CN102199434A - Method for quick pyrolysis of coal direct liquefaction residues by utilizing microwaves - Google Patents
Method for quick pyrolysis of coal direct liquefaction residues by utilizing microwaves Download PDFInfo
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Abstract
The invention relates to a method for the quick pyrolysis of coal direct liquefaction residues by utilizing microwaves, which comprises the following steps of: heating the coal direct liquefaction residues to the temperature of between 500 and 900 DEG C by utilizing the microwaves as a heating heat source; crushing the coal direct liquefaction residues to less than 30 millimeters, and putting into drying equipment for drying; and putting the dried coal direct liquefaction residues into a microwave pyrolysis reactor, heating to the temperature of between 500 and 900 DEG C to obtain solid coke and pyrolysis gas, and cooling to separate liquid oil from gas. The method is mainly used for recycling the coal direct liquefaction residues comprehensively, and hydrogen-rich gas is obtained while the liquid oil is separated quickly and efficiently, so the method has characteristics of high pyrolysis speed, production efficiency, yield of the liquid oil and hydrogen content in the gas.
Description
Technical field
The invention belongs to the coal pyrolysis technical field, relate to a kind of coal directly-liquefied residue pyrolytic method, be specifically related to a kind of method of utilizing microwave fast pyrogenation coal directly-liquefied residue.
Background technology
The characteristics of China's energy structure are " many coals, few oil, deficencys ", along with the raising of rapid development of economy and living standards of the people, to the demand of the energy particularly the demand of oil entered rapid growth period.Because a large amount of Imported oils, not only increased degree of dependence to the external energy, and the fluctuation of international petroleum market and change and can directly influence the economy of China and the safety of power supply.China has the abundant in coal resource, makes full use of the coal resources of China's abundant, and developing Direct liquefaction technology energetically is one of effective way that solves oil shortage, has important strategic and economic implications.
In the DCL/Direct coal liquefaction process,, all can produce the liquefied residue that accounts for about 30% no matter adopt which kind of liquefaction process and solid-liquid separation technique.Liquefied residue is a kind of high-sulfur, high ash and high-carbon material, unconverted coal organic substance, mineral substance and catalyzer in the liquefaction raw coal, the main body of formation coal liquefaction residue.The content of liquefied residue with form along with the organic structure of different liquefaction process and coal is formed and inorganic mineral composition different and different, in the liquefied residue, generally contain elements such as C, H, O, N, S, the content of C element is up to 70%-85%.The classical group of underpressure distillation residue becomes: mink cell focus 30%, asphaltene 20%, preceding asphaltene 5% and tetrahydrofuran insoluble (unreacted coal and mineral substance) 45%, wherein unreacted coal accounts for about 30%.Therefore, from improving DCL/Direct coal liquefaction process economy and comprehensive utilization of resources and point of view of environment protection, realize that fast, efficiently utilizing of coal directly-liquefied residue is very necessary.
At present, one of the approach that utilizes of liquefied residue is that coal liquefaction residue is used for gasification hydrogen-producing, both for the gelatin liquefaction process provides the part hydrogen source, can be depleted to whole liquefied residues again, realizes the organic coupling that residue comprehensive utilization and gelatin liquefaction are produced.Though adopting liquefied residue gasification hydrogen-producing technology is a kind of effective way that solves the residue comprehensive utilization, but people also are in the starting stage to the understanding of liquefied residue, and the formation condition of liquefied residue, the enrichment of catalyzer and inorganic mineral content still await further research to the influence of gasification etc. and explores.In China, though gelatin liquefaction company of group of Shenhua has finished the research work in early stage of residue gasification hydrogen-producing, and selected Texaco and Shell gasifying process to carry out the liquefied residue gasification respectively and attempted, but do not find a complete feasible suitability for industrialized production route so far as yet.
