CN114354884A - Device and method for measuring slagging property in strong reducing atmosphere - Google Patents

Device and method for measuring slagging property in strong reducing atmosphere Download PDF

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CN114354884A
CN114354884A CN202111404057.4A CN202111404057A CN114354884A CN 114354884 A CN114354884 A CN 114354884A CN 202111404057 A CN202111404057 A CN 202111404057A CN 114354884 A CN114354884 A CN 114354884A
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tube
temperature
furnace
reducing gas
inlet pipe
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CN114354884B (en
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纪明俊
李建
王双美
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Jiangsu Design And Research Institute Of Geology And Mineral Resources Test Center Of China Coal Geology Administration
Anhui University of Science and Technology
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Jiangsu Design And Research Institute Of Geology And Mineral Resources Test Center Of China Coal Geology Administration
Anhui University of Science and Technology
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Abstract

The invention discloses a device and a method for measuring slagging property of strong reducing atmosphere, and the device comprises a shell, wherein a hollow furnace tube penetrates through the shell, the furnace tube is used for placing a corundum tube, a plurality of cupels are arranged on the corundum tube, one end of the furnace tube is opened and is detachably provided with a sight glass, one end of the furnace tube close to the sight glass is communicated with a mixed gas inlet tube, one end of the mixed gas inlet tube far away from the furnace tube is communicated with a mixing cavity in the mixing tube, and the mixing cavity is communicated with a strong reducing gas inlet tube and an N2The intake pipe, just the fixed fan that is provided with in the mixing chamber to blow the gas in the mixing chamber to the mist intake pipe, the boiler tube is kept away from the one end intercommunication of sight glass has the blast pipe, still be provided with the heating rod in the casing, the heating rod distributes the both sides of boiler tube, the casing upper end is still fixed voltmeter, flow table and the temperature controller of being provided with. The method can be used for measuring the slagging property of the strong reducing atmosphere.

Description

Device and method for measuring slagging property in strong reducing atmosphere
Technical Field
The invention relates to the technical field of slagging characteristic measurement, in particular to a device and a method for measuring slagging characteristic of strong reducing atmosphere.
Background
In the dry slagging gasification process, in order to increase the carbon conversion rate to the maximum extent, the operation temperature (but lower than the slagging temperature) must be properly increased, so that the slagging problem is easily caused, the gasification efficiency is affected if the slagging is light, and the production is stopped due to the blockage of a slag hole of the gasification furnace in serious cases. Therefore, the research on the gasification slagging characteristic of the dry slagging has very important theoretical and practical significance. The slagging property is an important index of normal, efficient and economic production of coal gasification enterprises, and in the past research, a JX-1 type slagging property tester is generally adopted to measure the slagging property of coal combustion under an oxidizing atmosphere, and the experimental condition cannot accurately measure the slagging property under a reaction gasification condition (reducing atmosphere).
Disclosure of Invention
Based on the technical problems in the background art, the invention provides the device and the method for measuring the slagging property of the strong reducing atmosphere, which can be used for measuring the slagging property of the strong reducing atmosphere and have high measurement accuracy.
The device for measuring the slagging property of the strong reducing atmosphere comprises a shell, wherein a hollow furnace tube penetrates through the shell and is used for placing a corundum tube, a plurality of cupels are arranged on the corundum tube, one end of the furnace tube is opened and is detachably provided with a sight glass, one end of the furnace tube close to the sight glass is communicated with a mixed gas inlet tube, one end of the mixed gas inlet tube far away from the furnace tube is communicated with a mixing cavity in the mixing tube, and the mixing cavity is communicated with a strong reducing gas inlet tube and an N2The intake pipe, just the fixed fan that is provided with in the mixing chamber to blow the gas in the mixing chamber to the mist intake pipe, the boiler tube is kept away from the one end intercommunication of sight glass has the blast pipe, still be provided with the heating rod in the casing, the heating rod distributes the both sides of boiler tube, the casing upper end is still fixed voltmeter, flow table and the temperature controller of being provided with.
Preferably, the heating rod is a type 1800 silicon molybdenum rod.
