CN110702560A - Device and method for measuring viscosity-temperature characteristics of coal ash slag in presence of high-temperature steam - Google Patents
Device and method for measuring viscosity-temperature characteristics of coal ash slag in presence of high-temperature steam Download PDFInfo
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- CN110702560A CN110702560A CN201910970736.4A CN201910970736A CN110702560A CN 110702560 A CN110702560 A CN 110702560A CN 201910970736 A CN201910970736 A CN 201910970736A CN 110702560 A CN110702560 A CN 110702560A
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Abstract
The invention relates to the field of coal gasification, in particular to a device for measuring the viscosity-temperature characteristic of coal ash slag in the presence of high-temperature steam. The invention has the beneficial effects that: the viscosity-temperature characteristic of the coal ash slag in the presence of high-temperature steam can be accurately measured, the measurement precision is high, the operation is simple, and the viscosity-temperature characteristic of the coal ash slag in the presence of steam in the coal gasification process can be accurately reflected.
Description
Technical Field
The invention relates to the field of coal gasification, in particular to a device and a method for measuring viscosity-temperature characteristics of coal ash slag in the presence of high-temperature steam.
Background
Entrained flow gasification has the technical advantages of high temperature, high pressure, high carbon conversion rate, wide coal adaptability, easiness in large-scale production and the like, and becomes a preferred coal gasification technology. Because the operating temperature of the entrained-flow bed gasification furnace is generally higher than 1300 ℃, and the mineral substances in the coal are melted into liquid slag under the condition, the entrained-flow bed gasification furnace is a slag tapping gasification furnace, and the smooth discharge of the slag is the key for ensuring the long-period safe and stable operation of the gasification furnace.
The viscosity-temperature characteristic of the slag is the most important parameter for ensuring the slag tapping process of the entrained flow gasifier, taking Shell (Shell) as an example, the viscosity of the slag at the slag tapping temperature should be 2.5 ~ 25 pas, and the corresponding temperature range should be 1300 ~ 1500 ℃ (slag tapping operation temperature window), meanwhile, since the gasification operation temperature of the entrained flow gasifier is generally higher than the slag tapping temperature of 100 ~ 150 ℃, the temperature corresponding to the slag viscosity of 25 pas should be lower than 1400 ℃CV) And the slag should be vitreous slag.
Atmosphere is an important factor influencing the viscosity-temperature characteristics of the molten slag, and the gas in the entrained-flow bed gasification furnace mainly comprises CO and H2、CO2And H2And O. Long-term research and industrial practice have demonstrated that CO and H are reduced with the atmosphere2The increase of the content and the decrease of the viscosity of the slag at the same temperature are caused by the coal ash slagFe2O3Is reduced to Fe2+And Fe in coal ash2O3The higher the content of (b), the more significant the influence of the atmosphere on the viscosity-temperature characteristics of the slag.
The entrained-flow bed gasification is divided into two types of pulverized coal gasification and coal water slurry gasification according to different feeding modes, wherein the coal water slurry is used as the raw material to feed H in the entrained-flow bed gasification furnace gas2The content of O can reach about 20 percent, but at present, no device and method for measuring the viscosity-temperature characteristic of the coal ash slag in the presence of high-temperature steam exist, so that the influence of the steam in the gas of the entrained flow gasifier on the slag tapping process cannot be known.
Disclosure of Invention
The technical problem to be solved by the invention is as follows: aiming at the defects of the existing coal ash slag viscosity-temperature characteristic measuring technology, the device and the method for measuring the coal ash slag viscosity-temperature characteristic in the presence of high-temperature water vapor are provided.
The technical scheme adopted by the invention is as follows: a device for measuring the viscosity temperature characteristic of coal ash slag in the presence of high-temperature steam is characterized in that a support frame (16) is fixed on the ground, a first lifting device (6) is installed on the support frame (16), a fixed platform (8) is installed on the first lifting device (6), a second lifting device (22) is installed above the fixed platform (8), a rheometer (5) is fixed on the second lifting device (22), a furnace tube (11) is installed below the fixed platform (8), a support (12) prepared by coiling a Perkin tube is installed in the furnace tube (11), a crucible (15) is installed below the support (12), a gas channel (9) is arranged at the upper part of the furnace tube (11), a thermocouple (23) is arranged outside the crucible in the furnace tube (11), two ends of the Perkin tube are connected with a cold medium inlet and outlet, an inlet of the gas channel (9) is connected with a water vapor generator (4), a rotating rod through hole is arranged at the position, between the furnace tube (11, lifting hook (7) of rheometer (5) are connected bull stick (10), it is gapped between bull stick through-hole and bull stick (10), rotor (14) of bull stick (10) bottom is located inside crucible (15), the lower part of boiler tube (11) is in the inside cavity of box-like furnace body (17) of insulation material (18) preparation, install heating device (19) in the inside cavity of furnace body (17), water vapor generator (4) is connected with water injection pump (3) and gas cylinder (20), refrigerant body control valve, thermocouple (23), heating device (19) electric signal connection temperature control module (2), rheometer (5), first elevating gear (6), computer (1) is connected in second elevating gear (22).
A protective cover (21) is arranged on the outer side of the rheometer (5), the protective cover (21) is fixed on the fixed platform (8), and the second lifting device (22) and the rheometer (5) are both arranged in the protective cover (21).
The support (12) is a cylindrical barrier bar support formed by coiling a hollow platinum tube with an opening at the upper part and the inside, and the crucible (15) is fixed below the support (12) and is positioned in the support.
The rotor is made of corundum or platinum; the material of the rotating rod is corundum, the material of the crucible is corundum or platinum, and the water injection pump is a trace water injection pump.
