CN112816361B - System and method for evaluating thermal conversion of organic matter-containing solid - Google Patents
System and method for evaluating thermal conversion of organic matter-containing solid Download PDFInfo
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- CN112816361B CN112816361B CN202110007712.6A CN202110007712A CN112816361B CN 112816361 B CN112816361 B CN 112816361B CN 202110007712 A CN202110007712 A CN 202110007712A CN 112816361 B CN112816361 B CN 112816361B
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- 238000005303 weighing Methods 0.000 claims abstract description 113
- 238000010438 heat treatment Methods 0.000 claims abstract description 107
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- 238000004868 gas analysis Methods 0.000 claims abstract description 42
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- 238000011156 evaluation Methods 0.000 claims abstract description 26
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- 239000007789 gas Substances 0.000 claims description 500
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- 238000002485 combustion reaction Methods 0.000 claims description 21
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- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N5/00—Analysing materials by weighing, e.g. weighing small particles separated from a gas or liquid
- G01N5/04—Analysing materials by weighing, e.g. weighing small particles separated from a gas or liquid by removing a component, e.g. by evaporation, and weighing the remainder
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N31/00—Investigating or analysing non-biological materials by the use of the chemical methods specified in the subgroup; Apparatus specially adapted for such methods
- G01N31/12—Investigating or analysing non-biological materials by the use of the chemical methods specified in the subgroup; Apparatus specially adapted for such methods using combustion
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Abstract
A system and a method for carrying out thermal conversion evaluation on solids containing organic substances are disclosed, wherein the system comprises a gas distribution unit, a gas heating unit, a weighing unit, a cooling unit and a gas analysis unit; each unit respectively includes in proper order: protection gas circuit and N arranged in parallel 2 Gas path, CO 2 Gas path, CH 4 Gas path H 2 The device comprises a gas path, an air path, a gas mixer, an emptying gas path and an analysis gas path; a heater; the device comprises a weighing structure and a heat conversion structure, wherein the weighing structure comprises a balance chamber, a weighing rod, a cooling water jacket, a first connector and a sample basket, the heat conversion structure comprises a tubular furnace, a furnace tube with the same central axis is arranged in the center of the tubular furnace, a second connector is arranged at the top end of the furnace tube, a mixed gas inlet is formed in the side wall of the upper part of the furnace tube, and a tubular furnace outlet is formed in the bottom end of the furnace tube; a gas purifier; a gas analyzer and a second vent valve. The system and the method can evaluate the thermal conversion process of the solid containing the organic matters.
Description
Technical Field
The invention belongs to the technical field of energy, and particularly relates to a system and a method for evaluating thermal conversion of solids containing organic matters.
Background
Organic solids such as coal, oil sand, biomass, municipal solid waste and sludge contain a large amount of energy, and can be converted into liquid or gas fuel in a pyrolysis and gasification manner besides combustion utilization, so that the utilization manner and the way of the organic solids are expanded undoubtedly. There are many factors that affect the yield and properties of the organic-containing solid, mainly the organic-containing solid itself and the process conditions. The self characteristics of the solid containing organic matters comprise ash content, moisture content, organic matter content, types and the like; thermal conversion process conditions include temperature, heating rate, pressure, residence time, atmosphere, and the like. The method needs to evaluate the organic solid in a certain thermal conversion process condition, comprehensively compares the product distribution, yield, energy consumption and economy, and is particularly important for establishing a set of thermal conversion evaluation device and method.
The thermal conversion temperature is a major factor affecting product yield and properties. In the case of thermal conversion of coal, generally, the higher the temperature, the greater the degree of coal conversion, the higher the total volatiles yield, and the less solid residue (char or coke). The heating rate itself has no significant effect on the overall volatiles yield when pyrolyzing coal, but affects the rate of devolatilization production at different temperatures. The results of the research on the thermal conversion of the single-particle coal in the inert atmosphere by an electrothermal method show that when the heating speed is changed within the range of 100-1500 ℃/s, the removal of volatile matters from the bituminous coal is slightly influenced, and the total yield of volatile matters can be improved only by increasing the heating speed when the heating speed reaches over 1000 ℃/s. The bituminous coal is subjected to thermal conversion by using an electric heating metal net within the range of 0.0001-10MPa, and the total volatile matter yield is monotonically reduced along with the increase of the pressure. The thermal weight loss under vacuum is 1.14 times that under normal pressure, and the thermal weight loss under 10MPa is 74% under normal pressure. The removal of the volatile matter requires a certain time, and the lower the temperature is, the longer the complete removal of the volatile matter requires; while the time required to complete a degree of devolatilization at higher temperatures is very short. In the case of thermal conversion in a hydrogen atmosphere, CH 4 And C 2 The content of the above hydrocarbons is higher than that of CH in nitrogen atmosphere and helium atmosphere 4 The yield is high. The pyrolysis of lignite in a coke oven gas atmosphere reduces the conversion by about 7% compared to that in a hydrogen atmosphere, the tar yield increases by about 7%, and the tar yield under both conditions is higher than that in a nitrogen atmosphere (Liao Hongjiang et al, journal of fuel chemistry, 1997, 104). In the presence of 400mL/min CH in the reaction gas 4 And 100mL/min O 2 When the pyrolysis temperature is 700 ℃ and the pressure is 2MPa, the tar yield of Yanzhou coal is under the same condition H 2 Tar in atmosphereThe yield is 1.7 times, accordingly, hu Haoquan provides a method (CN 101747922A) for improving the yield of tar produced by coal pyrolysis in a fluidized bed by taking methane-rich mixed gas as a reaction atmosphere, the method improves the yield of the tar produced by coal pyrolysis in the fluidized bed by replacing hydrogen used in conventional hydropyrolysis after the methane-rich mixed gas is subjected to catalytic conversion, the process can reduce the cost of hydropyrolysis, simplify the operation, increase the treatment capacity and realize large-scale production, and the yield of the obtained tar is higher than that of the tar produced by hydropyrolysis under the same conditions. Therefore, only by systematically evaluating the thermal conversion conditions of the organic-containing solids can a route be found that maximizes the value utilization of the organic-containing solids.
However, the existing evaluation method has the defects of complicated process and poor repeatability. CN 110441491A discloses a coal gasification evaluation device and method, which can obtain relatively reliable material balance data, but the device has many unit systems, the daily treatment reaches 1 ton, the whole evaluation period needs 1 week, and the time and cost for evaluating one coal type are relatively large. CN 108519301A discloses a method for evaluating coal and biomass coke reactivity by using a thermogravimetric analyzer, which has the characteristics of simple operation and generally requires a sample amount below 1g to obtain some thermal conversion characteristic indexes, but because the sample amount is too small and the general uniformity of solid organic matters is poor, the influence of the amount and representativeness of the sample amount on the detection result is great, and the obtained solid and liquid products are difficult to collect due to too small mass, and the material balance data and the product yield are difficult to obtain. GB/T220-2018 provides a method for determining the reactivity of coal to carbon dioxide, which is often used for evaluating the gasification reaction activity of coal, and the method requires that the coal is subjected to dry distillation, coke with a specific particle size is selected and then reacts with the carbon dioxide, and a reactivity curve of temperature-carbon dioxide reduction rate is drawn.
Disclosure of Invention
The first purpose of the invention is to provide a system for carrying out thermal conversion evaluation on the solid containing organic substances, which has simple structure and convenient use, and can evaluate the influence of the conditions such as temperature, heating form, heating rate, atmosphere, retention time and the like on the thermal conversion in the thermal conversion process of the solid containing organic substances;
the second purpose of the invention is to provide a method for evaluating the thermal conversion of the solid containing organic substances by utilizing the system, which evaluates the influence of the conditions such as temperature, heating form, heating rate, atmosphere and residence time of the solid containing organic substances in the thermal conversion process on the thermal conversion by adjusting the process conditions.