The invention provides a testing method of the device for measuring the slagging property of the strong reducing atmosphere, which comprises the following steps:
s1: putting an ash sample into an ash pan for cinder burning, and then putting the ash pan on a corundum boat;
s2: opening a left end sight glass of the furnace, horizontally pushing the corundum boat into the furnace tube, and then screwing down the sight glass to ensure air tightness;
s3: setting a temperature rise program through a temperature controller;
s4: by controlling the strong reducing gas inlet pipe and N2The flow of the reducing gas entering the furnace pipe is adjusted by the flow of the gas inlet pipe;
s5: when the temperature in the furnace tube reaches the required temperature point, closing a valve of the strong reducing gas inlet tube, increasing the flow of the N2 inlet tube until the strong reducing gas in the furnace tube is blown away, then quickly taking out the corundum tube, putting the corundum tube into a dryer for cooling, and sealing and storing;
s6: taking out the slag sample, adding N2For shielding gas, keep N2The flow rate of the N-containing refractory material is 40-60mL/min so as to prevent a corundum tube of the furnace from being broken in the temperature reduction process, and the N is closed after the temperature of the furnace is reduced to 600 DEG C2And turning off the power supply when the furnace temperature is reduced to the room temperature.
Preferably, the strong reducing gas in S4 is CO and/or H2
Preferably, the strong reducing gas in S4 is CO and H2Mixing at a ratio of 2-4: 1.
Preferably, the procedure of raising the temperature in S3 is: when the temperature is lower than 900 ℃, the heating rate is 12-18 ℃/min, when the temperature is 900-1400 ℃, the heating rate is 4-6 ℃/min, and 1400 ℃ is taken as the heating end point.
Preferably, the reducing gas inlet pipe and N in S42The air inlet pipe flow control program is as follows: when the temperature is lower than 900 ℃, only N is opened2An air inlet pipe, the flow rate of which is controlled to be 80-120mL/min, and when the temperature is 900 ℃ and 1400 ℃, the reducing gas inlet pipe and N are opened simultaneously2An inlet pipe, a reducing gas inlet pipe and N2The flow ratio of the gas inlet pipe is 3-5:1, and the reducing gas and the N are controlled2The total flow rate of (A) is 350-450 mL/min.
The invention has the beneficial technical effects that:
(1) the method can be used for measuring the characteristics of the slagging in a strong reducing atmosphere, and has high accuracy.
(2) The mixing pipe of the invention can realize strong reducing gas and N2Thereby ensuring the accuracy of the subsequent slagging property.
(3) The strong reducing gas of the invention consists of CO and H2The accuracy of the measuring result is also improved by designing a temperature rising program and a gas flow control program.
Drawings
FIG. 1 is a schematic structural diagram of a strong reducing atmosphere slagging property measuring device provided by the invention;
A-E in FIG. 2 are the ash-like slagging morphologies at 1000 deg.C, 1100 deg.C, 1200 deg.C, 1300 deg.C, and 1400 deg.C, respectively.
In the figure: 1-shell, 2-exhaust pipe, 3-voltmeter, 4-ammeter, 5-temperature controller, 6-mixed gas inlet pipe, 7-strong reducing gas inlet pipe, 8-mixing cavity, 9-mixing pipe, 10-fan, 11-N2The device comprises an air inlet pipe, 12-furnace tubes, 13-corundum tubes, 14-cupel and 15-heating rods.
Detailed Description
Referring to fig. 1, the device for measuring the slagging property of the strong reducing atmosphere provided by the invention comprises a shell, wherein a hollow furnace tube penetrates through the shell, the furnace tube is used for placing a corundum tube, a plurality of cupels are arranged on the corundum tube, a sight glass is detachably arranged at an opening at one end of the furnace tube, which is close to the sight glass, is communicated with a mixed gas inlet tube, one end of the mixed gas inlet tube, which is far away from the furnace tube, is communicated with a mixing cavity in the mixing tube, and the mixing cavity is communicated with a strong reducing gas inlet tube and an N (nitrogen) reducing gas inlet tube2An air inlet pipe, a fan is fixedly arranged in the mixing cavity to blow the gas in the mixing cavity to the mixed gas inlet pipe, the furnace tube is far away from one end of the viewing mirror is communicated with an exhaust pipe, and the shell is internally provided with a fanThe heating rod is distributed on two sides of the furnace tube, and a voltmeter, a flow meter and a temperature controller are fixedly arranged at the upper end of the shell.
