CN104327900A - Direct desulfurization method of high-sulfur coal by microwave radiation - Google Patents
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- 239000003245 coal Substances 0.000 title claims abstract description 111
- 230000005855 radiation Effects 0.000 title claims abstract description 74
- 229910052717 sulfur Inorganic materials 0.000 title claims abstract description 62
- 239000011593 sulfur Substances 0.000 title claims abstract description 62
- 238000006477 desulfuration reaction Methods 0.000 title claims abstract description 48
- 230000023556 desulfurization Effects 0.000 title claims abstract description 48
- 238000000034 method Methods 0.000 title claims abstract description 36
- 238000006243 chemical reaction Methods 0.000 claims abstract description 34
- 239000012159 carrier gas Substances 0.000 claims abstract description 18
- 239000007789 gas Substances 0.000 claims abstract description 8
- 239000010453 quartz Substances 0.000 claims description 24
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 24
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 claims description 22
- 229910052734 helium Inorganic materials 0.000 claims description 7
- 239000001307 helium Substances 0.000 claims description 7
- SWQJXJOGLNCZEY-UHFFFAOYSA-N helium atom Chemical compound [He] SWQJXJOGLNCZEY-UHFFFAOYSA-N 0.000 claims description 7
- 239000002245 particle Substances 0.000 claims description 7
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 5
- 229910052757 nitrogen Inorganic materials 0.000 claims description 2
- 239000005864 Sulphur Substances 0.000 claims 1
- 230000001186 cumulative effect Effects 0.000 claims 1
- 238000005070 sampling Methods 0.000 claims 1
- 238000005265 energy consumption Methods 0.000 abstract description 6
- 239000000126 substance Substances 0.000 abstract description 5
- 238000010924 continuous production Methods 0.000 abstract description 3
- 238000004519 manufacturing process Methods 0.000 abstract description 3
- 238000010438 heat treatment Methods 0.000 abstract description 2
- 230000036632 reaction speed Effects 0.000 abstract description 2
- 238000004458 analytical method Methods 0.000 description 11
- NIFIFKQPDTWWGU-UHFFFAOYSA-N pyrite Chemical class [Fe+2].[S-][S-] NIFIFKQPDTWWGU-UHFFFAOYSA-N 0.000 description 7
- 125000001741 organic sulfur group Chemical group 0.000 description 6
- 229910052683 pyrite Inorganic materials 0.000 description 6
- 238000000921 elemental analysis Methods 0.000 description 5
- 239000011028 pyrite Substances 0.000 description 5
- 230000000694 effects Effects 0.000 description 3
- RWSOTUBLDIXVET-UHFFFAOYSA-N Dihydrogen sulfide Chemical class S RWSOTUBLDIXVET-UHFFFAOYSA-N 0.000 description 2
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 2
- 239000003513 alkali Substances 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 230000007613 environmental effect Effects 0.000 description 2
- 239000011261 inert gas Substances 0.000 description 2
- 229910052500 inorganic mineral Inorganic materials 0.000 description 2
- 229910052960 marcasite Inorganic materials 0.000 description 2
- 230000000813 microbial effect Effects 0.000 description 2
- 238000000053 physical method Methods 0.000 description 2
- MBMLMWLHJBBADN-UHFFFAOYSA-N Ferrous sulfide Chemical compound [Fe]=S MBMLMWLHJBBADN-UHFFFAOYSA-N 0.000 description 1
- QAOWNCQODCNURD-UHFFFAOYSA-L Sulfate Chemical compound [O-]S([O-])(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-L 0.000 description 1
- UCKMPCXJQFINFW-UHFFFAOYSA-N Sulphide Chemical compound [S-2] UCKMPCXJQFINFW-UHFFFAOYSA-N 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 238000003915 air pollution Methods 0.000 description 1
- 150000001491 aromatic compounds Chemical class 0.000 description 1
- TZCXTZWJZNENPQ-UHFFFAOYSA-L barium sulfate Chemical class [Ba+2].[O-]S([O-])(=O)=O TZCXTZWJZNENPQ-UHFFFAOYSA-L 0.000 description 1
- 229910052601 baryte Inorganic materials 0.000 description 1
- 239000010428 baryte Chemical class 0.000 description 1