In order to achieve the first purpose of the invention, the following technical scheme is adopted:
a system for thermal conversion evaluation of solids containing organic matter, the system comprising a gas distribution unit, a gas heating unit, a weighing unit, a cooling unit, and a gas analysis unit;
the gas distribution unit comprises a protection gas circuit and N which are arranged in parallel 2 Gas path, CO 2 Gas path, CH 4 Gas path H 2 The gas circuit and the air circuit, and the gas mixer, the emptying gas circuit and the analysis gas circuit; wherein,
the protection gas path branch is a protection gas branch and a drying gas branch; the protective gas branch is connected to the weighing unit and used for providing nitrogen as protective gas for the weighing unit; the dry gas branch is connected to the gas heating unit and used for introducing nitrogen from the protective gas circuit into the gas heating unit for heating;
said N is 2 Gas path, CO 2 Gas path, the CH 4 Gas path H 2 The gas circuit and the air circuit are respectively connected to the gas mixer and are used for respectively providing corresponding gas to mix the gas in the gas mixer to obtain mixed gas;
said N is 2 The gas circuit is also connected to the weighing unit and used for inputting hot nitrogen into the weighing unit to purge and preheat; said N is 2 The gas circuit is also provided with five branch gas circuits which are five branchesThe first ends of the gas circuits are respectively connected to the N 2 The second end of the gas path is respectively connected to the CO gas path and the CO 2 Gas path, the CH 4 Gas path H 2 The air inlet ends of the air path and the air path are used for respectively purging the air path and the air path;
one end of the analysis gas circuit is connected to the gas mixer, and the other end of the analysis gas circuit is connected to the gas analysis unit and used for outputting the mixed gas from the gas mixer to the gas analysis unit for gas analysis;
one end of the emptying gas circuit is connected to the gas mixer, and the other end of the emptying gas circuit is connected with a first emptying valve and used for outputting the mixed gas from the gas mixer to be emptied;
the gas heating unit comprises a heater, the heater is connected to the dry gas branch and used for heating the nitrogen from the dry gas branch so as to be used as the dry gas of the weighing unit;
the weighing unit comprises a weighing structure and a heat conversion structure; wherein,
the weighing structure comprises a balance chamber, a weighing rod, a cooling water jacket, a first connector and a sample basket;
an electronic balance is arranged in the balance chamber and used for recording the weight change of the sample in the sample basket in real time;
the top end of the weighing rod extends into the balance chamber and is fixed to the bottom end of the electronic balance in the balance chamber, and the sample basket is suspended at the bottom end of the weighing rod;
the cooling water jacket is sleeved outside the weighing rod and used for cooling the weighing rod, and a cooling space surrounded by the inner wall of the cooling water jacket is formed and used as a sample standby chamber; the lower end of the sample preparation chamber is provided with a dry gas inlet, the dry gas inlet is connected to a gas outlet of the heater through a pipeline and is used for introducing dry gas from the heater into the sample preparation chamber so as to dry a sample in the sample preparation chamber;
the first connector is fixed at the bottom end of the cooling water jacket and is used for being connected with the heat conversion structure;
the heat conversion structure comprises a tube furnace, a furnace tube with the same central axis is arranged in the center of the tube furnace, a second connector is arranged at the top end of the furnace tube, and the second connector is matched with the first connector and is used for being connected in a matched manner to communicate the sample standby chamber and the furnace tube;
a mixed gas inlet is formed in the side wall of the upper part of the furnace tube, a tubular furnace outlet is formed in the bottom end of the furnace tube, and the mixed gas is introduced from the mixed gas inlet so that a sample in the sample basket is subjected to thermal conversion in the furnace tube, and the thermal conversion gas is output from the tubular furnace outlet; the thermal conversion process comprises combustion and gasification;
the cooling unit comprises a gas purifier, the gas purifier is connected to the outlet of the tube furnace through a pipeline and is used for purifying and decontaminating the thermal conversion gas from the weighing unit to obtain decontaminated gas which is used as the inlet gas of the gas analysis unit;
the gas analysis unit comprises a gas analyzer and a second vent valve; the gas analyzer is connected to an outlet pipeline of the gas purifier and is used for carrying out gas analysis on impurity-removed gas from the gas purifier; the second vent valve is connected to the outlet line of the gas analyzer for venting the incoming gas.
Preferably, the thermal conversion procedure further comprises pyrolysis; the cooling unit further comprises a condenser and a condensate collector; the condenser is arranged on a pipeline from the outlet of the tube furnace to the gas purifier and is used for condensing the hot converted gas from the weighing unit to obtain condensate and non-condensable gas; the condensate collector is arranged on a pipeline from the condenser to the gas purifier and is used for receiving condensate and non-condensable gas from the condenser and collecting the condensate; the gas purifier is used for receiving the non-condensable gas from the condensate collector and purifying and removing impurities of the non-condensable gas to obtain impurity-removed gas which is used as the inlet gas of the gas analysis unit.
Preferably, the gas distribution unit further comprises a heating gas path, one end of the heating gas path is connected to the gas mixer, and the other end of the heating gas path is connected to the gas heating unit, and is used for outputting the mixed gas from the gas mixer to the gas heating unit for heating;
the gas heating unit also comprises a gas heating furnace, the gas heating furnace is connected to the heating gas circuit and is used for heating the mixed gas from the heating gas circuit to obtain the heated mixed gas as the inlet gas of the weighing unit;
the furnace tube is used for introducing the mixed gas from the gas heating unit from the mixed gas inlet so as to heat and pyrolyze the sample in the sample basket, and the pyrolysis gas serving as the thermal conversion gas is output from the outlet of the tube furnace.
Preferably, in the weighing unit, the weighing structure further comprises a protective sleeve, the protective sleeve is sleeved outside the weighing rod, and the top end of the protective sleeve is fixed to the bottom end of the balance chamber; the cooling water jacket is sleeved outside the protective sleeve.
Preferably, a graphite sealing ring is arranged at the top of the cooling water jacket, and the graphite sealing ring is sleeved on the protective sleeve together with the cooling water jacket and used for sealing the top of the sample chamber to be prepared.
Preferably, the weighing structure further comprises a sample feeding rod, a balance chamber supporting rod and a horizontal fixing rod; the sample feeding rod is arranged in parallel with the weighing rod, and a first slide rail is arranged on the sample feeding rod along the length direction of the sample feeding rod; the horizontal fixed rod is perpendicular to the sample feeding rod, and a first end of the horizontal fixed rod is fixed to the first connecting head, and a second end of the horizontal fixed rod is fixed to the bottom end of the sample feeding rod; balance room bracing piece with horizontal fixed rod parallel arrangement, its first end is fixed extremely on the upper portion outer wall of protective case, the second end be provided with first slide rail matched with first slider, balance room bracing piece passes through first slider with first slide rail with advance kind of pole slip and set up, be used for following advance kind of pole and slide from top to bottom, in order to drive the sample basket certainly the bottom of cooling water jacket gets into or sees off the sample is treated and is equipped with the room.
Preferably, the weighing unit further comprises a rotating structure, and the rotating structure comprises a rotating support rod and a rotating transverse plate;
the rotary supporting rod is vertically arranged;
the rotating transverse plate is provided with a first through hole perpendicular to the plane of the rotating transverse plate, and the rotating transverse plate is vertically and rotatably sleeved on the rotating support rod through the first through hole and is used for rotating in the horizontal plane by taking the rotating support rod as a rotating shaft;
the cooling water jacket is connected to the first end of the rotating transverse plate and used for connecting the weighing structure to the top end of the furnace tube along with the horizontal rotation of the rotating transverse plate.
Preferably, the first through hole is arranged at the center of the rotating transverse plate; the second end of the rotating transverse plate is provided with a sealing cover, and the sealing cover is matched with the second connector and used for rotating the horizontal rotating transverse plate to connect the weighing structure/the sealing cover to the top end of the furnace tube.
Preferably, the balance chamber is provided with a shielding gas inlet, and the shielding gas inlet is communicated with the shielding gas branch and is used for introducing nitrogen from the shielding gas branch into the balance chamber to serve as shielding gas of an electronic balance therein.
Preferably, the gas analysis unit further comprises a back pressure valve, the back pressure valve and the gas analyzer are arranged between the gas purifier and the second emptying valve in parallel, and the back pressure valve is used for adjusting the gas pressure of the impurity-removed gas from the cooling unit, so that a part of the impurity-removed gas is input into the gas analyzer, and the rest of the impurity-removed gas is emptied.
Preferably, the gas analysis unit further comprises a gas washing bottle, which is arranged on a pipeline from the gas analyzer to the second emptying valve and is used for washing impurities from the gas analyzer for emptying.