Wherein: the heating rod is 1800 type silicon-molybdenum rod; the temperature shows a descending trend along with the increase of the distance from the center of the hearth to the furnace mouth, and the arrangement sequence of the cupels is arranged on the corundum tube according to a certain distance according to the requirement of a temperature gradient curve, wherein the measured temperature of the invention comprises 1400 ℃, 1300 ℃, 1200 ℃, 1100 ℃, 1000 ℃ and 900 ℃; the shell and the control system are designed integrally, the inner wall of the shell is made of silicon oxide multi-fiber materials, and two ends of the furnace tube are sealed by stainless steel vacuum flanges; the exhaust pipe is communicated with a tail gas treatment system, and the tail gas is discharged after being qualified, so that the environmental pollution is reduced.
The mixing pipe of the invention can realize strong reducing gas and N2Thereby ensuring the accuracy of the subsequent slagging property.
Example 1
The invention provides a testing method of the device for measuring the slagging property of the strong reducing atmosphere, which comprises the following steps:
s1: putting an ash sample into an ash pan for cinder burning, and then putting the ash pan on a corundum boat;
s2: opening a left end sight glass of the furnace, horizontally pushing the corundum boat into the furnace tube, and then screwing down the sight glass to ensure air tightness;
s3: setting a temperature rise program through a temperature controller;
s4: by controlling the strong reducing gas inlet pipe and N2The flow of the reducing gas entering the furnace pipe is adjusted by the flow of the gas inlet pipe;
s5: when the temperature in the furnace tube reaches the required temperature point, closing a valve of the strong reducing gas inlet tube, increasing the flow of the N2 inlet tube until the strong reducing gas in the furnace tube is blown away, then quickly taking out the corundum tube, putting the corundum tube into a dryer for cooling, and sealing and storing;
s6: taking out the slag sample, adding N2For shielding gas, keep N2The flow rate of (A) is 50mL/min, so as to prevent the corundum tube of the furnace from being broken in the cooling process, and the temperature of the furnace is reduced to 600 ℃ so as to prevent the corundum tube of the furnace from being brokenThen, turn off N2And turning off the power supply when the furnace temperature is reduced to the room temperature.
The strong reducing gas in S4 is CO and H2Mixing at a ratio of 3: 1.
The temperature raising procedure in S3 is: when the temperature is lower than 900 ℃, the heating rate is 15 ℃/min, when the temperature is 900 ℃ and 1400 ℃, the heating rate is 5 ℃/min, and 1400 ℃ is taken as the heating end point.
Reducing gas inlet pipe and N in S42The air inlet pipe flow control program is as follows: when the temperature is lower than 900 ℃, only N is opened2An air inlet pipe, the flow rate of which is controlled to be 100mL/min, and when the temperature is 900 ℃ and 1400 ℃, the reducing gas inlet pipe and N are opened simultaneously2An inlet pipe, a reducing gas inlet pipe and N2The flow ratio of the gas inlet pipe is 4:1, and the reducing gas and the N are controlled2The total flow rate of (2) was 400 mL/min.
Example 2
The invention provides a testing method of the device for measuring the slagging property of the strong reducing atmosphere, which comprises the following steps:
s1: putting an ash sample into an ash pan for cinder burning, and then putting the ash pan on a corundum boat;
s2: opening a left end sight glass of the furnace, horizontally pushing the corundum boat into the furnace tube, and then screwing down the sight glass to ensure air tightness;
s3: setting a temperature rise program through a temperature controller;
s4: by controlling the strong reducing gas inlet pipe and N2The flow of the reducing gas entering the furnace pipe is adjusted by the flow of the gas inlet pipe;
s5: when the temperature in the furnace tube reaches the required temperature point, closing a valve of the strong reducing gas inlet tube, increasing the flow of the N2 inlet tube until the strong reducing gas in the furnace tube is blown away, then quickly taking out the corundum tube, putting the corundum tube into a dryer for cooling, and sealing and storing;
s6: taking out the slag sample, adding N2For shielding gas, keep N2The flow rate of the N-containing gas is 40mL/min so as to prevent the corundum tube of the furnace from being broken in the temperature reduction process, and the N is closed after the temperature of the furnace is reduced to 600 DEG C2And turning off the power supply when the furnace temperature is reduced to the room temperature.