- 238000004939 coking Methods 0.000 description 1
- 238000002485 combustion reaction Methods 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 238000001816 cooling Methods 0.000 description 1
- 229910001873 dinitrogen Inorganic materials 0.000 description 1
- 150000002019 disulfides Chemical class 0.000 description 1
- 150000002170 ethers Chemical class 0.000 description 1
- 239000010419 fine particle Substances 0.000 description 1
- 238000005188 flotation Methods 0.000 description 1
- 230000005484 gravity Effects 0.000 description 1
- 229910052602 gypsum Inorganic materials 0.000 description 1
- 239000010440 gypsum Chemical class 0.000 description 1
- 229910052742 iron Inorganic materials 0.000 description 1
- 238000002386 leaching Methods 0.000 description 1
- 239000011707 mineral Substances 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 239000005416 organic matter Substances 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 229910052952 pyrrhotite Inorganic materials 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
- 238000003860 storage Methods 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 150000003457 sulfones Chemical class 0.000 description 1
- 150000003462 sulfoxides Chemical class 0.000 description 1
- 150000003467 sulfuric acid derivatives Chemical class 0.000 description 1
- 230000002459 sustained effect Effects 0.000 description 1
- 150000003568 thioethers Chemical class 0.000 description 1
- 229930192474 thiophene Natural products 0.000 description 1
- 150000003577 thiophenes Chemical class 0.000 description 1
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Abstract
Description
技术领域technical field
本发明涉及一种煤炭脱硫的方法，特别是涉及一种微波辐射高硫煤炭直接脱硫的方法。The invention relates to a method for coal desulfurization, in particular to a method for direct desulfurization of high-sulfur coal by microwave radiation.
背景技术Background technique
煤炭在我国能源消耗结构中占有70％左右的比例，是经济持续快速发展的重要保证。但煤炭中的硫在燃烧与炼焦过程中生成SO2，造成严重的空气污染并引发一系列环境问题。因此，煤炭脱硫对提高煤炭资源利用效率和环境保护有重要的意义。煤中硫依照存在状态可分为无机硫和有机硫，其中，无机硫主要包括黄铁矿、白铁矿、重晶石、石膏类化合物及一些含铁类硫酸盐，有机硫主要以噻吩类芳香化合物、硫醇、硫醚、二硫化物和硫醌等形式存在于有机质结构中。煤中的无机硫可以通过重选和浮选等物理方法脱除，但物理法仅能脱除部分黄铁矿，而且对细粒嵌布的如硫酸盐等无机矿物质的脱除并不适用。有机硫脱除比较困难，通常采用热碱浸出法和氧化法等化学方法，化学法一般需在强酸/碱或在高压条件下反应，可能会降低煤炭的黏结性、膨胀性以及热值。微生物脱硫能耗低，对煤质没有影响，但现有脱硫菌种单一，生产周期长，设备投资高，微生物产生变异的情况无法避免，脱硫工艺尚不成熟，仅适用于脱除微细粒的黄铁矿硫。Coal accounts for about 70% of my country's energy consumption structure, which is an important guarantee for sustained and rapid economic development. However, the sulfur in coal generates SO 2 in the process of combustion and coking, which causes serious air pollution and a series of environmental problems. Therefore, coal desulfurization is of great significance to improving the utilization efficiency of coal resources and environmental protection. Sulfur in coal can be divided into inorganic sulfur and organic sulfur according to the state of existence. Among them, inorganic sulfur mainly includes pyrite, marcasite, barite, gypsum compounds and some iron-containing sulfates, and organic sulfur mainly consists of thiophenes. Aromatic compounds, mercaptans, thioethers, disulfides and thioquinones exist in organic matter structures. Inorganic sulfur in coal can be removed by physical methods such as gravity separation and flotation, but physical methods can only remove part of pyrite, and are not suitable for the removal of fine-grained inorganic minerals such as sulfate . Organic sulfur removal is difficult, and chemical methods such as hot alkali leaching and oxidation are usually used. Chemical methods generally need to be reacted under strong acid/alkali or high pressure conditions, which may reduce the cohesiveness, expansion and calorific value of coal. Microbial desulfurization has low energy consumption and has no effect on coal quality. However, the existing desulfurization strains are single, the production cycle is long, the equipment investment is high, and the situation of microbial variation is unavoidable. The desulfurization process is not yet mature and is only suitable for the removal of fine particles. pyrite sulfur.