In order to achieve the second object of the present invention, the present invention also provides a method for evaluating the thermal conversion of the organic matter-containing solid by using the system.
The invention has the beneficial effects that:
the system for carrying out thermal conversion evaluation on the solid containing the organic substances has a simple structure, is convenient to use, and can evaluate the influence of conditions such as temperature, heating form, heating rate, atmosphere, retention time and the like on the thermal conversion in the thermal conversion process of the solid containing the organic substances;
according to the method for evaluating the thermal conversion of the solid containing the organic substances by using the system, the influence of conditions such as temperature, heating form, heating rate, atmosphere and residence time of the solid containing the organic substances on the thermal conversion in the thermal conversion process can be evaluated by adjusting the process conditions;
the system and the method of the invention can realize the following functions: 1. the maximum treatment capacity of the sample is 100g, the weighing unit tracks and records the mass change (namely the weight loss condition) of the sample in the thermal conversion process in real time, and the collection of solid, liquid and gas products can be realized; 2. the gas distribution unit realizes the regulation of the composition of the thermal conversion atmosphere for the inert atmosphere (N) 2 ) Reducing atmosphere (H) 2 ) Simulating thermal conversion evaluation under the atmosphere of coke oven gas, and realizing combustion, pyrolysis and gasification evaluation of solids containing organic substances by adjusting the atmosphere; 3. the thermal conversion evaluation temperature range can be controlled between 300 ℃ and 1100 ℃, the rapid heating of hot gas can be realized, and the heating rate is 50 ℃/min to 100 ℃/min; the tubular furnace thermal radiation heating can also be realized, and the heating rate is 5-30 ℃/min; or the two heating modes are simultaneously used; 4. the rapid cooling of the solid-liquid product can be realized, the rapid cooling of the solid product obtained after the thermal conversion is realized by blowing inert cold gas into the sample standby chamber, and the rapid cooling of the liquid product is realized by adjusting the heat exchange area in the cooling unit and the flow of the cooling medium.
Drawings
FIG. 1 is a schematic diagram of a system for thermal conversion evaluation of an organic-containing solid according to one embodiment of the present invention;
fig. 2-5 are state diagrams of the weighing unit shown in fig. 1 at four stages in a sample introduction process, wherein the four stages are sequentially that the sample basket is positioned outside the sample preparation chamber, the sample basket enters the sample preparation chamber, the sample preparation chamber is communicated with the furnace tube, and the sample basket enters the furnace tube from the sample preparation chamber.
Detailed Description
The technical solution and effects of the present invention will be further described with reference to the accompanying drawings and the detailed description. The following embodiments are merely illustrative of the present invention, and the present invention is not limited to the following embodiments or examples. Simple modifications of the invention applying the inventive concept are within the scope of the invention as claimed.
As shown in fig. 1 to 5, the present invention provides a system for thermal conversion evaluation of organic matter-containing solids, the system comprising a gas distribution unit 1, a gas heating unit 2, a weighing unit 3, a cooling unit 4 and a gas analysis unit 5;
the gas distribution unit 1 comprises protection gas circuits 6 and N which are arranged in parallel 2 Gas path 7, CO gas path 8, CO 2 Gas path 9, CH 4 Gas circuit 10, H 2 A gas path 11 and an air path 12, and a gas mixer 13, a venting gas path 17 and an analyzing gas path 18; wherein,
the protective gas path 6 is branched into a protective gas branch 14 and a drying gas branch 15; the shielding gas branch 14 is connected to the weighing unit 3 and is used for providing nitrogen gas as shielding gas for the weighing unit 3; the dry gas branch 15 is connected to the gas heating unit 2 and is used for introducing nitrogen from the protective gas circuit 6 into the gas heating unit 2 for heating;
said N is 2 Gas path 7, CO gas path 8, CO 2 Gas path 9, CH 4 Gas path 10, H 2 The gas circuit 11 and the air circuit 12 are respectively connected to the gas mixer 13, and are used for respectively providing corresponding gas to perform gas blending in the gas mixer 13 to obtain a mixed gas;
said N is 2 The gas circuit 7 is also connected to the weighing unit 3 and is used for inputting hot nitrogen into the weighing unit 3 to purge and preheat; said N is 2 The gas circuit 7 is also provided with five branch gas circuits, and the first ends of the five branch gas circuits are respectively connected to the N 2 The air inlet end of the air passage 7,a second end is connected to the CO gas path 8 and the CO respectively 2 Gas path 9, CH 4 Gas path 10, H 2 The air inlet ends of the air path 11 and the air path 12 are used for respectively purging the air path and the air path;
one end of the analysis gas path 18 is connected to the gas mixer 13, and the other end is connected to the gas analysis unit 5, and is configured to output the mixture gas from the gas mixer 13 to the gas analysis unit 5 for gas analysis;
one end of the air release path 17 is connected to the gas mixer 13, and the other end is connected to a first air release valve for outputting the mixed gas from the gas mixer 13 to release air;
the gas heating unit 2 comprises a heater 39, the heater 39 is connected to the drying gas branch 15 and is used for heating the nitrogen gas from the drying gas branch 15 to be used as the drying gas of the weighing unit 3;
the weighing unit 3 comprises a weighing structure and a heat conversion structure; wherein,
the weighing structure comprises a balance chamber 24, a weighing rod 25, a cooling water jacket 29, a first connecting head 32 and a sample basket 35;
an electronic balance is arranged in the balance chamber 24 and used for recording the weight change of the sample in the sample basket 35 in real time;
the top end of the weighing rod 25 extends into the balance chamber 24 and is fixed to the bottom end of the electronic balance in the balance chamber 24, and the sample basket 35 is hung at the bottom end of the weighing rod 25;
the cooling water jacket 29 is sleeved outside the weighing rod 25 and used for cooling the weighing rod, and a cooling space surrounded by the inner wall of the cooling water jacket 29 is formed and used as a sample standby chamber 28; a dry gas inlet is arranged at the lower end of the sample preparation chamber 28, and is connected to the gas outlet of the heater 39 through a pipeline, so that dry gas from the heater 39 is introduced into the sample preparation chamber 28 to dry a sample in the sample preparation chamber;
the first connector 32 is fixed at the bottom end of the cooling water jacket 29 and is used for connecting with the heat conversion structure;
the thermal conversion structure comprises a tube furnace 36, a furnace tube 37 with the same central axis is arranged in the center of the tube furnace 36, a second connector 33 is arranged at the top end of the furnace tube 37, and the second connector 33 is matched with the first connector 32 and is used for matching connection to communicate the sample standby chamber 28 with the furnace tube 31;
a mixed gas inlet 34 is arranged on the upper side wall of the furnace tube 37, a tubular furnace outlet 38 is arranged at the bottom end of the furnace tube 37, and the mixed gas is introduced from the mixed gas inlet 34 so that the sample in the sample basket 35 is thermally converted in the furnace tube 37, and the thermally converted gas is output from the tubular furnace outlet 38; the thermal conversion process comprises combustion and gasification;
the cooling unit 4 comprises a gas purifier 46, wherein the gas purifier 46 is connected to the outlet 38 of the tube furnace through a pipeline and is used for purifying and decontaminating the thermal conversion gas from the weighing unit 3 to obtain decontaminated gas which is used as the inlet gas of the gas analysis unit 5;
the gas analysis unit 5 comprises a gas analyzer 49 and a second vent valve; the gas analyzer 49 is connected to an outlet line of the gas purifier 46 for performing gas analysis on the impurity-removed gas from the gas purifier 46; the second vent valve is connected to the outlet line of the gas analyzer 49 for venting the incoming gas.
It will be appreciated by those skilled in the art that the shielding gas circuit 6 provides cold nitrogen gas. In the invention, the protective gas branch 14 introduces cold nitrogen into the balance chamber 24 to generate gas pressure, and on one hand, the protective gas branch is used as cooling gas to cool and protect the electronic balance in the balance chamber 24 and prevent hot gas in the furnace tube 37 from rising, so that the temperature in the balance chamber 24 rises to damage the electronic balance therein; on the other hand, the hot reformed gas can be prevented from rising and is output from the bottom of the furnace tube 37; and the dry gas branch circuit 15 leads cold nitrogen gas into the sample preparation chamber 28 as dry gas after the cold nitrogen gas is heated by the heater 39, and can dry the sample in the sample basket 35.