In addition, generally contain have an appointment 30% mink cell focus and about 25% asphaltene and preceding asphaltene in the liquefied residue, therefore, at first just become another kind and utilize approach economically and reasonably by the comprehensive refiltered oil series products of pyrolysis.The pyrolysis of liquefied residue is meant heats residue under the condition of secluding air or inert atmosphere, the complex process of a series of physical changes and chemical reaction takes place under different temperature.The pyrolysis of residue is the same with the pyrolysis of coal, be in the trans-utilization processes such as liquefaction, gasification at first and must through reactions steps, it almost occurs in all liquefied residue trans-utilization processes, utilizes process that very big influence is arranged to the subsequent conversion of residue.The pyrolysis of liquefied residue can make the asphaltene in the residue be converted into mink cell focus and retortable oil to greatest extent, has increased the liquid product yield of coal liquefaction craft.When liquefied residue and coal carried out mixed pyrolysis, liquefied residue can produce the hydrogen supply effect, can take place simultaneously to interact significantly, and this distribution to product has very big influence.
Microwave heating is a kind of novel heating technique, has that rate of heating is fast, characteristics of homogeneous heating, efficient energy-saving.In order to prevent that microwave power from causing interference to radio communication, broadcasting, TV and radar etc., general provision 915MHz and 2450MHz are civilian microwave frequency band in the world.Traditional type of heating is first heating object surface, and to internal delivery, and microwave heating is directly object integral body to be heated to heat, can strengthen to improve heat-transfer effect by body surface then, reduces the heat transfer loss of pyrolytic process.At present, microwave heating be widely used in that food-processing, medicine are produced, chemical industry is synthetic, agricultural byproducts are dry, fields such as the drying of mineral processing, disinfection and coal and biomass etc., desulfurization, pyrolysis.
Present technique is applied to microwave heating in the pyrolysis of liquefied residue, has great importance for improving pyrolysis efficient and oils product yield.
Summary of the invention
In order to overcome above-mentioned the deficiencies in the prior art, the object of the present invention is to provide a kind of method of utilizing microwave fast pyrogenation coal directly-liquefied residue, this method is mainly used in the comprehensive recovery and the utilization of coal directly-liquefied residue, rapidly and efficiently obtaining hydrogen-rich gas in the separating oil series products, have that pyrolysis rate is fast, production efficiency is high, liquid oils yield height, the high characteristics of hydrogen richness in the coal gas.
To achieve these goals, the technical solution used in the present invention is:
A kind of method of utilizing microwave fast pyrogenation coal directly-liquefied residue utilizes microwave as the heating thermal source, and coal directly-liquefied residue is heated to 500 ℃～900 ℃.
Specifically may further comprise the steps:
The first step utilizes grinding attachment that coal directly-liquefied residue is crushed to below the particle diameter 30mm;
In second step, the coal directly-liquefied residue after pulverizing is placed dry 30 ± 10min under 100 ℃ of conditions of drying plant;
The 3rd step placed the microwave-heating reactor with the coal directly-liquefied residue after pulverizing, and power-on is heated to 500 ℃～900 ℃, and the residence time 10 ± 5min obtains the burnt and pyrolysis gas of solid;
In the 4th step, solid Jiao collect after water-cooling system is cooled to normal temperature, and pyrolysis gas is collected respectively after the two-stage cooling system is isolated the liquid oil and gas.
Described two-stage cooling system refers to the cold air system and the partial liquid phase condensate system of the first step.
Described heating is the 915MHz of national regulation and the civilian microwave frequency band of 2450MHz with the frequency of microwave.
Compared with prior art, method of the present invention is to utilize the basic fine structure coupling of special wave band that microwave has and material to produce heat to heat, the intensification of liquefied residue is not by heat transfer but finishes by outfield and object interaction, it is fast that it has the heating rate degree, selectivity is good, material is heated evenly, capable of fast starting and stop, easy to operate, characteristics such as energy utilization rate and heating efficiency height.In addition, the volatile matter in the residue can obtain sufficient pyrolysis, oils product yield height; Simultaneously can obtain superior in quality solid Jiao and hydrogen-rich gas, help the comprehensive utilization of resource.
