CN104327900A - Direct desulfurization method of high-sulfur coal by microwave radiation - Google Patents
Direct desulfurization method of high-sulfur coal by microwave radiation Download PDFInfo
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Abstract
The invention discloses a direct desulfurization method of high-sulfur coal by microwave radiation, which comprises the following steps: 1) putting high-sulfur coal in a reactor, and putting the reactor in a microwave radiation reaction furnace; and 2) introducing carrier gas, switching on the microwave radiation reaction furnace to perform microwave radiation on the high-sulfur coal after the gas flow is stable, and switching off the microwave radiation reaction furnace. The desulfurization percent is 50% or so, the microwave-radiation high-sulfur coal desulfurization process has small influence on the major structure of coal, the heating amount, binding property, intrinsic structure characteristic, crystallinity, stability, thermal chemical properties and the like of the coal are kept stable, and the loss rate of coal is very low; and the microwave-radiation high-sulfur coal direct desulfurization method has the advantages of short production cycle, low equipment investment, high reaction speed, low energy consumption and high controllability, and can implement continuous production.
Description
Technical field
The present invention relates to a kind of method of coal desulfurization, particularly relate to a kind of method of microwave radiation high-sulfur coal direct desulfurization.
Background technology
Coal occupies the ratio of about 70% in AND ENERGY RESOURCES CONSUMPTION IN CHINA structure, is the important guarantee of sustain economic fast development.But the sulphur in coal generates SO in burning with process of coking
2, cause serious atmospheric pollution and cause series of environmental problems.Therefore, coal desulfurization has important meaning to raising coal resources utilising efficiency and environment protection.In coal, sulphur can be divided into inorganic sulfur and organosulfur according to existence, wherein, inorganic sulfur mainly comprises pyrite, white pyrite, barite, gypsum compound and some iron content class vitriol, and organosulfur is mainly present in organic structure with forms such as thiophene-based aromatic compound, mercaptan, thioether, disulphide and thioquinones.Inorganic sulfur in coal can be removed by the physical method such as gravity treatment and flotation, but Physical only can remove part pyrite, and to fine-grained disseminated grain as the inorganic minerals such as vitriol remove and inapplicable.Organic sulfur removal is more difficult, and usually adopt the chemical process such as thermokalite lixiviation process and oxidation style, chemical method generally at strong acid/alkali or need react under elevated pressure conditions, may reduce the agglutinating value(of coal) of coal, swelling property and calorific value.Microbial desulfurization energy consumption is low, does not affect ature of coal, but existing Desulphurization Strains is single, and the production cycle is long, and facility investment is high, and the production by biological different situation that changes cannot be avoided, and sulfur removal technology is still immature, is only applicable to the pyritic sulphur removing microfine.
Microwave be frequency at 0.3-300GHz, wavelength is at the hertzian wave of 1mm-100cm, and the frequency that different substances absorbs micro-wave energy is different.FeS in coal
2higher than ature of coal with the heat absorption rate of ash content, when sulfide is rapidly heated to temperature of reaction, ature of coal is not obviously generated heat, and the raising of ature of coal temperature needs the carrying out of pre-heat transfer process.Therefore, microwave radiation may realize the physical structure that is not only stripped of sulphur content but also do not destroy ature of coal.Coal directly irradiates by microwave direct desulfurization method exactly under microwave, utilizes microwave excellence heat effect fast, makes the containing sulfur minerals decomposes in coal, thus reaches the object of desulfurization.When raw coal 2.45GHz frequency, power at 500W or higher time, after microwave irradiation for some time, organosulfur in coal decomposes, and discharges H
2s and SO
2gas, at coal Surface Creation elemental sulfur.In addition, the inorganic sulfurs such as pyrite in coal can be converted into acid-soluble pyrrhotite and troilite under the irradiation of microwave, and this removes follow-up the condition of creating for inorganic sulfur.