Those skilled in the art will appreciate that the weighing rod 25 can move up and down along the central axis of the cooling water jacket 29 relative to the cooling water jacket 29.
It will be appreciated by those skilled in the art that the first connector 32 and the second connector 33 may be connectors commonly used in the art, and preferably are flange structures.
In the present invention, after the sample after thermal conversion rises to the sample preparation chamber 28 along with the sample basket 35, the sample may be removed along with the cooling water jacket 29 for natural cooling, or under the condition that the heater 39 is not activated, the dry gas branch 15 may be used to output cold nitrogen gas, and the cold nitrogen gas is conveyed to the sample preparation chamber 28 after passing through the heater 39 which is not activated, so as to rapidly cool the sample in the sample basket 35 therein.
Those skilled in the art understand that each gas path is provided with a flow meter, such as a mass flow meter, and the mass flow meter on each gas path can control the transportation of the gas in each gas path to the gas mixer 13, so as to realize the mixing of different gases.
Those skilled in the art will appreciate that the gas purifier 46 may be a gas filter having a filter layer that may be filled with absorbent cotton and calcium oxide.
Those skilled in the art will appreciate that sometimes it is desirable to first analyze the composition of the gas mixture, and this may be done by analyzing gas path 18.
The system for carrying out thermal conversion evaluation on the solid containing the organic substances has a simple structure, is convenient to use, and can evaluate the influence of conditions such as temperature, heating form, heating rate, atmosphere, retention time and the like on the thermal conversion in the thermal conversion process of the solid containing the organic substances; the maximum treatment capacity of the sample is 100g, and the weighing unit tracks and records the mass change (namely the weight loss condition) of the sample in the thermal conversion process in real time, so that the collection of solid, liquid and gas products can be realized; the gas distribution unit realizes the regulation of the composition of the thermal conversion atmosphere for the inert atmosphere (N) 2 ) Reducing atmosphere (H) 2 ) And simulating thermal conversion evaluation under the atmosphere of coke oven gas, and realizing the purpose of solid containing organic matters by adjusting the atmosphereThermal conversion evaluation of (3).
In one embodiment, the thermal conversion procedure further comprises pyrolysis; the cooling unit 4 further comprises a condenser and condensate collector 45; the condenser is arranged on a pipeline from the outlet 38 of the tube furnace to the gas purifier 46 and is used for condensing the hot converted gas from the weighing unit 3 to obtain condensate and non-condensable gas;
the condensate collector 45 is provided on a line from the condenser to the gas purifier 46, and receives the condensate and the non-condensable gas from the condenser and collects the condensate;
the gas purifier 46 is configured to receive the non-condensable gas from the condensed liquid collector 45 and purify the non-condensable gas to obtain impurity-removed gas, which is used as the inlet gas of the gas analysis unit 5.
Those skilled in the art understand that thermal conversion processes involving organic solids include combustion, pyrolysis, and gasification; during combustion and gasification, tar is not generated, so that the hot converted gas does not need to be condensed and can be directly fed into the gas purifier to be purified and removed to be used as the inlet gas of the gas analysis unit; during pyrolysis, tar is generated, so that the hot converted gas needs to be condensed to liquefy the tar, so as to obtain a condensate and noncondensable gas, and then the noncondensable gas enters the gas purifier to be purified and impurity-removed and then can be used as the inlet gas of the gas analysis unit. Therefore, when the thermal conversion process includes pyrolysis, the cooling unit 4 is further provided with a condenser and a condensate collector 45; when the thermal reforming process includes only combustion and gasification, but does not include pyrolysis, the cooling unit 4 does not need to be provided with a condenser and a condensate collector 45, and if provided, the condensate may not be introduced to perform a condensation function when the thermal reforming gas is introduced into the condenser, and the thermal reforming gas passes through the condenser and the condensate collector 45, but enters the gas purifier without being condensed to be purified. Therefore, the system is suitable for the thermal conversion evaluation of the combustion and gasification of the organic matter-containing solid as well as the pyrolysis of the organic matter-containing solid, after the cooling unit 4 is provided with the condenser and the condensate collector 45.
In one embodiment, the gas distribution unit 1 further includes a heating gas path 16, one end of the heating gas path 16 is connected to the gas mixer 13, and the other end is connected to the gas heating unit 2, for outputting the mixture gas from the gas mixer 13 to the gas heating unit 2 for heating;
the gas heating unit 2 further comprises a gas heating furnace 40, wherein the gas heating furnace 40 is connected to the heating gas path 16 and is used for heating the mixed gas from the heating gas path 16 to obtain the heated mixed gas as the inlet gas of the weighing unit 3;
the furnace tube 37 is used for introducing the mixed gas from the gas heating unit 2 from the mixed gas inlet 34 to perform heating pyrolysis on the sample in the sample basket 35, and outputting the pyrolysis gas as the thermal conversion gas from the tube furnace outlet 38.
Those skilled in the art will appreciate that when pyrolysis is carried out, organic-containing solids may not only be pyrolyzed by radiatively heating them using the tube furnace 36, but may also be pyrolyzed by rapidly heating them using hot gases. Therefore, the gas distribution unit 1 is provided with the heating gas path 16, and the gas heating unit 2 is provided with the gas heating furnace 40, so that the mixed gas mixed in the gas distribution unit 1 can be heated, for example, to 600-700 ℃, to thermally pyrolyze the sample placed in the sample basket 35 in the furnace tube 37. The arrangement provides a pyrolysis mode for solids containing organic matters, so that the system is more convenient to use, and the pyrolysis mode can be selected at will according to needs.
In order to protect the weighing rod 25 and prolong the service life of the weighing rod 25, in one embodiment, in the weighing unit 3, the weighing structure further comprises a protective sleeve 26, the protective sleeve 26 is sleeved outside the weighing rod 25, and the top end of the protective sleeve 26 is fixed to the bottom end of the balance chamber 24; the cooling water jacket 29 is sleeved outside the protection sleeve 26. Meanwhile, the protective sleeve 26 can also avoid direct interference of gas flow on the weighing rod 25, so that the measurement accuracy of the electronic balance in the balance chamber 24 is prevented from being influenced, the measurement precision of the thermal weight loss condition is improved, and an accurate thermal weight loss curve is obtained.
In one embodiment, the top of the cooling water jacket 29 is provided with a graphite sealing ring 27, and the graphite sealing ring 27 is sleeved on the protection sleeve 26 together with the cooling water jacket 29 for sealing the top of the sample chamber 28.
The graphite sealing ring 27 is arranged to seal the top of the sample standby chamber 28 on one hand, and to fix the weighing rod 25 in the horizontal direction on the other hand, so that the weighing rod is prevented from shaking left and right in the sample standby chamber 28 to influence the measurement accuracy of the electronic balance in the balance chamber 24, and the measurement accuracy of the thermal weight loss condition is improved to obtain an accurate thermal weight loss curve.
In one embodiment, in the weighing unit 3, the weighing structure further comprises a sample feeding rod 22, a balance chamber support rod 23 and a horizontal fixing rod 321;
the sample feeding rod 22 and the weighing rod 25 are arranged in parallel, and a first sliding rail is arranged on the sample feeding rod 22 along the length direction of the sample feeding rod;
the horizontal fixing rod 321 is perpendicular to the sample feeding rod 22, and a first end thereof is fixed to the first connector 32, and a second end thereof is fixed to the bottom end of the sample feeding rod 22;
balance room bracing piece 23 with horizontal fixed rod 321 parallel arrangement, its first end is fixed extremely on the upper portion outer wall of protective case 26, the second end be provided with first slider of first slide rail matched with, balance room bracing piece 23 pass through first slider with first slide rail with advance kind of pole 22 and slide and set up, be used for following advance kind of pole 22 and slide from top to bottom, in order to drive sample basket 35 certainly the bottom of cooling water jacket 29 gets into or sends out the sample is waited for room 28.
The arrangement of the sample feeding rod 22, the balance chamber supporting rod 23 and the horizontal fixing rod 321 enables the weighing rod 25 to move in the vertical direction for sample feeding during sample feeding, so that the influence of the left-right shaking of the weighing rod by other conditions on the measurement accuracy of the electronic balance in the balance chamber 24 is prevented, the measurement accuracy of the condition of thermal weightlessness of the solid containing organic matters is improved, and an accurate thermal weightlessness curve is obtained.