微波是频率在0.3-300GHz，波长在1mm-100cm的电磁波，不同物质吸收微波能的频率不同。煤中FeS2和灰分的吸热速率比煤质高，当硫化物被迅速加热到反应温度时，煤质并未明显发热，煤质温度的提高有待预热传导过程的进行。因此，微波辐射可能实现既脱除了硫分又不破坏煤质的物理结构。微波直接脱硫法就是将煤直接在微波下照射，利用微波优异快速的加热作用，使煤中的含硫矿物受热分解，从而达到脱硫的目的。当原煤在2.45GHz频率、功率在500W或更高时，经微波照射一段时间后，煤中的有机硫分解，释放出H2S和SO2气体，在煤表面生成单质硫。此外，煤中黄铁矿等无机硫在微波的照射下可转化为可溶于酸的磁黄铁矿和陨硫铁，这为无机硫在后续脱除创造了条件。Microwave is an electromagnetic wave with a frequency of 0.3-300GHz and a wavelength of 1mm-100cm. Different substances absorb microwave energy at different frequencies. The heat absorption rate of FeS2 and ash in coal is higher than that of coal. When the sulfide is rapidly heated to the reaction temperature, the coal does not generate heat obviously, and the increase of coal temperature depends on the preheating process. Therefore, microwave radiation may achieve the removal of sulfur without destroying the physical structure of coal. Microwave direct desulfurization method is to directly irradiate coal under microwave, and use the excellent and rapid heating effect of microwave to decompose sulfur-containing minerals in coal by heat, so as to achieve the purpose of desulfurization. When the raw coal has a frequency of 2.45GHz and a power of 500W or higher, after a period of microwave irradiation, the organic sulfur in the coal decomposes, releases H 2 S and SO 2 gases, and generates elemental sulfur on the coal surface. In addition, inorganic sulfur such as pyrite in coal can be converted into acid-soluble pyrrhotite and troilite under microwave irradiation, which creates conditions for the subsequent removal of inorganic sulfur.
使用微波辐射直接脱硫技术的优势是脱硫过程对煤质的主体结构影响较小，脱硫反应速度快、条件温和、能耗低、易于控制，该技术在煤炭脱硫方面的应用潜力巨大、前景广阔。The advantage of direct desulfurization technology using microwave radiation is that the desulfurization process has little impact on the main structure of coal quality, fast desulfurization reaction speed, mild conditions, low energy consumption, and easy control. This technology has great application potential and broad prospects in coal desulfurization.
发明内容Contents of the invention
本发明要解决的技术问题是提供一种微波辐射高硫煤炭直接脱硫的方法。该方法能解决煤炭含硫量高且现有脱硫工艺不能满足对煤炭质量的需要的现状，而且我国煤炭消费量大，因此，具有广泛的应用前景。The technical problem to be solved by the present invention is to provide a method for direct desulfurization of high-sulfur coal by microwave radiation. The method can solve the current situation that the coal has high sulfur content and the existing desulfurization process cannot meet the needs of coal quality, and the coal consumption in my country is large, so it has broad application prospects.
为解决上述技术问题，本发明的微波辐射高硫煤炭直接脱硫的方法，包括步骤：In order to solve the above-mentioned technical problems, the method for direct desulfurization of high-sulfur coal by microwave radiation of the present invention comprises steps:
1)将高硫煤炭置于反应装置中，并将该反应装置置于微波辐射反应炉内；1) placing high-sulfur coal in a reaction device, and placing the reaction device in a microwave radiation reaction furnace;
2)通入载气，待气流平稳后，打开微波辐射反应炉开关，对高硫煤炭进行微波辐射(以直接进行脱硫处理)，然后，关闭微波辐射反应炉开关(即停止微波辐射)。2) Pass in the carrier gas, and after the gas flow is stable, turn on the switch of the microwave radiation reaction furnace to irradiate the high-sulfur coal with microwaves (for direct desulfurization treatment), and then turn off the switch of the microwave radiation reaction furnace (that is, stop the microwave radiation).
所述方法，还包括步骤：将微波辐射(即脱硫处理)后的煤炭冷却至室温，取样保存并分析。The method also includes the step of: cooling the coal after microwave radiation (that is, desulfurization treatment) to room temperature, taking samples for storage and analysis.