Description of drawings
Accompanying drawing is a process flow sheet of the present invention;
Embodiment
Below in conjunction with drawings and Examples the present invention is described in further details.
Embodiment one
As shown in Figure 1, utilize the method for microwave fast pyrogenation coal directly-liquefied residue, it is characterized in that, may further comprise the steps:
The first step utilizes grinding attachment that coal directly-liquefied residue is crushed to particle diameter 30mm;
In second step, the coal directly-liquefied residue after pulverizing is placed dry 20min under 100 ℃ of conditions of drying plant;
The 3rd step placed the microwave-heating reactor with dried coal directly-liquefied residue, power-on, and setting heating is 2450MHz with microwave frequency, is heated to 900 ℃, residence time 15min obtains solid Jiao and pyrolysis gas;
In the 4th step, solid Jiao collect after water-cooling system is cooled to normal temperature, and pyrolysis gas is through main air cooling system and secondary liquid phase condensate system, collects respectively after isolating the liquid oil and gas.
Embodiment two
As shown in Figure 1, utilize the method for microwave fast pyrogenation coal directly-liquefied residue, it is characterized in that, may further comprise the steps:
The first step utilizes grinding attachment that coal directly-liquefied residue is crushed to particle diameter 10mm;
In second step, the coal directly-liquefied residue after pulverizing is placed dry 30min under 100 ℃ of conditions of drying plant;
The 3rd step placed the microwave-heating reactor with dried coal directly-liquefied residue, power-on, and setting heating is 2450MHz with microwave frequency, is heated to 800 ℃, residence time 10min obtains the burnt and pyrolysis gas of solid;
In the 4th step, solid Jiao collect after water-cooling system is cooled to normal temperature, and pyrolysis gas is through main air cooling system and secondary liquid phase condensate system, and sub-argument is collected respectively after going out the liquid oil and gas.
Embodiment three
As shown in Figure 1, utilize the method for microwave fast pyrogenation coal directly-liquefied residue, it is characterized in that, may further comprise the steps:
The first step utilizes grinding attachment that coal directly-liquefied residue is crushed to particle diameter 5mm;
In second step, the coal directly-liquefied residue after pulverizing is placed dry 40min under 100 ℃ of conditions of drying plant;
The 3rd step placed the microwave-heating reactor with dried coal directly-liquefied residue, power-on, and setting heating is 915MHz with microwave frequency, is heated to 500 ℃, residence time 5min obtains the burnt and pyrolysis gas of solid;
In the 4th step, solid Jiao collect after water-cooling system is cooled to normal temperature, and pyrolysis gas is through main air cooling system and secondary liquid phase condensate system, and sub-argument is collected respectively after going out the liquid oil and gas.
Embodiment four
In the present embodiment, the coal directly-liquefied residue composition analysis is as shown in table 1.
Table 1
Pyrolytic process is as follows:
The first step utilizes grinding attachment that coal directly-liquefied residue is crushed to particle diameter 5～10mm;
In second step, the coal directly-liquefied residue after pulverizing is placed dry 30min under 100 ℃ of conditions of loft drier;
The 3rd step placed the microwave-heating reactor with dried coal directly-liquefied residue, power-on, and setting heating is 2450MHz with microwave frequency, heating stops 15min between 500 ℃～900 ℃, obtain solid Jiao and pyrolysis gas;
In the 4th step, solid Jiao collect after water-cooling system is cooled to normal temperature, and pyrolysis gas is through main air cooling system and secondary liquid phase condensate system, collects respectively after isolating the liquid oil and gas.