In one embodiment, the weighing unit 3 further comprises a rotating structure comprising a rotating support bar 20 and a rotating cross plate 201;
the rotary supporting rod 20 is vertically arranged;
the rotating transverse plate 201 is provided with a first through hole perpendicular to the plane of the rotating transverse plate, and the rotating transverse plate 201 is vertically and rotatably sleeved on the rotating support rod 20 through the first through hole and is used for rotating in the horizontal plane by taking the rotating support rod 20 as a rotating shaft;
the cooling water jacket 29 is connected to a first end of the rotating transverse plate 201 and is used for connecting the weighing structure to the top end of the furnace tube 37 along with the horizontal rotation of the rotating transverse plate 201.
The setting of revolution mechanic for advance the kind process and need not manual control weigh the overall position of structure, only need rotate rotation diaphragm 201, can remove weigh the overall position of structure, it is convenient weigh the structure with the connection and the assembly of thermal conversion structure also make things convenient for simultaneously after the thermal conversion will weigh the structure and follow in the thermal conversion structure the top of boiler tube 37 is removed for advance kind process and the process of appearance of going out convenient and fast more. After the weighing structure is removed from the top end of the furnace tube 37 in the thermal conversion structure, a sealing cover can be covered on the top end of the furnace tube 37.
In order to prevent the sealing cover from being lost, in a preferred embodiment, the first through hole is arranged at the center of the rotating transverse plate 201; the second end of the rotating transverse plate 201 is provided with a sealing cover 21, and the sealing cover 21 is matched with the second connector 33 and used for connecting the weighing structure/the sealing cover 21 to the top end of the furnace tube 37 along with the horizontal rotation of the rotating transverse plate 201.
By the arrangement, the sealing cover 21 can be prevented from being lost, and after the distance from the rotating support rod 20 to the furnace tube 37 is adjusted, the weighing structure and the sealing cover 21 can be alternated at the top end of the furnace tube 37 only by rotating the rotating transverse plate 201, so that the weighing structure is convenient and quick to use, and easy to operate.
In one embodiment, the weighing unit 3 further comprises a rotating structure comprising a rotating support bar 20 and a rotating cross plate 201;
the rotary supporting rod 20 is vertically arranged;
a first through hole perpendicular to the plane of the rotating transverse plate 201 is formed in the center of the rotating transverse plate 201, and the rotating transverse plate 201 is vertically and rotatably sleeved on the rotating support rod 20 through the first through hole and is used for rotating in the horizontal plane by taking the rotating support rod 20 as a central shaft;
the first end of the rotating transverse plate 201 is connected to the cooling water jacket 29, the second end of the rotating transverse plate is provided with a sealing cover 21, and the sealing cover 21 is matched with the second connecting head 33 and used for enabling the rotating transverse plate 201 to rotate around the rotating support rod 20 horizontally so as to connect the weighing structure/the sealing cover 21 to the top end of the furnace tube 37.
The setting of revolution mechanic for advance the kind process and need not manual control weigh the overall position of structure, only need rotate rotation diaphragm 201, can remove weigh the overall position of structure, it is convenient weigh the structure with the connection and the assembly of thermal conversion structure also make things convenient for simultaneously after the thermal conversion will weigh the structure follow in the thermal conversion structure the top of boiler tube 37 is removed and is covered sealed lid 21 for advance the kind process and go out the appearance process convenient and fast more.
Those skilled in the art will understand that the first end of the rotating transverse plate 201 and the cooling water jacket 29 may be fixedly connected or slidably connected. In one embodiment, a third slide rail is disposed outside the cooling water jacket 29 along the vertical direction, a third slide block matched with the third slide rail is disposed at the first end of the rotating transverse plate 201, and the cooling water jacket 29 is slidably disposed with the first end of the rotating transverse plate 201 through the third slide rail and the third slide block, and is configured to slide up and down to adjust the vertical position of the cooling water jacket 29, so that convenience is further provided.
It is understood by those skilled in the art that when the rotating structure is not provided, a separate sealing cover may be additionally used to cover the top end of the furnace tube 37 when the sealing cover needs to be used for sealing the top end of the furnace tube 37.
It is understood by those skilled in the art that when the sealing cover 21 and the first connection head 32 are at the same level, the sealing cover 21 and the first connection head 32 can be replaced at the top end of the furnace tube 37 only by rotating the rotating horizontal plate 201. In one embodiment, the top of the sealing cover 21 is provided with a vertical fixing rod, and the vertical fixing rod is vertically arranged at the second end of the rotating transverse plate 201.
In an embodiment, a second slide rail is arranged on the vertical fixing rod along the length direction of the vertical fixing rod, a second slider matched with the second slide rail is arranged at the second end of the rotating transverse plate 201, and the vertical fixing rod is arranged at the second end of the rotating transverse plate 201 in a sliding manner through the second slide rail and the second slider and used for sliding up and down to adjust the vertical position of the sealing cover 21, so that the vertical fixing rod is more convenient to use.
Those skilled in the art will appreciate that during the evaluation, the hot gas in the furnace tube 37 will travel upward and enter the sample preparation chamber 28 and the balance chamber 24 in sequence, thereby damaging the electronic balance in the balance chamber 24. In one embodiment, the balance chamber 24 is provided with a shielding gas inlet, and the shielding gas inlet is communicated with the shielding gas branch 14, and is used for introducing cold nitrogen from the shielding gas branch 14 into the balance chamber 24 to serve as shielding gas for the electronic balance therein, so as to perform a cooling function, and perform cooling protection on the electronic balance therein.
In one embodiment, the cooling unit 4 comprises a first-stage condenser, a second-stage condenser and a third-stage condenser connected in series in sequence, and is used for condensing the thermal conversion gas from the weighing unit 3 in three stages in sequence.
It is understood by those skilled in the art that the primary condenser, the secondary condenser and the tertiary condenser are all condensers commonly used in the art, such as a double pipe condenser.
In one embodiment, the gas analysis unit 5 further comprises a backpressure valve 47, the backpressure valve 47 is arranged between the gas purifier 46 and the second emptying valve in parallel with the gas analyzer 49, and is used for adjusting the gas pressure of the impurity-removed gas from the cooling unit 4, so that a part of the impurity-removed gas is input into the gas analyzer 49, and the rest of the impurity-removed gas is emptied;
in one embodiment, the gas analysis unit 5 further comprises a purge gas bottle 48, the purge gas bottle 48 being arranged on the line from the gas analyzer 49 to the second vent valve for washing the gas from the gas analyzer 49 away from impurities for venting.