The strong reducing gas in S4 is CO and H2Mixing at a ratio of 2: 1.
The temperature raising procedure in S3 is: when the temperature is lower than 900 ℃, the heating rate is 12 ℃/min, when the temperature is 900 ℃ and 1400 ℃, the heating rate is 4 ℃/min, and 1400 ℃ is taken as the heating end point.
Reducing gas inlet pipe and N in S42The air inlet pipe flow control program is as follows: when the temperature is lower than 900 ℃, only N is opened2An air inlet pipe, the flow rate of which is controlled to be 80mL/min, and when the temperature is 900 ℃ and 1400 ℃, the reducing gas inlet pipe and N are opened simultaneously2An inlet pipe, a reducing gas inlet pipe and N2The flow ratio of the gas inlet pipe is 3:1, and the reducing gas and the N are controlled2The total flow rate of (2) was 350 mL/min.
Example 3
The invention provides a testing method of the device for measuring the slagging property of the strong reducing atmosphere, which comprises the following steps:
s1: putting an ash sample into an ash pan for cinder burning, and then putting the ash pan on a corundum boat;
s2: opening a left end sight glass of the furnace, horizontally pushing the corundum boat into the furnace tube, and then screwing down the sight glass to ensure air tightness;
s3: setting a temperature rise program through a temperature controller;
s4: by controlling the strong reducing gas inlet pipe and N2The flow of the reducing gas entering the furnace pipe is adjusted by the flow of the gas inlet pipe;
s5: when the temperature in the furnace tube reaches the required temperature point, closing a valve of the strong reducing gas inlet tube, increasing the flow of the N2 inlet tube until the strong reducing gas in the furnace tube is blown away, then quickly taking out the corundum tube, putting the corundum tube into a dryer for cooling, and sealing and storing;
s6: taking out the slag sample, adding N2For shielding gas, keep N2The flow rate of the N-containing gas is 60mL/min so as to prevent the corundum tube of the furnace from being broken in the temperature reduction process, and the N is closed after the temperature of the furnace is reduced to 600 DEG C2And turning off the power supply when the furnace temperature is reduced to the room temperature.
The strong reducing gas in S4 is CO and H2According to the ratio of 4:1And (4) mixing.
The temperature raising procedure in S3 is: when the temperature is lower than 900 ℃, the heating rate is 18 ℃/min, when the temperature is 900 ℃ and 1400 ℃, the heating rate is 6 ℃/min, and 1400 ℃ is taken as the heating end point.
Reducing gas inlet pipe and N in S42The air inlet pipe flow control program is as follows: when the temperature is lower than 900 ℃, only N is opened2Gas inlet pipe, the flow rate of the gas inlet pipe is controlled to be 120mL/min, and when the temperature is 1400 ℃, the reducing gas inlet pipe and the N are opened simultaneously2An inlet pipe, a reducing gas inlet pipe and N2The flow ratio of the gas inlet pipe is 5:1, and the reducing gas and the N are controlled2The total flow rate of (2) was 450 mL/min.