Use the advantage of microwave radiation direct desulfurization technology to be that the agent structure impact of sweetening process on ature of coal is less, desulphurization reaction speed is fast, mild condition, energy consumption are low, be easy to control, the application potential of this technology in coal desulfurization be huge, have a extensive future.
Summary of the invention
The technical problem to be solved in the present invention is to provide a kind of method of microwave radiation high-sulfur coal direct desulfurization.The method can solve the present situation that the high and existing sulfur removal technology of coal sulphur content can not meet the needs to Coal Quality, and coal in China consumption is large, therefore, is with a wide range of applications.
For solving the problems of the technologies described above, the method for microwave radiation high-sulfur coal direct desulfurization of the present invention, comprises step:
1) high-sulfur coal is placed in reaction unit, and this reaction unit is placed in microwave radiation Reaktionsofen;
2) pass into carrier gas, after air-flow is steady, opens microwave radiation Reaktionsofen switch, microwave radiation (directly to carry out desulfurization process) is carried out to high-sulfur coal, then, close microwave radiation Reaktionsofen switch (namely stopping microwave radiation).
Described method, also comprises step: the coal after microwave radiation (i.e. desulfurization process) is cooled to room temperature, and sampling is preserved and analyzes.
Described step 1) in, the high-sulfur coal of high-sulfur coal to be sulphur content be 2.0wt% ~ 6.0wt% (weight percent);
Reaction unit comprises: quartz reactor and quartzy airway etc.
Optimum condition high-sulfur coal being placed in reaction unit is: the thickness of coal seam of high-sulfur coal is 2 ~ 10cm (coal seam as high-sulfur coal accounts for 1/5 ~ 3/5 of the quartz reactor cumulative volume of reaction unit), and the coal particle diameter of high-sulfur coal is 0.1 ~ 5cm.
Described step 2) in, the method passing into carrier gas can be carries out passing into of carrier gas by the quartzy airway of above-mentioned reaction unit.Carrier gas comprises: one or more in air or rare gas element; Wherein, rare gas element comprises: nitrogen or helium; The flow velocity of carrier gas is 0 ~ 300ml/min.
Step 2) in, the optimum condition of microwave radiation is as follows:
Microwave radiation frequencies is 2450 ± 50MHz, and microwave irradiation power is 500 ~ 1000W, and microwave irradiation time is 2 ~ 15min, and microwave radiation temperature is 100 ~ 250 DEG C.
The present invention be directed to coal in China sulphur content generally higher, sulfur removal technology is loaded down with trivial details, the present situation of inefficiency proposes, and compared with prior art, the present invention has the following advantages:
1) microwave radiation high-sulfur coal desulfurization can deviate from sulfoxide type, sulfone class and the mercaptan/ether in organosulfur while deviating from inorganic sulfur sulfurous iron ore, and desulfurization degree is about 50%;
2) relative to chemical method desulfurization, the agent structure impact of microwave radiation high-sulfur Desulphurization Process of Coal on ature of coal is less, the thermal value, cohesiveness, immanent structure characteristic, degree of crystallinity, stability, thermochemistry etc. of coal keep stable, and the rate of loss of coal is extremely low;
3) microwave radiation high-sulfur coal direct desulfurization is with short production cycle, facility investment is low, speed of response is fast, energy consumption is low, be easy to control and can continuous prodution be realized.
Embodiment
Below in conjunction with embodiment, further detailed description is done to the present invention, but be only not used in for illustration of the present invention and limit the scope of the invention.Other any do not deviate from do under spirit of the present invention and principle change, modification, substitute, combine, simplify, be equivalents, fall within the application's appended claims limited range equally.
Embodiment 1
Accurately take 30g Shanxi high-sulfur coal in 200ml quartz reactor, quartz reactor is fixed in microwave radiation Reaktionsofen, the air that flow is 100ml/min is passed into through quartzy airway, after steady air current, turn on the power switch, the related process parameters of setting microwave treatment, design parameter condition is as follows:
Microwave radiation frequencies 2.45GHz, microwave power 600W, microwave irradiating time 10min, radiation temperature 120 DEG C, thickness of coal seam 6cm (accounting for 1/5 of quartz reactor cumulative volume), coal particle diameter 2cm.