As shown in fig. 1, the system for evaluating the thermal conversion of solids containing organic substances according to the present invention is operated as follows:
the weighing rod 25 with its outer protective sleeve 26 is passed in from the top of the sample preparation chamber 28 and out from the bottom thereof; the sample is then placed in the sample basket 35, and the sample basket 35 is then suspended to the bottom of the weigh bar 25; then sliding the balance chamber support rod 23 upwards along the sample injection rod 22 to drive the weighing rod 25 and the sample basket 35 to move upwards until the sample basket 35 is positioned in the sample preparation chamber 28; then horizontally rotating the horizontal rotating plate 201 around the horizontal rotating support rod 20 to connect the first connecting head 32 and the second connecting head 33 so as to communicate the sample preparation chamber 28 and the furnace tube 37;
opening a related gas path in the gas distribution unit 1; the protective gas branch 14 conveys the cold nitrogen gas from the protective gas circuit 6 to the balance chamber 24 in the weighing unit 3 to carry out cooling protection on the electronic balance therein; the drying gas branch circuit 15 conveys the cold nitrogen gas from the protective gas circuit 6 to the heater 39 for heating, and then conveys the cold nitrogen gas to the sample preparation chamber 28 for pre-drying the sample in the sample basket 35 therein;
the CO gas path 8 and the CO 2 Gas path 9, CH 4 Gas path 10, H 2 At least one of the air path 11 and the air path 12 and the N 2 Gas path 7 mixes the gasThe device 13 delivers corresponding gas for mixing to obtain mixed gas;
the balance chamber support rod 23 slides downwards along the sample injection rod 22 to drive the weighing rod 25 and the sample basket 35 to move downwards until the sample basket 35 is positioned in the middle of the furnace tube 37;
starting the gas heating furnace 40, conveying the mixed gas to the gas heating furnace 40 of the gas heating unit 2 through the heating gas path 16, heating the mixed gas, conveying the heated mixed gas to the sample preparation chamber 28 to heat the sample in the sample basket 35 therein for thermal conversion (pyrolysis), and outputting the thermal conversion gas through the tube furnace outlet 38 of the furnace tube 37; or, the tube furnace 36 is started without starting the gas heating furnace 40, the mixed gas passes through the heating gas path 16 and the gas heating furnace 40 in sequence and is then conveyed into the furnace tube 37, and is subjected to temperature programming for thermal conversion (pyrolysis, combustion or gasification) by the tube furnace 36, and a thermal conversion gas is output through the tube furnace outlet 38 of the furnace tube 37;
during pyrolysis, introducing condensate into the condenser, conveying the hot converted gas to the condenser of the cooling unit for condensation, conveying the obtained condensate and non-condensable gas to the condensate collector 45 for collecting the condensate, and outputting the non-condensable gas from the condensate collector 45 to the gas purifier 46 for purification and impurity removal to obtain impurity-removed gas; the impurity-removed gas is input to the gas analyzer 49 in the gas analysis unit 5 for component analysis; during combustion and gasification, the condenser is not communicated with condensate, and the hot converted gas is conveyed to the gas purifier 46 through the condenser and the condensate collector 45 in sequence to be purified and decontaminated, so that decontaminated gas is obtained; the impurity-removed gas is input to the gas analyzer 49 in the gas analysis unit 5 for component analysis;
if necessary, the mixed gas output from the gas mixer 13 may be directly sent to the gas analyzer 49 in the gas analysis unit 5 for component analysis.
The system for carrying out thermal conversion evaluation on the solid containing the organic matter has simple structure and convenient use, and can evaluate the solid containing the organic matterThe influence of conditions such as temperature, heating form, heating rate, atmosphere and residence time on thermal conversion in the thermal conversion process of the body can realize the following functions: 1. the maximum treatment capacity of the sample is 100g, the weighing unit tracks and records the mass change (namely the weight loss condition) of the sample in the thermal conversion process in real time, and the collection of solid, liquid and gas products can be realized; 2. the gas distribution unit realizes the regulation of the composition of the thermal conversion atmosphere for the inert atmosphere (N) 2 ) Reducing atmosphere (H) 2 ) Simulating thermal conversion evaluation under the atmosphere of coke oven gas, and realizing combustion, pyrolysis and gasification evaluation of the solid containing organic substances through adjusting the atmosphere; 3. the thermal conversion evaluation temperature range can be controlled between 300 ℃ and 1100 ℃, the rapid heating of hot gas can be realized, and the heating rate is 50-100 ℃/min; the tubular furnace thermal radiation heating can also be realized, and the heating rate is 5-30 ℃/min; or the two heating modes are simultaneously used; 4. the rapid cooling of the solid-liquid product can be realized, the rapid cooling of the solid product obtained after the thermal conversion is realized by blowing inert cold gas into the sample standby chamber, and the rapid cooling of the liquid product is realized by adjusting the heat exchange area in the cooling unit and the flow of the cooling medium.
The invention also provides a method for evaluating the thermal conversion of the solid containing the organic matters by utilizing the system.
In one embodiment, the method comprises the steps of:
(1) Balance baseline
a1, hanging the sample basket 35 which does not contain the sample on the weighing rod 25, and lifting the sample basket to the sample preparation chamber 28;
b1, connecting the first connector 32 and the second connector 33 in a matching manner, so that the sample preparation chamber 28 is communicated with the furnace tube 37, and then lowering the sample basket 35 to the middle part of the furnace tube 37;
c1, opening corresponding gas paths in the gas distribution unit 1 according to different thermal conversion programs, adjusting the flow of the gas paths, starting an electronic balance in the balance chamber 24 after the flow is stable, and performing zero resetting correction on the electronic balance after the electronic balance is stable; the thermal conversion process includes combustion, pyrolysis and gasification;
(2) Thermal conversion
a2, weighing a sample, placing the weighed sample in the sample basket 35, hanging the weighed sample on the weighing rod 25, and lifting the weighed sample to the sample preparation chamber 28;
b2, connecting the first connector 32 and the second connector 33 in a matching manner, so that the sample preparation chamber 28 is communicated with the furnace tube 37, and then lowering the sample basket 35 to the middle part of the furnace tube 37;
c2, starting the tube furnace 36, setting a temperature rise program of the tube furnace, and recording a thermal transformation weight loss curve of the sample by using an electronic balance in the balance chamber 24;
(3) Sample cooling and sampling
a3, lifting the sample basket 35 to the sample preparation chamber 28, then separating the first connector 32 from the second connector 33, and removing the weighing structure from the upper part of the furnace tube 37 to cool the sample; when the weighing structure is removed from the upper part of the furnace tube 37, the top end of the furnace tube 37 needs to be sealed and covered;
b3, descending the sample basket 35, sending the sample preparation chamber 28 out from the bottom end of the cooling water jacket 29, and taking out the sample in the sample basket 35;
(4) Data analysis
a4, analyzing the thermal transformation weight loss curve obtained in the step (2);
b4, when the thermal conversion procedure is combustion or gasification, inputting the thermal conversion gas output by the outlet 38 of the tube furnace into the cooling unit 4, purifying and removing impurities by the gas purifier 46, and inputting the thermal conversion gas into the gas analysis unit 5 for component analysis;
when the thermal conversion procedure is pyrolysis, pyrolysis gas output from the outlet 38 of the tube furnace is input into the cooling unit 4, and condensate obtained after condensation by the condenser is collected in the condensate collector 45; the non-condensable gas obtained after condensation by the condenser is output from the condensate collector 45, purified and decontaminated by the gas purifier 46, and then input to the gas analysis unit 5 for component analysis.
Those skilled in the art will appreciate that when the thermal conversion process is pyrolysis, the sample containing organic solids may be heated either radiatively using a tube furnace 36 for pyrolysis or rapidly using hot gases. In one embodiment, when the thermal conversion procedure is pyrolysis, the c2 step in step (2) may be replaced with a d2 step; wherein the step d2 is as follows: the gas heater 40 was turned on, the heating power was set, and the thermal transition weight loss curve of the sample was recorded using an electronic balance in the balance chamber 24.
In one embodiment, the thermal conversion process is pyrolysis, and in c1 of step (1), the opened corresponding gas paths in the gas distribution unit 1 are the protection gas path 6 and the N 2 The gas circuit 7 adjusts the flow rate of the protective gas branch 14 to 5-10L/min, such as 6L/min, 7L/min, 8L/min and 9L/min, and N is 2 The flow rate of the gas circuit 7 is 20-50L/min, such as 25L/min, 30L/min, 35L/min, 40L/min and 45L/min; preferably, in d2 of the step (2), the heating power of the gas heater 40 is 5-10kw, such as 6kw, 7kw, 8kw and 9kw. As understood by those skilled in the art, when the thermal conversion process is pyrolysis, in a4 of step (4), the thermal conversion weight loss curve obtained in step (2) is analyzed, and the gas entering the gas analysis unit 5 is analyzed by using an on-line chromatograph. In one embodiment, the thermal conversion procedure is combustion, and in step (2), a2, the sample in the sample basket 35 is 50g of coal sample with a particle size of 3-6mm, and the standard accuracy is 0.01g.
In one embodiment, the thermal conversion procedure is combustion, and in step (1) c1, the opened corresponding gas paths in the gas distribution unit 1 are the protection gas path 6 and the protection gas path N 2 The gas circuit 7 and the air circuit 12 adjust the flow rate of the protective gas branch 14 to 20-50L/min, such as 25L/min, 30L/min, 35L/min, 40L/min and 45L/min, and the N is 2 The flow rate of the air path 7 is 5-10L/min, such as 6L/min, 7L/min, 8L/min and 9L/min, and the flow rate of the air path 12 is 50-150L/min, such as 60L/min, 70L/min, 80L/min, 90L/min, 100L/min, 110L/min, 120L/min, 130L/minMin and 140L/min; preferably, in c2 of the step (2), the temperature of the tube furnace 36 is raised from room temperature to 1000 ℃ at a temperature raising rate of 10-20 ℃/min (such as 12 ℃/min, 14 ℃/min, 16 ℃/min and 18 ℃/min). As understood by those skilled in the art, when the thermal conversion procedure is combustion, in step (4) a4, the thermal conversion weight loss curve obtained in step (2) is analyzed according to GB/T33304-2016. In one embodiment, when the thermal conversion process is combustion, in step (2), a2, the sample in the sample basket 35 is 10g of coal sample with a particle size of 3-6mm, and the standard precision is 0.01g.