所述步骤1)中，高硫煤炭是硫含量为2.0wt％～6.0wt％(重量百分比)的高硫煤炭；In the step 1), the high-sulfur coal is a high-sulfur coal with a sulfur content of 2.0wt% to 6.0wt% (weight percent);
反应装置包括：石英反应器和石英导气管等。The reaction device includes: a quartz reactor and a quartz gas pipe.
将高硫煤炭置于反应装置的优选条件为：高硫煤炭的煤层厚度为2～10cm(如高硫煤炭的煤层占反应装置中的石英反应器总体积的1/5～3/5)，高硫煤炭的煤粒径为0.1～5cm。The preferred condition for placing high-sulfur coal in the reaction device is: the thickness of the coal seam of high-sulfur coal is 2 to 10 cm (such as the coal seam of high-sulfur coal accounts for 1/5 to 3/5 of the total volume of the quartz reactor in the reaction device), The coal particle size of high-sulfur coal is 0.1-5cm.
所述步骤2)中，通入载气的方法可为通过上述反应装置的石英导气管进行载气的通入。载气包括：空气或惰性气体中的一种或多种；其中，惰性气体包括：氮气或氦气；载气的流速为0～300ml/min。In the step 2), the method of feeding the carrier gas may be to feed the carrier gas through the quartz gas guide tube of the above-mentioned reaction device. The carrier gas includes: one or more of air or inert gas; wherein, the inert gas includes: nitrogen or helium; the flow rate of the carrier gas is 0-300ml/min.
步骤2)中，微波辐射的优选条件如下：Step 2) in, the optimal condition of microwave radiation is as follows:
微波辐射频率为2450±50MHz，微波辐射功率为500～1000W，微波辐射时间为2～15min，微波辐射温度为100～250℃。The microwave radiation frequency is 2450±50MHz, the microwave radiation power is 500-1000W, the microwave radiation time is 2-15min, and the microwave radiation temperature is 100-250°C.
本发明是针对我国煤炭含硫量普遍偏高、脱硫工艺繁琐、效率低下的现状而提出的，而且与现有技术相比，本发明具有以下优点：The present invention is proposed aiming at the present situation that the coal sulfur content in my country is generally high, the desulfurization process is cumbersome, and the efficiency is low, and compared with the prior art, the present invention has the following advantages:
1)微波辐射高硫煤炭脱硫可以在脱出无机硫硫铁矿的同时脱出有机硫中的亚砜类、砜类和硫醇/醚，脱硫率在50％左右；1) Desulfurization of high-sulfur coal by microwave radiation can remove sulfoxides, sulfones and mercaptans/ethers in organic sulfur while removing inorganic sulfur pyrite, and the desulfurization rate is about 50%;
2)相对于化学法脱硫，微波辐射高硫煤炭脱硫过程对煤质的主体结构影响较小，煤炭的发热量、粘结性、内在结构特性、结晶度、稳定性、热化学性等保持稳定，煤炭的损失率极低；2) Compared with chemical desulfurization, the desulfurization process of microwave radiation high-sulfur coal has little effect on the main structure of coal quality, and the calorific value, cohesiveness, internal structural characteristics, crystallinity, stability, and thermochemical properties of coal remain stable. , the loss rate of coal is extremely low;
3)微波辐射高硫煤炭直接脱硫生产周期短、设备投资低，反应速度快、能耗低、易于控制且可实现连续化生产。3) Direct desulfurization of high-sulfur coal by microwave radiation has a short production cycle, low equipment investment, fast response, low energy consumption, easy control and continuous production.
具体实施方式Detailed ways
下面结合实施例对本发明做进一步详细的描述，但仅用于说明本发明而不用于限制本发明的范围。其他任何在未背离本发明的精神实质与原理下所作的改变、修饰、替代、结合、简化，均为等效形式，同样落于本申请所附权利要求书所限定的范围。The present invention will be described in further detail below in conjunction with the examples, but only for illustrating the present invention and not for limiting the scope of the present invention. Any other changes, modifications, substitutions, combinations, and simplifications made without departing from the spirit and principles of the present invention are all equivalent forms, and also fall within the scope defined by the appended claims of this application.
