CN115106038A - Utilize infrared rapid heating's broken coal pyrolysis experiment platform - Google Patents
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- 238000000197 pyrolysis Methods 0.000 title claims abstract description 74
- 239000003245 coal Substances 0.000 title claims abstract description 66
- 238000010438 heat treatment Methods 0.000 title claims abstract description 63
- 238000002474 experimental method Methods 0.000 title claims abstract description 13
- 239000007789 gas Substances 0.000 claims abstract description 53
- 239000007788 liquid Substances 0.000 claims abstract description 39
- 238000000926 separation method Methods 0.000 claims abstract description 28
- 238000006243 chemical reaction Methods 0.000 claims abstract description 22
- 238000009826 distribution Methods 0.000 claims abstract description 19
- 239000012159 carrier gas Substances 0.000 claims abstract description 12
- 238000000034 method Methods 0.000 claims abstract description 11
- 238000001514 detection method Methods 0.000 claims abstract description 6
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 29
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 10
- 239000011148 porous material Substances 0.000 claims description 6
- 238000005033 Fourier transform infrared spectroscopy Methods 0.000 claims description 5
- 239000000203 mixture Substances 0.000 claims description 5
- 229910052757 nitrogen Inorganic materials 0.000 claims description 5
- 238000012544 monitoring process Methods 0.000 claims description 3
- 239000005457 ice water Substances 0.000 claims description 2
- 239000002245 particle Substances 0.000 abstract description 7
- 230000009286 beneficial effect Effects 0.000 abstract description 3
- 238000010517 secondary reaction Methods 0.000 abstract 1
- 230000006872 improvement Effects 0.000 description 4
- 238000005259 measurement Methods 0.000 description 4
- 238000001035 drying Methods 0.000 description 3
- 230000008569 process Effects 0.000 description 3
- 238000011160 research Methods 0.000 description 3
- 239000000571 coke Substances 0.000 description 2
- 238000011161 development Methods 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 238000010926 purge Methods 0.000 description 2
- 238000012546 transfer Methods 0.000 description 2
- 239000004215 Carbon black (E152) Substances 0.000 description 1
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 1
- 230000004075 alteration Effects 0.000 description 1
- 238000001816 cooling Methods 0.000 description 1
- 230000008878 coupling Effects 0.000 description 1
- 238000010168 coupling process Methods 0.000 description 1
- 238000005859 coupling reaction Methods 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 229930195733 hydrocarbon Natural products 0.000 description 1
- 150000002430 hydrocarbons Chemical class 0.000 description 1
- 239000001257 hydrogen Substances 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 230000000149 penetrating effect Effects 0.000 description 1
- 229920001296 polysiloxane Polymers 0.000 description 1
- 230000001737 promoting effect Effects 0.000 description 1
- 238000004445 quantitative analysis Methods 0.000 description 1
- 238000011897 real-time detection Methods 0.000 description 1
- 238000007789 sealing Methods 0.000 description 1
- 239000000377 silicon dioxide Substances 0.000 description 1
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J19/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
- B01J19/08—Processes employing the direct application of electric or wave energy, or particle radiation; Apparatus therefor
- B01J19/12—Processes employing the direct application of electric or wave energy, or particle radiation; Apparatus therefor employing electromagnetic waves
- B01J19/122—Incoherent waves
- B01J19/128—Infrared light
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J6/00—Heat treatments such as Calcining; Fusing ; Pyrolysis
- B01J6/008—Pyrolysis reactions
-
- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10B—DESTRUCTIVE DISTILLATION OF CARBONACEOUS MATERIALS FOR PRODUCTION OF GAS, COKE, TAR, OR SIMILAR MATERIALS
- C10B53/00—Destructive distillation, specially adapted for particular solid raw materials or solid raw materials in special form
- C10B53/04—Destructive distillation, specially adapted for particular solid raw materials or solid raw materials in special form of powdered coal
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- Oil, Petroleum & Natural Gas (AREA)
- Chemical Kinetics & Catalysis (AREA)
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- General Health & Medical Sciences (AREA)
- Toxicology (AREA)
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Abstract
The invention discloses a crushed coal pyrolysis experiment platform utilizing infrared rapid heating, which comprises a gas distribution and supply system, a pyrolysis reaction system, a gas-liquid separation system and a gas collection/detection system, wherein the gas distribution and supply system is connected with the gas distribution and supply system; the gas distribution and supply system is used for introducing pyrolysis atmosphere carrier gas into the pyrolysis reaction system; the pyrolysis reaction system is used for carrying out coal pyrolysis; the gas-liquid separation system performs gas-liquid separation on the product of the pyrolysis reaction system after the coal is pyrolyzed; the gas collecting/detecting system is used for collecting/detecting gas-phase products after gas-liquid separation of the gas-liquid separating system. The invention designs a pyrolysis experiment platform and a method for researching crushed coal under different working conditions such as different particle sizes, heating rates, atmospheres and the like by using an infrared rapid heating furnace. Compare in traditional pyrolysis experiment, this experiment platform adopts infrared heating's mode, has advantages such as the heating is fast, the penetrability is strong, temperature gradient is little. Meanwhile, the invention can well reduce secondary reaction and is beneficial to improving the yield and quality of tar.