In one embodiment, the thermal conversion procedure is gasification, and in step (1) c1, the opened corresponding gas paths in the gas distribution unit 1 are the protection gas path 6 and the protection gas path N 2 Gas path 7 and the CO 2 The gas circuit 9 adjusts the flow rate of the protective gas branch 14 to 10-20L/min, such as 12L/min, 14L/min, 16L/min and 18L/min, wherein N is 2 The flow rate of the gas path 7 is 0-1L/min, such as 0.2L/min, 0.4L/min, 0.6L/min and 0.8L/min, and the CO is 2 The flow rate of the gas circuit 9 is 0.5-2L/min, such as 0.7L/min, 0.8L/min, 1.0L/min, 1.2L/min, 1.4L/min, 1.6L/min and 1.8L/min; after the electronic balance is reset to zero, the protective gas circuit 6 and the N are closed 2 Gas path 7 and the CO 2 A gas path 9; preferably, in the step c2 of the step (2), the temperature of the tube furnace 36 is raised from room temperature to 750 ℃ at a temperature raising rate of 20-25 ℃/min, the temperature is maintained for 5min, and the protection gas circuit 6 and the N are opened again 2 Gas path 7 and the CO 2 Gas path 9 in the CO 2 The gas path 9 is opened again for 2.5min, the gas introduced into the gas analyzer 49 in the gas analysis unit 5 is analyzed, the analysis process is 1min, and the percentages of carbon dioxide and carbon monoxide in the gas are analyzed and recorded; then continuously heating at a heating rate of 20-25 ℃/min, wherein the temperature per liter is increased by 50 ℃, and keeping the temperature for 5min; the gas introduced into the gas analyzer 49 of the gas analysis unit 5 is then analyzed for 1min and recorded until the temperature reaches 1100 ℃.
As understood by those skilled in the art, when the thermal conversion procedure is gasification, in step (4), in step a4, the thermal conversion weight loss curve of 750-1100 ℃ obtained in step (2) is analyzed according to GB/T220-2018.
In one embodiment, when the thermal conversion process is gasification, in step (2), the sample in the sample basket 35 is 10g of coal sample with a particle size of 3-6mm, and the standard precision is 0.01g.
The method for evaluating the thermal conversion of the organic matter-containing solid by using the system can evaluate the influence of conditions such as temperature, heating form, heating rate, atmosphere and residence time of the organic matter-containing solid in the thermal conversion process on the thermal conversion, and can realize the following functions: 1. the maximum treatment capacity of the sample is 100g, the weighing unit tracks and records the mass change (namely the weight loss condition) of the sample in the thermal conversion process in real time, and the collection of solid, liquid and gas products can be realized; 2. the gas distribution unit realizes the regulation of the composition of the thermal conversion atmosphere for the inert atmosphere (N) 2 ) Reducing atmosphere (H) 2 ) Simulating thermal conversion evaluation under the atmosphere of coke oven gas, and realizing combustion, pyrolysis and gasification evaluation of the solid containing organic substances through adjusting the atmosphere; 3. the thermal conversion evaluation temperature range can be controlled between 300 ℃ and 1100 ℃, the rapid heating of hot gas can be realized, and the heating rate is 50-100 ℃/min; the tubular furnace thermal radiation heating can also be realized, and the heating rate is 5-30 ℃/min; or the two heating modes are simultaneously used; 4. the rapid cooling of the solid-liquid product can be realized, the rapid cooling of the solid product obtained after the thermal conversion is realized by blowing inert cold gas into the sample standby chamber, and the rapid cooling of the liquid product is realized by adjusting the heat exchange area in the cooling unit and the flow of the cooling medium.
Claims (9)
1. A system for thermal conversion evaluation of solids containing organic matter, characterized in that the system comprises a gas distribution unit (1), a gas heating unit (2), a weighing unit (3), a cooling unit (4) and a gas analysis unit (5);
the gas heating unit (2) comprises a heater (39) and a gas heating furnace (40);
the gas distribution unit (1) comprises protection gas circuits which are arranged in parallel(6)、N 2 Gas circuit (7), CO gas circuit (8), CO 2 Gas path (9), CH 4 Gas circuit (10), H 2 A gas path (11) and an air path (12), and a gas mixer (13), an emptying gas path (17) and an analysis gas path (18); wherein,
the protection gas circuit (6) is branched into a protection gas branch (14) and a drying gas branch (15); the shielding gas branch (14) is connected to the weighing unit (3) and is used for providing nitrogen as shielding gas for the weighing unit (3); the dry gas branch (15) is connected to the heater (39) in the gas heating unit (2) and is used for introducing nitrogen from the protective gas circuit (6) into the heater (39) for heating so as to be used as a dry gas for the weighing unit (3);
said N is 2 A gas circuit (7), the CO gas circuit (8) and the CO 2 Gas path (9) and the CH 4 A gas path (10) and H 2 The gas circuit (11) and the air circuit (12) are respectively connected to the gas mixer (13) and are used for respectively providing corresponding gas to mix the gas in the gas mixer (13) to obtain mixed gas;
said N is 2 The gas circuit (7) is also connected to the weighing unit (3) and is used for inputting hot nitrogen into the weighing unit (3) to purge and preheat; said N is 2 The gas circuit (7) is also provided with five branch gas circuits, and the first ends of the five branch gas circuits are respectively connected to the N 2 The air inlet end of the air passage (7) and the second end of the air passage are respectively connected to the CO air passage (8) and the CO 2 Gas path (9) and the CH 4 A gas path (10) and H 2 The air inlet ends of the air path (11) and the air path (12) are used for respectively purging the air path and the air path;
one end of the analysis gas circuit (18) is connected to the gas mixer (13), and the other end of the analysis gas circuit is connected to the gas analysis unit (5) and is used for outputting the mixed gas from the gas mixer (13) to the gas analysis unit (5) for gas analysis;
one end of the emptying gas circuit (17) is connected to the gas mixer (13), and the other end of the emptying gas circuit is connected with a first emptying valve for outputting the mixed gas from the gas mixer (13) to be emptied;
the weighing unit (3) comprises a weighing structure and a heat conversion structure; wherein,
the weighing structure comprises a balance chamber (24), a weighing rod (25), a cooling water jacket (29), a first connecting head (32) and a sample basket (35);
an electronic balance is arranged in the balance chamber (24) and used for recording the weight change of the sample in the sample basket (35) in real time;
the top end of the weighing rod (25) extends into the balance chamber (24) and is fixed to the bottom end of the electronic balance in the balance chamber (24), and the sample basket (35) is hung at the bottom end of the weighing rod (25);
the cooling water jacket (29) is sleeved outside the weighing rod (25) and used for cooling the weighing rod, and a cooling space surrounded by the inner wall of the cooling water jacket (29) is formed to serve as a sample standby chamber (28); a drying gas inlet is formed in the lower end of the sample preparation chamber (28), and is connected to a gas outlet of the heater (39) through a pipeline and used for introducing drying gas from the heater (39) into the sample preparation chamber (28) so as to dry a sample in the sample preparation chamber;
the first connecting head (32) is fixed at the bottom end of the cooling water jacket (29) and is used for being connected with the heat conversion structure;
the thermal conversion structure comprises a tube furnace (36), a furnace tube (37) with the same central axis is arranged in the center of the tube furnace (36), a second connector (33) is arranged at the top end of the furnace tube (37), and the second connector (33) is matched with the first connector (32) and is used for being connected in a matching manner to communicate the sample standby chamber (28) with the furnace tube (31);
a mixed gas inlet (34) is formed in the side wall of the upper part of the furnace tube (37), a tubular furnace outlet (38) is formed in the bottom end of the furnace tube (37), and the mixed gas is introduced from the mixed gas inlet (34) so that the sample in the sample basket (35) is thermally converted in the furnace tube (37), and the thermally converted gas is output from the tubular furnace outlet (38); the thermal conversion comprises combustion and gasification;
the cooling unit (4) comprises a gas purifier (46), the gas purifier (46) is connected to the outlet (38) of the tube furnace through a pipeline and is used for purifying and impurity-removing the hot converted gas from the weighing unit (3) to obtain impurity-removed gas which is used as the inlet gas of the gas analysis unit (5);
the gas analysis unit (5) comprises a gas analyzer (49) and a second vent valve; the gas analyzer (49) is connected to an outlet line of the gas purifier (46) for gas analysis of the purge gas from the gas purifier (46); the second vent valve is connected to the outlet line of the gas analyzer (49) for venting the incoming gas;