Example 4
The invention provides a testing method of the device for measuring the slagging property of the strong reducing atmosphere, which comprises the following steps:
s1: putting an ash sample into an ash pan for cinder burning, and then putting the ash pan on a corundum boat;
s2: opening a left end sight glass of the furnace, horizontally pushing the corundum boat into the furnace tube, and then screwing down the sight glass to ensure air tightness;
s3: setting a temperature rise program through a temperature controller;
s4: by controlling the strong reducing gas inlet pipe and N2The flow of the reducing gas entering the furnace pipe is adjusted by the flow of the gas inlet pipe;
s5: when the temperature in the furnace tube reaches the required temperature point, closing a valve of the strong reducing gas inlet tube, increasing the flow of the N2 inlet tube until the strong reducing gas in the furnace tube is blown away, then quickly taking out the corundum tube, putting the corundum tube into a dryer for cooling, and sealing and storing;
s6: taking out the slag sample, adding N2For shielding gas, keep N2The flow rate of the N-containing gas is 50mL/min so as to prevent the corundum tube of the furnace from being broken in the temperature reduction process, and the N is closed after the temperature of the furnace is reduced to 600 DEG C2And turning off the power supply when the furnace temperature is reduced to the room temperature.
The strong reducing gas in S4 is CO.
The temperature raising procedure in S3 is: when the temperature is lower than 900 ℃, the heating rate is 15 ℃/min, when the temperature is 900 ℃ and 1400 ℃, the heating rate is 5 ℃/min, and 1400 ℃ is taken as the heating end point.
Reducing gas inlet pipe and N in S42The air inlet pipe flow control program is as follows: when the temperature is lower than 900 ℃, only N is opened2An air inlet pipe, the flow rate of which is controlled to be 100mL/min, and when the temperature is 900 ℃ and 1400 ℃, the reducing gas inlet pipe and N are opened simultaneously2An inlet pipe, a reducing gas inlet pipe and N2The flow ratio of the gas inlet pipe is 4:1, and the reducing gas and the N are controlled2The total flow rate of (2) was 400 mL/min.
Example 5
The invention provides a testing method of the device for measuring the slagging property of the strong reducing atmosphere, which comprises the following steps:
s1: putting an ash sample into an ash pan for cinder burning, and then putting the ash pan on a corundum boat;
s2: opening a left end sight glass of the furnace, horizontally pushing the corundum boat into the furnace tube, and then screwing down the sight glass to ensure air tightness;
s3: setting a temperature rise program through a temperature controller;
s4: by controlling the strong reducing gas inlet pipe and N2The flow of the reducing gas entering the furnace pipe is adjusted by the flow of the gas inlet pipe;
s5: when the temperature in the furnace tube reaches the required temperature point, closing a valve of the strong reducing gas inlet tube, increasing the flow of the N2 inlet tube until the strong reducing gas in the furnace tube is blown away, then quickly taking out the corundum tube, putting the corundum tube into a dryer for cooling, and sealing and storing;
s6: taking out the slag sample, adding N2For shielding gas, keep N2The flow rate of the N-containing gas is 50mL/min so as to prevent the corundum tube of the furnace from being broken in the temperature reduction process, and the N is closed after the temperature of the furnace is reduced to 600 DEG C2And turning off the power supply when the furnace temperature is reduced to the room temperature.
The strong reducing gas in S4 is H2
The temperature raising procedure in S3 is: when the temperature is lower than 900 ℃, the heating rate is 15 ℃/min, when the temperature is 900 ℃ and 1400 ℃, the heating rate is 5 ℃/min, and 1400 ℃ is taken as the heating end point.
Reducing gas inlet pipe and N in S42The air inlet pipe flow control program is as follows: when the temperature is lower than 900 ℃, only N is opened2An air inlet pipe, the flow rate of which is controlled to be 100mL/min, and when the temperature is 900 ℃ and 1400 ℃, the reducing gas inlet pipe and N are opened simultaneously2An inlet pipe, a reducing gas inlet pipe and N2The flow ratio of the gas inlet pipe is 4:1, and the reducing gas and the N are controlled2The total flow rate of (2) was 400 mL/min.
The shape of the ash sample slagging obtained in the embodiment 1 of the invention is shown in fig. 2, and the results of the compression strength test of the ash sample slagging obtained at different temperatures by using a digital display type WDW-S10 electronic universal tester are shown in table 1.
TABLE 1 compression Strength of ash sample slagging
Figure BDA0003372121100000071
As can be seen from table 1, the compressive strength of the slag sample is in an increasing trend along with the increase of the temperature, when the temperature is 1000 ℃, the compressive strength of the slag sample is very small, the sample is agglomerated but not melted, and when the temperature is 1100 ℃, the slag sample is sintered, the compressive strength is increased rapidly, and the higher the temperature is, the more obvious the sintering state is, the compressive strength is in an increasing trend, that is, the slagging strength is also in an increasing trend; in addition, when CO and H are used2When the reducing gas is mixed in a ratio of 3:1, the compressive strength of the obtained sample is high.