Open microwave radiation Reaktionsofen switch (namely starting microwave radiation) and carry out microwave radiation desulfurization, after reaction terminates, be cooled to room temperature, collect the coal after microwave treatment in the enterprising row element analysis of German FLASH-2000 type organic element analyzer, be carrier gas with helium during ultimate analysis, furnace temperature is set to 950 DEG C.From ultimate analysis: after microwave radiation, the sulphur content of coal is 2.73%, desulfurization degree is 35.36%.
In addition, known by infrared, thermal weight loss, X-ray diffractometer and scanning electron microscope analysis, Shanxi Ci Linshan high-sulfur coal is through microwave radiation processing, and except desulfurization, the immanent structure characteristic, degree of crystallinity, stability, thermal value etc. of coal sample keep stable.
Embodiment 2
Accurately take 50g Shanxi high-sulfur coal in 200ml quartz reactor, quartz reactor is fixed in microwave radiation Reaktionsofen, the air that flow is 50ml/min is passed into through quartzy airway, after steady air current, turn on the power switch, the related process parameters of setting microwave treatment, design parameter condition is as follows:
Microwave radiation frequencies 2.45GHz, microwave power 800W, microwave irradiating time 6min, radiation temperature 150 DEG C, thickness of coal seam 3cm (accounting for 3/5 of quartz reactor cumulative volume), coal particle diameter 0.5cm.
Open microwave radiation Reaktionsofen switch (namely starting microwave radiation) and carry out microwave radiation desulfurization, after reaction terminates, be cooled to room temperature, collect the coal after microwave treatment in the enterprising row element analysis of German FLASH-2000 type organic element analyzer, be carrier gas with helium during ultimate analysis, furnace temperature is set to 950 DEG C.From ultimate analysis: after microwave radiation, the sulphur content of coal is 2.65%, desulfurization degree is 37.20%.
In addition, known by infrared, thermal weight loss, X-ray diffractometer and scanning electron microscope analysis, Shanxi Ci Linshan high-sulfur coal is through microwave radiation processing, and except desulfurization, the immanent structure characteristic, degree of crystallinity, stability, thermal value etc. of coal sample keep stable.
Embodiment 3
Accurately take 50g Shanxi high-sulfur coal in 200ml quartz reactor, be fixed on by quartz reactor in microwave radiation Reaktionsofen, no carrier gas passes into, and turns on the power switch, the related process parameters of setting microwave treatment, and design parameter condition is as follows:
Microwave radiation frequencies 2.45GHz, microwave power 800W, microwave irradiating time 8min, radiation temperature 180 DEG C, thickness of coal seam 4cm (accounting for 3/5 of quartz reactor cumulative volume), coal particle diameter 3cm (raw coal do not pulverized).
Open microwave radiation Reaktionsofen switch (namely starting microwave radiation) and carry out microwave radiation desulfurization, after reaction terminates, be cooled to room temperature, collect the coal after microwave treatment in the enterprising row element analysis of German FLASH-2000 type organic element analyzer, be carrier gas with helium during ultimate analysis, furnace temperature is set to 950 DEG C.From ultimate analysis: after microwave radiation, the sulphur content of coal is 2.19%, desulfurization degree is 47.66%.
In addition, known by infrared, thermal weight loss, X-ray diffractometer and scanning electron microscope analysis, Shanxi Ci Linshan high-sulfur coal is through microwave radiation processing, and except desulfurization, the immanent structure characteristic, degree of crystallinity, stability, thermal value etc. of coal sample keep stable.