Description
Technical Field
The invention belongs to the field of efficient clean coal receiving, and particularly relates to a crushed coal pyrolysis experiment platform utilizing infrared rapid heating.
Background
The pyrolysis of coal is affected by the coupling of various factors, such as coal particle size, pyrolysis atmosphere, rate of temperature rise, pyrolysis temperature, and the like. The heat transfer is an important factor influencing the pyrolysis reaction of the low-rank coal, the pyrolysis process of the coal is controlled after the heat is transferred from the outside to the inside of the coal and reaches the threshold value, and the size of coal particles and the temperature rise rate are also important for influencing the heat transfer process. The traditional pyrolysis experiment table mainly comprises TGA and a fixed bed, basically adopts an electric furnace as a heating mode, has large hysteresis and has the disadvantages of causing overlarge temperature gradient when being researched for crushed coal. The infrared heating adopted by the invention has certain penetrating performance and can well reduce the temperature gradient, and meanwhile, the linear temperature rise at any temperature rise rate of less than 50 ℃/s can be realized through PID control.
Although the previous experimental platform can meet basic experimental research, the temperature rise rate cannot reach a higher interval, only trace samples (mg level) can be processed, the generally obtained product distribution accuracy is low, and the method is applied to comprehensive multi-parameter quantitative analysis of the pyrolysis products of the crushed coal, especially pyrolysis product information in the hydrogen atmosphere. Therefore, the experiment platform for pyrolysis of crushed coal by utilizing infrared rapid heating can comprehensively solve the problems and develop research on pyrolysis characteristics of crushed coal under the influence of related multiple factors. In the industry, the method is beneficial to promoting the development and application of the Huifu furnace, and can provide certain constructive significance for the Huifu furnace.
Disclosure of Invention
The invention designs a crushed coal pyrolysis experimental platform utilizing infrared rapid heating, in particular to a device which can research the influence of multiple factors such as coal particle size, heating rate, pyrolysis final temperature, pyrolysis atmosphere and the like on the pyrolysis characteristics of crushed coal and even pulverized coal and can qualitatively and quantitatively analyze pyrolysis products. The problems that the temperature rise rate of a traditional pyrolysis experiment platform cannot reach a high range, only trace samples can be processed, the accuracy of product acquisition is low and the like are solved.
The invention is realized by adopting the following technical scheme:
a crushed coal pyrolysis experiment platform utilizing infrared rapid heating comprises a gas distribution and supply system, a pyrolysis reaction system, a gas-liquid separation system and a gas collection/detection system;
the gas distribution and supply system is used for introducing pyrolysis atmosphere carrier gas into the pyrolysis reaction system;
the pyrolysis reaction system is used for carrying out coal pyrolysis; the gas-liquid separation system performs gas-liquid separation on the product of the pyrolysis reaction system after the coal is pyrolyzed;
the gas collecting/detecting system is used for collecting/detecting gas-phase products after gas-liquid separation of the gas-liquid separating system.
The invention has the further improvement that the gas distribution and supply system comprises high-pressure gas cylinders, the inlet and outlet of each high-pressure gas cylinder are provided with a pressure reducing valve and a high-precision mass flowmeter, and a plurality of high-pressure gas cylinders can distribute carrier gas in various pyrolysis atmospheres.