实施例1Example 1
精确称取30g山西高硫煤炭于200ml石英反应器中，将石英反应器固定于微波辐射反应炉内，经石英导气管通入流量为100ml/min的空气，等气流稳定后，打开电源开关，设定微波处理的相关工艺参数，具体参数条件如下：Accurately weigh 30g of Shanxi high-sulfur coal in a 200ml quartz reactor, fix the quartz reactor in the microwave radiation reaction furnace, pass air with a flow rate of 100ml/min through the quartz air duct, and turn on the power switch after the air flow is stable. Set the relevant process parameters of microwave treatment, the specific parameter conditions are as follows:
微波辐射频率2.45GHz，微波功率600W，微波照射时间10min，辐射温度120℃，煤层厚度6cm(占石英反应器总体积的1/5)，煤粒径2cm。The microwave radiation frequency is 2.45GHz, the microwave power is 600W, the microwave irradiation time is 10min, the radiation temperature is 120°C, the coal seam thickness is 6cm (accounting for 1/5 of the total volume of the quartz reactor), and the coal particle size is 2cm.
打开微波辐射反应炉开关(即启动微波辐射)进行微波辐射脱硫，反应结束后，冷却至室温，收集微波处理后的煤炭在德国FLASH-2000型有机元素分析仪上进行元素分析，元素分析时以氦气为载气，炉温设置为950℃。由元素分析可知：微波辐射后煤炭的硫含量为2.73％，脱硫率为35.36％。Turn on the microwave radiation reaction furnace switch (i.e. start microwave radiation) to carry out microwave radiation desulfurization. After the reaction is over, cool to room temperature, collect the microwave-treated coal and carry out element analysis on the German FLASH-2000 organic element analyzer. Helium was used as the carrier gas, and the furnace temperature was set at 950 °C. According to the elemental analysis, the sulfur content of the coal after microwave radiation is 2.73%, and the desulfurization rate is 35.36%.
另外，通过红外、热失重、X射线衍射仪及扫描电镜分析可知，山西慈林山高硫煤炭经微波辐射处理，除脱硫外，煤样的内在结构特性、结晶度、稳定性、发热量等保持稳定。In addition, through infrared, thermogravimetric, X-ray diffractometer and scanning electron microscope analysis, it can be seen that the high-sulfur coal in Cilin Mountain, Shanxi Province is treated with microwave radiation. In addition to desulfurization, the internal structural characteristics, crystallinity, stability, and calorific value of the coal sample remain stable. .
实施例2Example 2
精确称取50g山西高硫煤炭于200ml石英反应器中，将石英反应器固定于微波辐射反应炉内，经石英导气管通入流量为50ml/min的空气，等气流稳定后，打开电源开关，设定微波处理的相关工艺参数，具体参数条件如下：Accurately weigh 50g of Shanxi high-sulfur coal in a 200ml quartz reactor, fix the quartz reactor in the microwave radiation reaction furnace, pass air with a flow rate of 50ml/min through the quartz air duct, and turn on the power switch after the air flow is stable. Set the relevant process parameters of microwave treatment, the specific parameter conditions are as follows:
微波辐射频率2.45GHz，微波功率800W，微波照射时间6min，辐射温度150℃，煤层厚度3cm(占石英反应器总体积的3/5)，煤粒径0.5cm。The microwave radiation frequency is 2.45GHz, the microwave power is 800W, the microwave irradiation time is 6min, the radiation temperature is 150°C, the coal seam thickness is 3cm (3/5 of the total volume of the quartz reactor), and the coal particle size is 0.5cm.
打开微波辐射反应炉开关(即启动微波辐射)进行微波辐射脱硫，反应结束后，冷却至室温，收集微波处理后的煤炭在德国FLASH-2000型有机元素分析仪上进行元素分析，元素分析时以氦气为载气，炉温设置为950℃。由元素分析可知：微波辐射后煤炭的硫含量为2.65％，脱硫率为37.20％。Turn on the microwave radiation reaction furnace switch (i.e. start microwave radiation) to carry out microwave radiation desulfurization. After the reaction is over, cool to room temperature, collect the microwave-treated coal and carry out element analysis on the German FLASH-2000 organic element analyzer. Helium was used as the carrier gas, and the furnace temperature was set at 950 °C. According to elemental analysis, the sulfur content of coal after microwave radiation is 2.65%, and the desulfurization rate is 37.20%.
