its gas forming amount reaches 265L/Kg.
Embodiment 5
Be the long-flame coal (composition is in table 2) of 0.5 ~ 5mm and Wingdale (calcium carbonate mass content is greater than 98%) by particle diameter after preliminary grinding according to mol ratio be carry out extra-fine grinding after C:Ca=4:1 mixing, obtain the ultra-fine mixture that particle that granularity is less than 25 μm accounts for more than 90%, depress at the pressure hydropress that is 50MPa that diameter is 5cm, thickness is the disk of 1cm.The weight of every sheet is about 20g.Above-mentioned 3 mixing raw materials are positioned in the crucible of microwave reactor, regulate microwave power to make temperature of reaction in 25mins, rise to 1670 DEG C from room temperature and keep 1670 DEG C to react 25min.Material is taken out after reaction end cools to 400 DEG C.Material surface is canescence, and internal structure is compacted sintering, is obtained calcium carbide product.Product is through detection of getting angry, and its gas forming amount reaches 301L/Kg.
Table 2 long-flame coal composition
| Project | M ad | A ad | V ad | FC ad | Ultimate analysis C ad |
| Content | 3.63 | 4.39 | 44.60 | 47.38 | 73.77 |
Embodiment 6
Be the brown coal (composition is in table 3) of 0.5 ~ 5mm and Wingdale (calcium carbonate mass content is greater than 97%) by particle diameter after preliminary grinding according to mol ratio be carry out extra-fine grinding after C:Ca=4.1:1 mixing, obtain the ultra-fine mixture that particle that granularity is less than 48 μm accounts for more than 90%, depress at the pressure hydropress that is 50MPa that diameter is 5cm, thickness is the disk of 1cm.The weight of every sheet is about 20g.Above-mentioned 3 mixing raw materials are positioned in microwave reactor, regulate microwave power to make temperature of reaction in 30mins, rise to 1680 DEG C from room temperature and keep 1680 DEG C to react 30min.Material is taken out after reaction end cools to 400 DEG C.Material surface is canescence, and internal structure densification has sintering, is obtained calcium carbide product.Product is through detection of getting angry, and its gas forming amount reaches 278L/Kg.
Table 3 brown coal composition
| Project | M ad | A ad | V daf | FC daf | Ultimate analysis C ad |
| Content | 24.79 | 7.88 | 45.50 | 54.50 | 71.33 |
Example 7
Be the semicoke (composition is in table 4) of 0.5 ~ 5mm and Wingdale (calcium carbonate mass content is greater than 97%) by particle diameter after preliminary grinding according to mol ratio be carry out extra-fine grinding after C:Ca=4.1:1 mixing, obtain the ultra-fine mixture that particle that granularity is less than 58 μm accounts for more than 90%, depress at the pressure hydropress that is 50MPa that diameter is 5cm, thickness is the disk of 1cm.The weight of every sheet is about 20g.Above-mentioned 3 mixing raw materials are positioned in microwave reactor, regulate microwave power to make temperature of reaction in 30mins, rise to 1650 DEG C from room temperature and keep 1650 DEG C to react 30min.Material is taken out after reaction end cools to 400 DEG C.Material surface is canescence, and internal structure densification has sintering, is obtained calcium carbide product.Product is through detection of getting angry, and its gas forming amount reaches 246L/Kg.
Table 4 semicoke composition
| Project | M c | A w | V a | W v |
| Content | 69.27 | 0.36 | 20.51 | 9.86 |
Example 8
Be the coke (composition is in table 5) of 0.5 ~ 5mm and lime (calcium oxide mass content is greater than 99%) by particle diameter after preliminary grinding according to mol ratio be carry out extra-fine grinding after C:Ca=3:1 mixing, obtain the ultra-fine mixture that particle that granularity is less than 25 μm accounts for more than 90%, depress at the pressure hydropress that is 50MPa that diameter is 5cm, thickness is the disk of 1cm.The weight of every sheet is about 20g.It is in the microwave reactor of 0.915GHz that above-mentioned 3 mixing raw materials are positioned over microwave frequency, regulates microwave power to make temperature of reaction in 30mins, rise to 1720 DEG C from room temperature and keep 1720 DEG C to react 30min.Material is taken out after reaction end cools to 400 DEG C.Material surface is white, and internal structure densification has sintering, is obtained calcium carbide product.Product is through detection of getting angry, and its gas forming amount reaches 309L/Kg.
Table 5 coke composition
| Project | M c | A w | V a | W v |
| Content | 87.34 | 0.27 | 7.79 | 4.60 |
Above are only part preferred embodiment of the present invention, the present invention is not limited in the content of embodiment.To those skilled in the art, can have various change and change in the concept of technical solution of the present invention, any change done and change, all within scope.
Claims (10)
1. utilize a method for micro-wave energy low-temperature growth calcium carbide, the method is: take coal as carbon source, Wingdale or lime be calcium source, under Microwave Heating, and Reactive Synthesis calcium carbide.
2. a kind of method utilizing micro-wave energy low-temperature growth calcium carbide as claimed in claim 1, is characterized in that: the temperature of reaction of synthesis calcium carbide is 1300 ~ 2000 DEG C, and reaction pressure is 0.3 ~ 1.1atm, and the reaction times is 3 ~ 120min.