Embodiment 4
Accurately take 40g Shanxi high-sulfur coal in 200ml quartz reactor, quartz reactor is fixed in microwave radiation Reaktionsofen, the nitrogen that flow is 50ml/min is passed into through quartzy airway, after steady air current, turn on the power switch, the related process parameters of setting microwave treatment, design parameter condition is as follows:
Microwave radiation frequencies 2.45GHz, microwave power 1000W, microwave irradiating time 6min, radiation temperature 160 DEG C, thickness of coal seam 5cm (accounting for 2/5 of quartz reactor cumulative volume), coal particle diameter 1cm.
Open microwave radiation Reaktionsofen switch (namely starting microwave radiation) and carry out microwave radiation desulfurization, after reaction terminates, be cooled to room temperature, collect the coal after microwave treatment in the enterprising row element analysis of German FLASH-2000 type organic element analyzer, be carrier gas with helium during ultimate analysis, furnace temperature is set to 950 DEG C.From ultimate analysis: after microwave radiation, the sulphur content of coal is 2.33%, desulfurization degree is 44.79%.
In addition, known by infrared, thermal weight loss, X-ray diffractometer and scanning electron microscope analysis, Shanxi Ci Linshan high-sulfur coal is through microwave radiation processing, and except desulfurization, the immanent structure characteristic, degree of crystallinity, stability, thermal value etc. of coal sample keep stable.
Embodiment 5
Accurately take 50g Shanxi high-sulfur coal in 200ml quartz reactor, be fixed on by quartz reactor in microwave radiation Reaktionsofen, no carrier gas passes into, and turns on the power switch, the related process parameters of setting microwave treatment, and design parameter condition is as follows:
Microwave radiation frequencies 2.45GHz, microwave power 800W, microwave irradiating time 8min, radiation temperature 190 DEG C, thickness of coal seam 3cm (accounting for 3/5 of quartz reactor cumulative volume), coal particle diameter 3cm (raw coal is not pulverized).
Open microwave radiation Reaktionsofen switch (namely starting microwave radiation) and carry out microwave radiation desulfurization, after reaction terminates, be cooled to room temperature, collect the coal after microwave treatment in the enterprising row element analysis of German FLASH-2000 type organic element analyzer, be carrier gas with helium during ultimate analysis, furnace temperature is set to 950 DEG C.From ultimate analysis: after microwave radiation, the sulphur content of coal is 2.05%, desulfurization degree is 50.19%.
In addition, known by infrared, thermal weight loss, X-ray diffractometer and scanning electron microscope analysis, Shanxi Ci Linshan high-sulfur coal is through microwave radiation processing, and except desulfurization, the immanent structure characteristic, degree of crystallinity, stability, thermal value etc. of coal sample keep stable.
From the above, microwave radiation high-sulfur coal desulfurization can deviate from inorganic sulfur in coal and organosulfur, desulfurization degree is about 50%, and the performance index of coal keep stable and rate of loss is extremely low before and after desulfurization, energy consumption of the present invention is low, be easy to control and can realize continuous prodution, can be used for the desulfurization upgrading of high-sulfur coal.
Claims (7)
1. a method for microwave radiation high-sulfur coal direct desulfurization, is characterized in that, comprise step:
1) high-sulfur coal is placed in reaction unit, and this reaction unit is placed in microwave radiation Reaktionsofen;
2) pass into carrier gas, after air-flow is steady, opens microwave radiation Reaktionsofen switch, microwave radiation is carried out to high-sulfur coal, then, close microwave radiation Reaktionsofen switch.
2. the method for claim 1, is characterized in that: described method, also comprises step: the coal after microwave radiation processing is cooled to room temperature, and sampling is preserved and analyzes.
3. the method for claim 1, is characterized in that: described step 1) in, the high-sulfur coal of high-sulfur coal to be sulphur content be 2.0wt% ~ 6.0wt%;
Reaction unit comprises: quartz reactor and quartzy airway.
4. the method for claim 1, is characterized in that: described step 1) in, condition high-sulfur coal being placed in reaction unit is:
The thickness of coal seam of high-sulfur coal is 2 ~ 10cm, and the coal particle diameter of high-sulfur coal is 0.1 ~ 5cm.