另外，通过红外、热失重、X射线衍射仪及扫描电镜分析可知，山西慈林山高硫煤炭经微波辐射处理，除脱硫外，煤样的内在结构特性、结晶度、稳定性、发热量等保持稳定。In addition, through infrared, thermogravimetric, X-ray diffractometer and scanning electron microscope analysis, it can be seen that the high-sulfur coal in Cilin Mountain, Shanxi Province is treated with microwave radiation. In addition to desulfurization, the internal structural characteristics, crystallinity, stability, and calorific value of the coal sample remain stable. .
实施例3Example 3
精确称取50g山西高硫煤炭于200ml石英反应器中，将石英反应器固定于微波辐射反应炉内，无载气通入，打开电源开关，设定微波处理的相关工艺参数，具体参数条件如下：Accurately weigh 50g of Shanxi high-sulfur coal in a 200ml quartz reactor, fix the quartz reactor in the microwave radiation reaction furnace, pass in no carrier gas, turn on the power switch, and set the relevant process parameters for microwave treatment. The specific parameter conditions are as follows :
微波辐射频率2.45GHz，微波功率800W，微波照射时间8min，辐射温度180℃，煤层厚度4cm(占石英反应器总体积的3/5)，煤粒径3cm(未粉碎的原煤)。The microwave radiation frequency is 2.45GHz, the microwave power is 800W, the microwave irradiation time is 8min, the radiation temperature is 180°C, the coal seam thickness is 4cm (accounting for 3/5 of the total volume of the quartz reactor), and the coal particle size is 3cm (unground raw coal).
打开微波辐射反应炉开关(即启动微波辐射)进行微波辐射脱硫，反应结束后，冷却至室温，收集微波处理后的煤炭在德国FLASH-2000型有机元素分析仪上进行元素分析，元素分析时以氦气为载气，炉温设置为950℃。由元素分析可知：微波辐射后煤炭的硫含量为2.19％，脱硫率为47.66％。Turn on the microwave radiation reaction furnace switch (i.e. start microwave radiation) to carry out microwave radiation desulfurization. After the reaction is over, cool to room temperature, collect the microwave-treated coal and carry out element analysis on the German FLASH-2000 organic element analyzer. Helium was used as the carrier gas, and the furnace temperature was set at 950 °C. According to the elemental analysis, the sulfur content of the coal after microwave radiation is 2.19%, and the desulfurization rate is 47.66%.
另外，通过红外、热失重、X射线衍射仪及扫描电镜分析可知，山西慈林山高硫煤炭经微波辐射处理，除脱硫外，煤样的内在结构特性、结晶度、稳定性、发热量等保持稳定。In addition, through infrared, thermogravimetric, X-ray diffractometer and scanning electron microscope analysis, it can be seen that the high-sulfur coal in Cilin Mountain, Shanxi Province is treated with microwave radiation. In addition to desulfurization, the internal structural characteristics, crystallinity, stability, and calorific value of the coal sample remain stable. .
实施例4Example 4
精确称取40g山西高硫煤炭于200ml石英反应器中，将石英反应器固定于微波辐射反应炉内，经石英导气管通入流量为50ml/min的氮气，等气流稳定后，打开电源开关，设定微波处理的相关工艺参数，具体参数条件如下：Accurately weigh 40g of Shanxi high-sulfur coal in a 200ml quartz reactor, fix the quartz reactor in the microwave radiation reaction furnace, and pass nitrogen gas with a flow rate of 50ml/min through the quartz gas guide tube, and turn on the power switch after the air flow is stable. Set the relevant process parameters of microwave treatment, the specific parameter conditions are as follows:
微波辐射频率2.45GHz，微波功率1000W，微波照射时间6min，辐射温度160℃，煤层厚度5cm(占石英反应器总体积的2/5)，煤粒径1cm。The microwave radiation frequency is 2.45GHz, the microwave power is 1000W, the microwave irradiation time is 6min, the radiation temperature is 160°C, the coal seam thickness is 5cm (2/5 of the total volume of the quartz reactor), and the coal particle size is 1cm.