The analytical results of coal gas is as shown in table 2 after the pyrolysis,
| H 2 | CO 2 | CO | CH 4 | |
| Sample 1 | 60.27 | 5.68 | 4.52 | 29.01 |
| Sample 2 | 61.79 | 4.18 | 5.04 | 28.52 |
| Mean value | 61.03 | 4.93 | 4.78 | 28.77 |
Table 2
Experimental result shows that the liquid oils rate of recovery can reach about 25%, and hydrogen content is about 60% in the pyrolysis coal gas.
Among the present invention, the all non-limitation of the present invention of the selection of the grain size after the pulverizing, the parameter area of drying plant and microwave heating temperature scope and time, such selection is for no other reason than that consider when guaranteeing to reach best effect and will save cost, as, grain size after the pulverizing is lower than 500 ℃ greater than the temperature of 30mm or heating, the pyrolytic final purpose still can realize, still can make that like this reaction times is long, and be unfavorable for Artificial Control.
Claims (7)
1. a method of utilizing microwave fast pyrogenation coal directly-liquefied residue is characterized in that, utilizes microwave as the heating thermal source, and coal directly-liquefied residue is heated to 500 ℃～900 ℃.
2. the method for utilizing microwave fast pyrogenation coal directly-liquefied residue according to claim 1 is characterized in that, may further comprise the steps:
The first step utilizes grinding attachment that coal directly-liquefied residue is crushed to below the particle diameter 30mm;
In second step, the coal directly-liquefied residue after pulverizing is placed dry 30 ± 10min under 100 ℃ of conditions of drying plant;
The 3rd step placed the microwave-heating reactor with dried coal directly-liquefied residue, and power-on is heated to 500 ℃～900 ℃, and the residence time 10 ± 5min obtains the burnt and pyrolysis gas of solid;
In the 4th step, solid Jiao is cooled to normal temperature through water-cooling system, and pyrolysis gas is collected respectively after isolating the liquid oil and gas behind the two-stage cooling system.
3. the method for utilizing microwave fast pyrogenation coal directly-liquefied residue according to claim 1 is characterized in that, may further comprise the steps:
The first step utilizes grinding attachment that coal directly-liquefied residue is crushed to particle diameter 30mm;
In second step, the coal directly-liquefied residue after pulverizing is placed dry 20min under 100 ℃ of conditions of drying plant;
The 3rd step placed the microwave-heating reactor with dried coal directly-liquefied residue, and power-on is heated to 900 ℃, and residence time 15min obtains the burnt and pyrolysis gas of solid;
In the 4th step, solid Jiao is cooled to normal temperature through water-cooling system, and pyrolysis gas is collected respectively after isolating the liquid oil and gas behind the two-stage cooling system.
4. the method for utilizing microwave fast pyrogenation coal directly-liquefied residue according to claim 1 is characterized in that, may further comprise the steps:
The first step utilizes grinding attachment that coal directly-liquefied residue is crushed to particle diameter 10mm;
In second step, the coal directly-liquefied residue after pulverizing is placed dry 30min under 100 ℃ of conditions of drying plant;
The 3rd step placed the microwave-heating reactor with dried coal directly-liquefied residue, and power-on is heated to 800 ℃, and residence time 10min obtains the burnt and pyrolysis gas of solid;
In the 4th step, solid Jiao is cooled to normal temperature through water-cooling system, and pyrolysis gas is collected respectively after isolating the liquid oil and gas behind the two-stage cooling system.
5. the method for utilizing microwave fast pyrogenation coal directly-liquefied residue according to claim 1 is characterized in that, may further comprise the steps:
The first step utilizes grinding attachment that coal directly-liquefied residue is crushed to particle diameter 5mm;
In second step, the coal directly-liquefied residue after pulverizing is placed dry 40min under 100 ℃ of conditions of drying plant;
The 3rd step placed the microwave-heating reactor with the coal directly-liquefied residue after pulverizing, and power-on is heated to 500 ℃, and residence time 5min obtains the burnt and pyrolysis gas of solid;
In the 4th step, solid Jiao is cooled to normal temperature through water-cooling system, and pyrolysis gas is collected respectively after isolating the liquid oil and gas behind the two-stage cooling system.