The invention has the further improvement that the pyrolysis reaction system comprises a quartz glass reactor, a thermocouple for measuring the central temperature of the coal sample, an infrared heating furnace body, a special orifice plate, an infrared heating lamp tube and a thermocouple for measuring the temperature of a hearth; the gas inlet of the quartz glass reactor is connected with a gas distribution and supply system, the quartz glass reactor is arranged in the infrared heating furnace body, the infrared heating lamp tube is arranged in the infrared heating furnace body and used for heating the quartz glass reactor, the special pore plate is arranged in the quartz glass reactor, the thermocouple for measuring the central temperature of the coal sample is used for measuring the temperature in the quartz glass reactor, and the thermocouple for measuring the hearth temperature is used for measuring the temperature between the infrared heating lamp tube and the quartz glass reactor.
The invention has the further improvement that the infrared heating lamp tube adopts an infrared heating mode, and can realize linear temperature rise at different temperature rise rates.
The invention is further improved in that the heating rate of the infrared heating lamp tube is 50 ℃/s fastest.
A further development of the invention is that the quartz glass reactor is a custom-made quartz glass tube.
The invention is further improved in that a cold source of the gas-liquid separation system is liquid nitrogen.
The invention is further improved in that the cold source of the gas-liquid separation system is an ice-water mixture.
The invention is further improved in that the method comprises the following steps in operation:
1) crushing a coal sample until the granularity is uniform, and placing the coal sample on a special pore plate in a quartz glass reactor;
2) continuously introducing carrier gas into the pyrolysis reaction system through a gas distribution and supply system;
3) the infrared heating lamp tube rapidly heats the coal sample in the quartz glass reactor according to a set heating rate, and gas and tar generated by pyrolysis vertically flow into a gas-liquid separation system for gas-liquid separation treatment;
4) the separated gas is collected by an air bag and then detected in a GC or the gas is directly introduced into a FTIR for on-line monitoring.
The invention has at least the following beneficial technical effects:
1. by utilizing the heating mode of the infrared ray with high energy characteristic, the coal sample can be rapidly heated, and the coal sample has small temperature gradient and is uniformly heated.
2. A maximum of 30mm of macro-crushed coal samples can be studied.
3. The influence of multiple factors such as coal particle size, heating rate and atmosphere on the coal pyrolysis characteristic can be comprehensively researched.
4. The pyrolysis product can be qualitatively and quantitatively analyzed, and the information of the pyrolysis product can be more accurately acquired.
Drawings
FIG. 1 is a schematic diagram of a process equipment connection of a crushed coal pyrolysis experimental platform utilizing infrared rapid heating;
FIG. 2 is a schematic illustration of a quartz glass reactor in a designed pyrolytic reaction system;
FIG. 3 is a schematic illustration of a U-tube in the gas-liquid separation system;
FIG. 4 is a top view of the reactor and U-tube connection.
FIG. 5 is a sectional view taken along A-A of the reactor and U-tube connection.
Description of reference numerals:
1. a gas distribution and supply system; 1-1, a high-pressure gas cylinder; 1-2 pressure reducing valves; 1-3, high-precision mass flowmeter; 2. A pyrolysis reaction system; 2-1, a quartz glass reactor; 2-2, measuring the central temperature of the coal sample by a thermocouple; 2-3, an infrared heating furnace body; 2-4, specially manufacturing a pore plate; 2-5, heating a lamp tube by infrared rays; 2-6, measuring the temperature of the hearth by a thermocouple; 3. a gas-liquid separation system; 3-1, liquid nitrogen cup; 3-2, U-shaped pipes; 4. a gas collection/detection instrument; 5-1, a support member; 5-2, reactor inlet; 5-3, atmosphere carrier gas inlet; 5-4, a reactor outlet; 6-1, a U-shaped pipe inlet; 6-2, gas outlet; 7. a reactor and a U-shaped pipe connector; 7-1, U-shaped pipe end; 7-2 and a reactor end.
Detailed Description
The present invention will be described in detail below with reference to the accompanying drawings and examples.
The invention discloses a structural composition and a using method of the invention by taking a crushed coal pyrolysis experimental platform utilizing infrared rapid heating as an example.