the gas distribution unit (1) further comprises a heating gas path (16), one end of the heating gas path (16) is connected to the gas mixer (13), the other end of the heating gas path is connected to the gas heating furnace (40) of the gas heating unit (2), and the heating gas path is used for outputting the mixed gas from the gas mixer (13) to the gas heating furnace (40) for heating so as to obtain the heated mixed gas as the inlet gas of the weighing unit (3);
the furnace tube (37) is used for introducing the mixed gas from the gas heating unit (2) from the mixed gas inlet (34);
in the weighing unit (3), the weighing structure further comprises a protective sleeve (26), the protective sleeve (26) is sleeved outside the weighing rod (25), and the top end of the protective sleeve is fixed to the bottom end of the balance chamber (24); the cooling water jacket (29) is sleeved outside the protective sleeve (26);
in the weighing unit (3), the weighing structure further comprises a sample feeding rod (22), a balance chamber supporting rod (23) and a horizontal fixing rod (321);
the sample feeding rod (22) and the weighing rod (25) are arranged in parallel, and a first slide rail is arranged on the sample feeding rod (22) along the length direction of the sample feeding rod;
the horizontal fixing rod (321) is perpendicular to the sample feeding rod (22), and a first end of the horizontal fixing rod is fixed to the first connector (32) and a second end of the horizontal fixing rod is fixed to the bottom end of the sample feeding rod (22);
the balance room supporting rod (23) is arranged in parallel with the horizontal fixing rod (321), the first end of the balance room supporting rod is fixed on the outer wall of the upper part of the protective sleeve (26), the second end of the balance room supporting rod is provided with a first sliding block matched with the first sliding rail, the balance room supporting rod (23) is arranged in a sliding way with the sample injection rod (22) through the first sliding block and the first sliding rail and is used for sliding up and down along the sample injection rod (22) so as to drive the sample basket (35) to enter or be sent out of the sample standby room (28) from the bottom end of the cooling water jacket (29);
the weighing unit (3) further comprises a rotating structure, and the rotating structure comprises a rotating support rod (20) and a rotating transverse plate (201);
the rotary supporting rod (20) is vertically arranged;
the rotating transverse plate (201) is provided with a first through hole perpendicular to the plane where the rotating transverse plate (201) is located, and the rotating transverse plate (201) is vertically and rotatably sleeved on the rotating support rod (20) through the first through hole and used for rotating in the horizontal plane by taking the rotating support rod (20) as a rotating shaft;
the cooling water jacket (29) is connected to a first end of the rotating transverse plate (201) and is used for connecting the weighing structure to the top end of the furnace tube (37) along with the horizontal rotation of the rotating transverse plate (201).
2. The system of claim 1, wherein the thermal conversion process further comprises pyrolysis; the cooling unit (4) further comprises a condenser and a condensate collector (45);
the condenser is arranged on a pipeline from the outlet (38) of the tube furnace to the gas purifier (46) and is used for condensing the hot converted gas from the weighing unit (3) to obtain condensate and non-condensable gas;
the condensate collector (45) is arranged on a pipeline from the condenser to the gas purifier (46) and is used for receiving condensate and non-condensable gas from the condenser and collecting the condensate;
the gas purifier (46) is used for receiving the non-condensable gas from the condensate collector (45) and purifying and removing impurities of the non-condensable gas to obtain impurity-removed gas which is used as the inlet gas of the gas analysis unit (5).
3. The system of claim 2,
the furnace tube (37) is used for introducing the mixed gas from the gas heating unit (2) from the mixed gas inlet (34) to carry out heating pyrolysis on the sample in the sample basket (35), and outputting pyrolysis gas serving as thermal conversion gas from the tube furnace outlet (38).
4. The system according to any one of claims 1-3,
the top of the cooling water jacket (29) is provided with a graphite sealing ring (27), and the graphite sealing ring (27) is sleeved on the protective sleeve (26) along with the cooling water jacket (29) and is used for sealing the top of the sample standby chamber (28).
5. The system according to claim 1, characterized in that said first through hole is provided in the centre of said rotating cross plate (201); the second end of rotating diaphragm (201) is provided with sealed lid (21), sealed lid (21) with second connector (33) cooperation sets up, be used for along with the horizontal rotation of rotating diaphragm (201) will weigh structure/sealed lid (21) are connected to the top of boiler tube (37).
6. The system according to any one of claims 1 to 3 and 5, characterized in that the balance chamber (24) is provided with a shielding gas inlet communicating with the shielding gas branch (14) for passing nitrogen gas from the shielding gas branch (14) into the balance chamber (24) as a shielding gas for the electronic balance therein.
7. The system according to claim 1, characterized in that the gas analysis unit (5) further comprises a backpressure valve (47), the backpressure valve (47) being arranged in parallel with the gas analyzer (49) between the gas purifier (46) and the second emptying valve for adjusting the gas pressure of the impure gas coming from the cooling unit (4) to feed a part of the impure gas into the gas analyzer (49) and to empty the remaining part.
8. A system according to any of claims 1-3, 5 and 7, characterized in that the gas analysis unit (5) further comprises a gas scrubber bottle (48), which scrubber bottle (48) is arranged on the line from the gas analyzer (49) to the second emptying valve for scrubbing the gas from the gas analyzer (49) with impurities for emptying.
9. A method for evaluating the thermal conversion of an organic-containing solid using the system of any one of claims 1-8, the method comprising the steps of:
(1) Balance baseline
a1, hanging the sample basket (35) not containing the sample on the weighing rod (25) and lifting the sample basket to the sample preparation chamber (28);
b1, the first connector (32) is matched and connected with the second connector (33), so that the sample preparation chamber (28) is communicated with the furnace tube (37), and then the sample basket (35) is lowered to the middle of the furnace tube (37);
c1, opening corresponding gas paths in the gas distribution unit (1) according to different thermal conversion programs, adjusting the flow of the gas paths, starting an electronic balance in the balance chamber (24) after the flow is stable, and performing zero resetting correction on the electronic balance after the electronic balance is stable; the thermal conversion process includes combustion, pyrolysis, and gasification;
(2) Thermal conversion
a2, weighing a sample, then placing the weighed sample in the sample basket (35), then hanging the weighed sample on the weighing rod (25), and lifting the weighed sample to the sample preparation chamber (28);
b2, connecting the first connector (32) with the second connector (33) in a matching way, so that the sample preparation chamber (28) is communicated with the furnace tube (37), and then descending the sample basket (35) to the middle part of the furnace tube (37);
c2, starting the tube furnace (36), setting a temperature rise program of the tube furnace, and recording a thermal transformation weight loss curve of the sample by using an electronic balance in the balance chamber (24);
(3) Sample cooling and sampling
a3, lifting the sample basket (35) to the sample preparation chamber (28), then separating the first connector (32) from the second connector (33), and removing the weighing structure from the upper part of the furnace tube (37) to cool the sample; the top end of the furnace tube (37) needs to be sealed and covered while the weighing structure is removed from the upper part of the furnace tube (37);
b3, descending the sample basket (35), sending the sample to-be-prepared chamber (28) out of the bottom end of the cooling water jacket (29), and taking out the sample in the sample basket (35);
(4) Data analysis
a4, analyzing the thermal transformation weight loss curve obtained in the step (2);
b4, the thermal conversion procedure comprises combustion or gasification, the thermal conversion gas output from the outlet (38) of the tube furnace is input into the cooling unit (4), purified and decontaminated by the gas purifier (46), and then input into the gas analysis unit (5) for component analysis.
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