6. according to the described method of utilizing microwave fast pyrogenation coal directly-liquefied residue of the arbitrary claim of claim 2 to 5, it is characterized in that described two-stage cooling system refers to the cold air system and the partial liquid phase condensate system of the first step.
7. according to the described method of utilizing microwave fast pyrogenation coal directly-liquefied residue of the arbitrary claim of claim 1 to 5, it is characterized in that described heating is the 915MHz of national regulation and the civilian microwave frequency band of 2450MHz with the frequency of microwave.
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| CN102653683A (en) * | 2012-01-26 | 2012-09-05 | 何巨堂 | Internal heating type coal carbonization gas production process based on pressurization method |
| CN102718383A (en) * | 2012-06-06 | 2012-10-10 | 上海中科高等研究院 | Pyrolysis device and method for in-situ conversion of carbon-containing resources by microwave-assisted pyrolysis |
| CN102942976A (en) * | 2012-10-19 | 2013-02-27 | 西安建筑科技大学 | Method for preparing formed coke with low metamorphic coal as main raw material in microwave field |
| CN103160325A (en) * | 2011-12-14 | 2013-06-19 | 上海麦风微波设备有限公司 | Technological method for direct production of coal gas by microwaves and device |
| CN103788975A (en) * | 2014-01-22 | 2014-05-14 | 中国科学院上海高等研究院 | Method for microwave pyrolysis utilization of lignite |
| CN104073275A (en) * | 2013-03-29 | 2014-10-01 | 广州市昊晟工程勘察设计有限公司 | Mild-reaction oil residue separation method for coal-based residual oil |
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| CN103160325B (en) * | 2011-12-14 | 2016-12-14 | 上海麦风微波设备有限公司 | The microwave of a kind of coal gas is directly produced process and device |
| US9598646B2 (en) | 2013-01-09 | 2017-03-21 | C20 Technologies, Llc | Process for treating coal to improve recovery of condensable coal derived liquids |
| CN108106460A (en) * | 2016-11-24 | 2018-06-01 | 神华集团有限责任公司 | The cooling system and method for a kind of coal directly-liquefied residue |
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| CN102653683A (en) * | 2012-01-26 | 2012-09-05 | 何巨堂 | Internal heating type coal carbonization gas production process based on pressurization method |
| CN102718383A (en) * | 2012-06-06 | 2012-10-10 | 上海中科高等研究院 | Pyrolysis device and method for in-situ conversion of carbon-containing resources by microwave-assisted pyrolysis |
| CN102718383B (en) * | 2012-06-06 | 2017-03-08 | 中国科学院上海高等研究院 | Convert pyrolysis installation and the method containing carbon resource using microwave-assisted pyrolysis on the spot |
| CN102942976A (en) * | 2012-10-19 | 2013-02-27 | 西安建筑科技大学 | Method for preparing formed coke with low metamorphic coal as main raw material in microwave field |
| US9598646B2 (en) | 2013-01-09 | 2017-03-21 | C20 Technologies, Llc | Process for treating coal to improve recovery of condensable coal derived liquids |
| CN104955921B (en) * | 2013-01-09 | 2017-09-15 | C2O技术发展公司 | Handle method of the coal to improve the recovery of condensable coal derived liquid |
| CN104073275A (en) * | 2013-03-29 | 2014-10-01 | 广州市昊晟工程勘察设计有限公司 | Mild-reaction oil residue separation method for coal-based residual oil |
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| CN105377794A (en) * | 2013-05-23 | 2016-03-02 | 埃克赛乐公司 | Producing fuels and biofertilizers from biomass |
| CN103788975A (en) * | 2014-01-22 | 2014-05-14 | 中国科学院上海高等研究院 | Method for microwave pyrolysis utilization of lignite |
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