As shown in the attached drawings 1-3, the invention designs a crushed coal pyrolysis experimental platform utilizing infrared rapid heating, which comprises a gas distribution and supply system, a pyrolysis reaction system, a gas-liquid separation system and a gas collection/detection system. The gas distribution and supply system mainly comprises a high-pressure gas cylinder 1-1, a pressure reducing valve 1-2 and a high-precision mass flowmeter 1-3. The pyrolysis reaction system mainly comprises a quartz glass reactor 2-1, a thermocouple 2-2 for measuring the central temperature of a coal sample, an infrared heating furnace body 2-3, a special orifice plate 2-4, an infrared heating lamp tube 2-5 and a thermocouple 2-6 for measuring the temperature of a hearth; the quartz glass reactor is shown in figure 2, a special orifice plate 2-4 is a placing plate with a small hole of a specific specification sintered in the reactor, a support member 5-1 is used for supporting the reactor to enable the reactor to be vertically arranged in an infrared heating furnace, a sample is placed in the reactor from an inlet 5-2, carrier gas is introduced from an atmosphere carrier gas inlet 5-3, and a generated gas-liquid mixture is taken out from an outlet 5-4 of the reactor by the carrier gas. The gas-liquid separation system mainly comprises a liquid nitrogen cup 3-1 and a U-shaped pipe 3-2, and liquid is separated by cooling a gas-liquid mixture by using liquid nitrogen. The quartz glass reactor and the U-shaped tube are connected by the reactor and U-shaped tube connecting piece 7 shown in FIG. 4 and FIG. 5, the reactor outlet 5-4 is connected to the reactor end 7-2, the U-shaped tube inlet 6-1 at one end of the U-shaped tube 3-2 is connected to the U-shaped tube end 7-1, and the other end of the U-shaped tube 3-2 is provided with the gas outlet 6-2. The gas collection/detection instrument 4 can perform both on-line and off-line measurements. Wherein, off-line measurement needs gas bag collection, and gas in the experiment is collected and measured by GC; the on-line measurement is carried out by introducing the separated gas into a gas cell of FTIR (Fourier infrared hydrocarbon detector) for real-time measurement.
The invention relates to an application of a crushed coal pyrolysis experimental platform by utilizing infrared rapid heating, which comprises the following steps:
1) crushing a coal sample until the granularity is uniform, and placing the coal sample on a pore plate in a pyrolysis reactor;
2) continuously introducing carrier gas into the pyrolysis reaction system through a gas distribution and supply system;
3) the infrared heating pipe rapidly heats the coal sample according to a set heating rate, and gas and tar generated by pyrolysis vertically flow into a gas-liquid separation system for gas-liquid separation treatment;
4) the separated gas is collected by an air bag and then detected in a GC or the gas is directly introduced into a FTIR for on-line monitoring.
Example 1
In this example, the gaseous product was measured off-line by pyrolyzing crushed coal having a particle size of 20mm using an infrared rapid heating pyrolysis experimental platform by first grinding raw coal into a nearly spherical body having a diameter of 20mm, then drying the same in a drying oven at 105 ℃ for 8 hours and placing the same in a perforated plate and then sealing the inlet of the reactor with a silica plug. After purging with 250ml/min N2 through a pressure reducing valve and a mass flow meter for 5min, the coal sample was warmed from room temperature to 1000 ℃ at a temperature ramp rate of 100K/min and pyrolyzed for 10 min. And collecting gas of the pyrolysis product after passing through the gas-liquid separation system by using a gas bag. The semi-coke and tar treatment techniques can be treated according to the prior art.
Example 2
In this example, a coal sample is first crushed into 3-5mm uniform coal particles, then dried in a drying oven at 105 ℃ for 8h and placed on a perforated plate, and then the inlet of the reactor is sealed with a silicone plug. After purging with 250ml/min N2 through a pressure reducing valve and a mass flow meter for 5min, the coal sample was warmed from room temperature to 1000 ℃ at a ramp rate of 500K/min and pyrolyzed for 10 min. And directly introducing gas of the pyrolysis product after passing through a gas-liquid separation system into a gas pool of FTIR for real-time detection. The semi-coke and tar treatment techniques can be treated according to the prior art.
Although the invention has been described in detail with respect to the general description and the specific embodiments thereof, it will be apparent to those skilled in the art that modifications and improvements can be made based on the invention. Accordingly, it is intended that all such modifications and alterations be included within the scope of this invention as defined in the appended claims.
Claims (9)
1. A crushed coal pyrolysis experiment platform utilizing infrared rapid heating is characterized by comprising a gas distribution and supply system (1), a pyrolysis reaction system (2), a gas-liquid separation system (3) and a gas collection/detection system;
the gas distribution and supply system (1) is used for introducing pyrolysis atmosphere carrier gas into the pyrolysis reaction system (2);
the pyrolysis reaction system (2) is used for carrying out coal pyrolysis; the gas-liquid separation system (3) is used for carrying out gas-liquid separation on the product of the pyrolysis reaction system (2) after the coal is pyrolyzed;
the gas collecting/detecting system is used for collecting/detecting gas-phase products after gas-liquid separation of the gas-liquid separating system (3).