The present invention is not limited to the above preferred embodiments, and any modifications, equivalent substitutions, improvements, etc. within the spirit and principle of the present invention should be included in the protection scope of the present invention.

Claims (7)

1. The device for measuring the slagging property of the strong reducing atmosphere is characterized by comprising a shell, wherein the shell is provided with a hollow furnace tube in a penetrating way, the furnace tube is used for placing a corundum tube, a plurality of cupels are arranged on the corundum tube, one end of the furnace tube is open, andcan dismantle and be provided with the sight glass, the boiler tube is close to the one end intercommunication of sight glass has the mist intake pipe, the mist intake pipe is kept away from the one end and the hybrid chamber intercommunication in the hybrid tube of boiler tube, the hybrid chamber intercommunication has strong reducing gas intake pipe and N2The intake pipe, just the fixed fan that is provided with in the mixing chamber to blow the gas in the mixing chamber to the mist intake pipe, the boiler tube is kept away from the one end intercommunication of sight glass has the blast pipe, still be provided with the heating rod in the casing, the heating rod distributes the both sides of boiler tube, the casing upper end is still fixed voltmeter, flow table and the temperature controller of being provided with.
2. The apparatus of claim 1, wherein the heating rod is a type 1800 silicon molybdenum rod.
3. The method for measuring the slagging property of a strong reducing atmosphere according to claim 1 or 2, characterized by comprising the following steps:
s1: putting an ash sample into an ash pan for cinder burning, and then putting the ash pan on a corundum boat;
s2: opening a left end sight glass of the furnace, horizontally pushing the corundum boat into the furnace tube, and then screwing down the sight glass to ensure air tightness;
s3: setting a temperature rise program through a temperature controller;
s4: by controlling the strong reducing gas inlet pipe and N2The flow of the reducing gas entering the furnace pipe is adjusted by the flow of the gas inlet pipe;
s5: when the temperature in the furnace tube reaches the required temperature point, closing a valve of the strong reducing gas inlet tube, increasing the flow of the N2 inlet tube until the strong reducing gas in the furnace tube is blown away, then quickly taking out the corundum tube, putting the corundum tube into a dryer for cooling, and sealing and storing;
s6: taking out the slag sample, adding N2For shielding gas, keep N2The flow rate of the N-containing refractory material is 40-60mL/min so as to prevent a corundum tube of the furnace from being broken in the temperature reduction process, and the N is closed after the temperature of the furnace is reduced to 600 DEG C2And turning off the power supply when the furnace temperature is reduced to the room temperature.
4. The method for measuring the slagging property of strong reducing atmosphere according to claim 3, wherein the strong reducing gas in S4 is CO and/or H2
5. The method for measuring the slagging property of strong reducing atmosphere according to claim 4, wherein the strong reducing gas in S4 is CO and H2Mixing at a ratio of 2-4: 1.
6. The method according to claim 3, wherein the temperature increase step in S3 is performed by: when the temperature is lower than 900 ℃, the heating rate is 12-18 ℃/min, when the temperature is 900-1400 ℃, the heating rate is 4-6 ℃/min, and 1400 ℃ is taken as the heating end point.
7. The method for measuring the slagging property in the strongly reducing atmosphere according to claim 3, wherein said reducing gas inlet pipe and N4 are used2The air inlet pipe flow control program is as follows: when the temperature is lower than 900 ℃, only N is opened2An air inlet pipe, the flow rate of which is controlled to be 80-120mL/min, and when the temperature is 900 ℃ and 1400 ℃, the reducing gas inlet pipe and N are opened simultaneously2An inlet pipe, a reducing gas inlet pipe and N2The flow ratio of the gas inlet pipe is 3-5:1, and the reducing gas and the N are controlled2The total flow rate of (A) is 350-450 mL/min.
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