5. method as claimed in claim 3, is characterized in that: described step 1) in, condition high-sulfur coal being placed in reaction unit is:
The coal seam of high-sulfur coal accounts for 1/5 ~ 3/5 of the quartz reactor cumulative volume in reaction unit.
6. the method for claim 1, is characterized in that: described step 2) in, the method passing into carrier gas is carry out passing into of carrier gas by quartzy airway;
Carrier gas comprises: one or more in air or rare gas element; Wherein, rare gas element comprises: nitrogen or helium; The flow velocity of carrier gas is 0 ~ 300ml/min.
7. the method for claim 1, is characterized in that: described step 2) in, the condition of microwave radiation is as follows:
Microwave radiation frequencies is 2450 ± 50MHz, and microwave irradiation power is 500 ~ 1000W, and microwave irradiation time is 2 ~ 15min, and microwave radiation temperature is 100 ~ 250 DEG C.
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Cited By (8)
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| CN105166034A (en) * | 2015-08-17 | 2015-12-23 | 中国科学院上海高等研究院 | Microwave radiation drying method for high-moisture grain |
| CN105542899A (en) * | 2015-12-24 | 2016-05-04 | 刘家容 | Coal desulfurization method |
| CN105623775A (en) * | 2016-01-19 | 2016-06-01 | 太原科技大学 | Method for removing mercury, sulfur and nitrogen from coal gangue by microwave pyrolysis |
| CN107150998A (en) * | 2017-06-07 | 2017-09-12 | 中国科学院过程工程研究所 | A kind of coal desulfurization and the system and method for reclaiming elemental sulfur |
| CN107880969A (en) * | 2017-11-29 | 2018-04-06 | 亿利洁能科技（颍上）有限公司 | A kind of clean coal utilization method |
| CN108359507A (en) * | 2018-03-01 | 2018-08-03 | 王号德 | A kind of method of organic sulfur compound in removing bituminous coal |
| CN108728201A (en) * | 2018-06-22 | 2018-11-02 | 山西焦煤集团有限责任公司 | A kind of micro ware auxiliary catalysis ozone liquid phase oxidation sulphur coal sulfur method |
| CN109266418A (en) * | 2018-09-30 | 2019-01-25 | 青岛大学 | A method of arsenic in coal being leached under ultraviolet light using flue gas |
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Cited By (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105166034A (en) * | 2015-08-17 | 2015-12-23 | 中国科学院上海高等研究院 | Microwave radiation drying method for high-moisture grain |
| CN105542899A (en) * | 2015-12-24 | 2016-05-04 | 刘家容 | Coal desulfurization method |
| CN105542899B (en) * | 2015-12-24 | 2018-08-03 | 青海盛鸿能源科技有限公司 | A kind of coal desulfurization method |
| CN105623775A (en) * | 2016-01-19 | 2016-06-01 | 太原科技大学 | Method for removing mercury, sulfur and nitrogen from coal gangue by microwave pyrolysis |
| CN107150998A (en) * | 2017-06-07 | 2017-09-12 | 中国科学院过程工程研究所 | A kind of coal desulfurization and the system and method for reclaiming elemental sulfur |
| CN107150998B (en) * | 2017-06-07 | 2020-01-07 | 中国科学院过程工程研究所 | System and method for coal desulfurization and elemental sulfur recovery |
| CN107880969A (en) * | 2017-11-29 | 2018-04-06 | 亿利洁能科技（颍上）有限公司 | A kind of clean coal utilization method |
| CN108359507A (en) * | 2018-03-01 | 2018-08-03 | 王号德 | A kind of method of organic sulfur compound in removing bituminous coal |
| CN108728201A (en) * | 2018-06-22 | 2018-11-02 | 山西焦煤集团有限责任公司 | A kind of micro ware auxiliary catalysis ozone liquid phase oxidation sulphur coal sulfur method |
| CN109266418A (en) * | 2018-09-30 | 2019-01-25 | 青岛大学 | A method of arsenic in coal being leached under ultraviolet light using flue gas |
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