2. The experimental platform for pyrolysis of crushed coal by using infrared rapid heating is characterized in that the gas distribution and supply system (1) comprises a high-pressure gas cylinder (1-1), a pressure reducing valve (1-2) and a high-precision mass flow meter (1-3) are arranged at an inlet and an outlet of the high-pressure gas cylinder (1-1), and a plurality of pyrolysis atmosphere carrier gases can be distributed from the high-pressure gas cylinders (1-1).
3. The experimental platform for pyrolysis of crushed coal by using infrared rapid heating as claimed in claim 1, wherein the pyrolysis reaction system (2) comprises a quartz glass reactor (2-1), a thermocouple (2-2) for measuring the central temperature of the coal sample, an infrared heating furnace body (2-3), a specially-made orifice plate (2-4), an infrared heating lamp tube (2-5) and a thermocouple (2-6) for measuring the temperature of a hearth; an air inlet of the quartz glass reactor (2-1) is connected with the air distribution and supply system (1), the quartz glass reactor (2-1) is arranged in the infrared heating furnace body (2-3), the infrared heating lamp tube (2-5) is arranged in the infrared heating furnace body (2-3) and used for heating the quartz glass reactor (2-1), the specially-made pore plate (2-4) is arranged in the quartz glass reactor (2-1), the thermocouple (2-2) for measuring the central temperature of the coal sample is used for measuring the temperature in the quartz glass reactor (2-1), and the thermocouple (2-6) for measuring the hearth temperature is used for measuring the temperature between the infrared heating lamp tube (2-5) and the quartz glass reactor (2-1).
4. The experimental platform for pyrolysis of crushed coal using infrared rapid heating as claimed in claim 3, wherein the infrared heating lamp (2-5) adopts an infrared heating method, which can realize linear temperature rise at different temperature rise rates.
5. The experimental platform for pyrolysis of crushed coal using infrared rapid heating as claimed in claim 4, wherein the heating rate of the infrared heating lamp tube (2-5) is 50 ℃/s fastest.
6. The experimental platform for pyrolysis of crushed coal using infrared rapid heating according to claim 3, characterized in that the quartz glass reactor (2-1) is a customized quartz glass tube.
7. The experimental platform for pyrolysis of crushed coal by using infrared rapid heating as claimed in claim 1, wherein the cold source of the gas-liquid separation system (3) is liquid nitrogen.
8. The experimental platform for pyrolysis of crushed coal by using infrared rapid heating as claimed in claim 1, wherein the cold source of the gas-liquid separation system (3) is an ice-water mixture.
9. The experimental platform for pyrolysis of crushed coal by using infrared rapid heating according to any one of claims 3 to 6, which is characterized by comprising the following steps in operation:
1) crushing a coal sample until the granularity is uniform, and placing the coal sample on a specially-made pore plate (2-4) in a quartz glass reactor (2-1);
2) continuously introducing carrier gas into the pyrolysis reaction system through a gas distribution and supply system;
3) the infrared heating lamp tube (2-5) rapidly heats the coal sample in the quartz glass reactor (2-1) according to a set heating rate, and gas and tar generated by pyrolysis vertically flow into the gas-liquid separation system (3) for gas-liquid separation treatment;
4) the separated gas is collected by an air bag and then detected in a GC or directly introduced into FTIR for on-line monitoring.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN115508518A (en) * | 2022-10-27 | 2022-12-23 | 清华大学深圳国际研究生院 | Full-visual multifunctional gas hydrate dynamics measurement system and method |
| CN117665041A (en) * | 2024-02-01 | 2024-03-08 | 中海石油气电集团有限责任公司 | Radio frequency heating oil-rich coal in-situ pyrolysis simulation test device and method |
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2022
- 2022-07-15 CN CN202210833560.XA patent/CN115106038A/en active Pending
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN115508518A (en) * | 2022-10-27 | 2022-12-23 | 清华大学深圳国际研究生院 | Full-visual multifunctional gas hydrate dynamics measurement system and method |
| CN115508518B (en) * | 2022-10-27 | 2023-03-28 | 清华大学深圳国际研究生院 | Full-visual multifunctional gas hydrate dynamics measurement system and method |
| CN117665041A (en) * | 2024-02-01 | 2024-03-08 | 中海石油气电集团有限责任公司 | Radio frequency heating oil-rich coal in-situ pyrolysis simulation test device and method |
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