3. a kind of method utilizing micro-wave energy low-temperature growth calcium carbide as claimed in claim 1, is characterized in that: the temperature of reaction of synthesis calcium carbide is 1550 ~ 1750 DEG C, and reaction pressure is 0.7 ~ 1.0atm, and the reaction times is 20 ~ 40min.
4. a kind of method utilizing micro-wave energy low-temperature growth calcium carbide as claimed in claim 1, is characterized in that: described coal is selected from hard coal, brown coal, long-flame coal, one or more in semicoke, coking coal.
5. a kind of method utilizing micro-wave energy low-temperature growth calcium carbide as claimed in claim 1, it is characterized in that: when described calcium source is lime, the mol ratio of carbon and calcium oxide is 4.5 ~ 3.5:1.
6. a kind of method utilizing micro-wave energy low-temperature growth calcium carbide as claimed in claim 1, it is characterized in that: when described calcium source is Wingdale, the mol ratio of carbon and calcium carbonate is 3.5 ~ 2.7:1.
7. a kind of method utilizing micro-wave energy low-temperature growth calcium carbide as claimed in claim 1, it is characterized in that: be mixed in proportion after described carbon source and the preliminary grinding of calcium source, then the mixture that super-refinement obtains super-refinement is carried out, recycling Microwave Heating Reactive Synthesis calcium carbide; The particle diameter of described preliminary grinding is 0.1 ~ 10mm, and the particle diameter of super-refinement is 5 μm ~ 0.1mm.
8. a kind of method utilizing micro-wave energy low-temperature growth calcium carbide as claimed in claim 1, is characterized in that: the mixture of described super-refinement is a granulated into particle rear feeding Reactive Synthesis calcium carbide, or the mixture of super-refinement direct charging Reactive Synthesis calcium carbide.
9. a kind of method utilizing micro-wave energy low-temperature growth calcium carbide as claimed in claim 1, it is characterized in that: utilize microwave radiation device to provide micro-wave energy, microwave radiation frequencies is the one or more frequencies within the scope of 0.915GHz ~ 140GHz.
10. a kind of method utilizing micro-wave energy low-temperature growth calcium carbide as claimed in claim 1, it is characterized in that: adopt boosting mode additional heat in calcium carbide building-up process, described boosting mode is selected from the waste heat of electrically heated, microwave heating, excess carbon combustion heating, emission.
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Cited By (6)
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| CN106629729A (en) * | 2016-12-07 | 2017-05-10 | 钢研晟华工程技术有限公司 | Method for smelting calcium carbide from limestone through one-step method |
| 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 |
| CN107937029A (en) * | 2017-12-22 | 2018-04-20 | 中国科学院上海高等研究院 | A kind of method and system of coal base calcium carbide acetylene |
| CN107986279A (en) * | 2017-12-22 | 2018-05-04 | 中国科学院上海高等研究院 | A kind of microwave furnace of calcium carbide reactor and prepare the method for calcium carbide using it |
| CN108675911A (en) * | 2018-08-21 | 2018-10-19 | 中国科学院上海高等研究院 | A kind of carbide acetylene production technology for reducing carbide slag and generating |
| CN113735126A (en) * | 2021-09-28 | 2021-12-03 | 北京化工大学 | Method for preparing calcium carbide at low temperature by utilizing electromagnetic induction technology |
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Cited By (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106629729A (en) * | 2016-12-07 | 2017-05-10 | 钢研晟华工程技术有限公司 | Method for smelting calcium carbide from limestone through one-step method |
| 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 |
| CN107857267B (en) * | 2017-12-12 | 2019-11-19 | 中国科学院上海高等研究院 | A kind of method that vacuum low-pressure prepares calcium carbide |
| CN107937029A (en) * | 2017-12-22 | 2018-04-20 | 中国科学院上海高等研究院 | A kind of method and system of coal base calcium carbide acetylene |
| CN107986279A (en) * | 2017-12-22 | 2018-05-04 | 中国科学院上海高等研究院 | A kind of microwave furnace of calcium carbide reactor and prepare the method for calcium carbide using it |
| CN107986279B (en) * | 2017-12-22 | 2023-03-10 | 中国科学院上海高等研究院 | Microwave calcium carbide furnace reactor and method for preparing calcium carbide by using same |
| CN108675911A (en) * | 2018-08-21 | 2018-10-19 | 中国科学院上海高等研究院 | A kind of carbide acetylene production technology for reducing carbide slag and generating |
| CN108675911B (en) * | 2018-08-21 | 2021-06-25 | 中国科学院上海高等研究院 | Calcium carbide acetylene production process capable of reducing generation of calcium carbide slag |
| CN113735126A (en) * | 2021-09-28 | 2021-12-03 | 北京化工大学 | Method for preparing calcium carbide at low temperature by utilizing electromagnetic induction technology |
| CN113735126B (en) * | 2021-09-28 | 2022-07-12 | 北京化工大学 | Method for preparing calcium carbide at low temperature by utilizing electromagnetic induction technology |
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