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.
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
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.