打开微波辐射反应炉开关(即启动微波辐射)进行微波辐射脱硫，反应结束后，冷却至室温，收集微波处理后的煤炭在德国FLASH-2000型有机元素分析仪上进行元素分析，元素分析时以氦气为载气，炉温设置为950℃。由元素分析可知：微波辐射后煤炭的硫含量为2.33％，脱硫率为44.79％。Turn on the microwave radiation reaction furnace switch (i.e. start microwave radiation) to carry out microwave radiation desulfurization. After the reaction is over, cool to room temperature, collect the microwave-treated coal and carry out element analysis on the German FLASH-2000 organic element analyzer. Helium was used as the carrier gas, and the furnace temperature was set at 950 °C. According to the elemental analysis, the sulfur content of the coal after microwave radiation is 2.33%, and the desulfurization rate is 44.79%.
另外，通过红外、热失重、X射线衍射仪及扫描电镜分析可知，山西慈林山高硫煤炭经微波辐射处理，除脱硫外，煤样的内在结构特性、结晶度、稳定性、发热量等保持稳定。In addition, through infrared, thermogravimetric, X-ray diffractometer and scanning electron microscope analysis, it can be seen that the high-sulfur coal in Cilin Mountain, Shanxi Province is treated with microwave radiation. In addition to desulfurization, the internal structural characteristics, crystallinity, stability, and calorific value of the coal sample remain stable. .
实施例5Example 5
精确称取50g山西高硫煤炭于200ml石英反应器中，将石英反应器固定于微波辐射反应炉内，无载气通入，打开电源开关，设定微波处理的相关工艺参数，具体参数条件如下：Accurately weigh 50g of Shanxi high-sulfur coal in a 200ml quartz reactor, fix the quartz reactor in the microwave radiation reaction furnace, pass in no carrier gas, turn on the power switch, and set the relevant process parameters for microwave treatment. The specific parameter conditions are as follows :
微波辐射频率2.45GHz，微波功率800W，微波照射时间8min，辐射温度190℃，煤层厚度3cm(占石英反应器总体积的3/5)，煤粒径3cm(原煤未粉碎)。The microwave radiation frequency is 2.45GHz, the microwave power is 800W, the microwave irradiation time is 8min, the radiation temperature is 190°C, the coal seam thickness is 3cm (accounting for 3/5 of the total volume of the quartz reactor), and the coal particle size is 3cm (the raw coal is not pulverized).
打开微波辐射反应炉开关(即启动微波辐射)进行微波辐射脱硫，反应结束后，冷却至室温，收集微波处理后的煤炭在德国FLASH-2000型有机元素分析仪上进行元素分析，元素分析时以氦气为载气，炉温设置为950℃。由元素分析可知：微波辐射后煤炭的硫含量为2.05％，脱硫率为50.19％。Turn on the microwave radiation reaction furnace switch (i.e. start microwave radiation) to carry out microwave radiation desulfurization. After the reaction is over, cool to room temperature, collect the microwave-treated coal and carry out element analysis on the German FLASH-2000 organic element analyzer. Helium was used as the carrier gas, and the furnace temperature was set at 950 °C. According to elemental analysis, the sulfur content of coal after microwave radiation is 2.05%, and the desulfurization rate is 50.19%.
另外，通过红外、热失重、X射线衍射仪及扫描电镜分析可知，山西慈林山高硫煤炭经微波辐射处理，除脱硫外，煤样的内在结构特性、结晶度、稳定性、发热量等保持稳定。In addition, through infrared, thermogravimetric, X-ray diffractometer and scanning electron microscope analysis, it can be seen that the high-sulfur coal in Cilin Mountain, Shanxi Province is treated with microwave radiation. In addition to desulfurization, the internal structural characteristics, crystallinity, stability, and calorific value of the coal sample remain stable. .
由上述可知，微波辐射高硫煤炭脱硫可以脱出煤炭中的无机硫和有机硫，脱硫率在50％左右，而且脱硫前后煤炭的性能指标保持稳定且损失率极低，本发明能耗低、易于控制且可实现连续化生产，可用于高硫煤炭的脱硫提质。As can be seen from the above, the desulfurization of high-sulfur coal by microwave radiation can remove the inorganic sulfur and organic sulfur in the coal, the desulfurization rate is about 50%, and the performance index of the coal before and after desulfurization remains stable and the loss rate is extremely low. The present invention has low energy consumption and is easy to use. It can control and realize continuous production, and can be used for desulfurization and upgrading of high-sulfur coal.
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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 |
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| 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 |
| CN117018531A (en) * | 2023-08-12 | 2023-11-10 | 福州大学 | Method for inhibiting spontaneous combustion of sulfide ores based on microwave heating rate |
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