The device is adopted and comprises the following steps:
(1) crushing the coal ash slag, and placing the crushed coal ash slag in a crucible (15);
(2) the temperature of the furnace tube (11) is controlled to rise through the temperature control module (2);
(3) after the temperature of a thermocouple (23) in the furnace tube (11) reaches 800 ℃, starting a water injection pump (3) and a water vapor generator (4), and opening the carrying gas in the gas cylinder (20);
(4) introducing mixed gas carrying gas and water vapor into the furnace tube, keeping the mixed gas flowing, continuously heating to heat the thermocouple (23) to 1600 +/-30 ℃, forming slag in the crucible (15), and keeping the temperature for 20min or more;
(5) controlling the temperature in the furnace tube (11) to be reduced through the temperature control module (2), continuously testing the viscosity of the molten slag in the temperature reduction process, and collecting analysis data until the torque exceeds the measuring range of the rheometer or the viscosity value exceeds 300 Pa & s;
(6) and (3) obtaining a viscosity-temperature curve of the coal ash slag according to the viscosity values of the coal ash slag at different temperatures measured by the rheometer (5), and determining the viscosity-temperature characteristic of the coal ash slag in the presence of high-temperature steam.
In the step (3), the carrier gas is one or more of non-reaction gas, reducing gas and oxidizing gas, wherein the non-reaction gas is Ar and N2The reducing gas is CO + CO2 and N2+ H2, and the oxidizing gas is air.
In the step (4), the volume fraction of the water vapor in the mixed gas is 5% ~ 30%.
In the step (5), the temperature reduction process of the rheometer (5) is continuous procedure temperature reduction.
The invention has the beneficial effects that: the viscosity-temperature characteristic of the coal ash slag in the presence of high-temperature steam can be accurately measured, the measurement precision is high, the operation is simple, and the viscosity-temperature characteristic of the coal ash slag in the presence of steam in the coal gasification process can be accurately reflected.
Drawings
FIG. 1 is a schematic diagram of the structure of the apparatus of the present invention;
FIG. 2 is a bottom view of the interior of the furnace tube;
the device comprises a computer 1, a computer 2, a temperature control module 3, a water injection pump 4, a water vapor generator 5, a rheometer 6, a first lifting device 7, a lifting hook 8, a fixed platform 9, a gas channel 10, a rotating rod 11, a furnace tube 12, a support 13, coal ash or coal ash slag 14, a rotor 15, a crucible 16, a support frame 17, a furnace body 18, a heat insulation material 19, a heating device 20, a gas cylinder 21, a protective cover 22, a second lifting device 23 and a thermocouple;
FIG. 3 is a slag viscosity temperature curve of coal ash in example 1 of the present invention with Ar, Ar +10% steam, Ar +20% steam, and Ar +30% steam;
FIG. 4 is a slag viscosity-temperature curve of coal ash in example 2 of the present invention with Ar, Ar +10% steam, Ar +20% steam, and Ar +30% steam.
Detailed Description
Example 1
As shown in FIG. 1, a device for measuring the viscous temperature characteristics of coal ash slag in the presence of high-temperature steam, wherein a support frame 16 is fixed on the ground, a first lifting device 6 is installed on the support frame 16, a fixed platform 8 is installed on the first lifting device 6, a second lifting device 22 is installed above the fixed platform 8, the lifting devices are all electric screw lifting devices in the embodiment, a rheometer 5 is fixed on the second lifting device 22, a furnace tube 11 is installed below the fixed platform 8, a support 12 prepared by coiling a Perkin tube is installed in the furnace tube 11, a crucible 15 is installed below the support 12, the crucible 15 is not contacted with the furnace tube 11, a gas channel 9 is arranged at the upper part of the furnace tube 11, the gas channel 9 comprises a gas inlet and a gas outlet, a thermocouple 23 is arranged outside the crucible in the furnace tube 11, two ends of the Perkin tube are connected with a cold medium generator, the inlet and the outlet of the gas channel 9 are connected with a steam generator 4, a rotating rod, a lifting hook 7 of a rheometer 5 is connected with a rotating rod 10, a gap is reserved between a rotating rod through hole and the rotating rod 10, a rotor 14 at the bottom of the rotating rod 10 is located inside a crucible 15, the lower part of a furnace tube 11 is located in a cavity inside a box-shaped furnace body 17 made of heat insulation materials 18, a heating device 19 is installed in the cavity inside the furnace body 17, a water injection pump 3 and a gas cylinder 20 are connected with a water vapor generator (4), a refrigerant body control valve, a thermocouple 23 and the heating device 19 are in electric signal connection with a temperature control module 2, and the temperature control module 2, the rheometer 5, a first lifting device 6 and a second lifting device 22 are connected with a computer. The water injection pump 3 is connected with a water source, the heating device 19 is an electric heating wire heating device, the cold medium is water or water vapor, and the temperature control module 2 is software or a chip.
A protective cover 21 is arranged outside the rheometer 5, the protective cover 21 is fixed on the fixed platform 8, and the second lifting device 22 and the rheometer (5) are both arranged in the protective cover 21.
The support 12 is a cylindrical barrier bar support formed by coiling a hollow platinum tube with an opening at the upper part and the inside, and the crucible 15 is fixed below the support 12 and is positioned in the support.
Crushing the coal ash slag, and placing the crushed coal ash slag in a crucible 15;
the temperature of the furnace tube 11 is controlled to rise through the temperature control module 2, and the heating device 19 provides the temperature rise;
after the temperature of the thermocouple 23 in the furnace tube 11 reaches 800 ℃, starting the water injection pump 3 and the water vapor generator 4, and starting the carrying gas (Ar in the embodiment) in the gas cylinder 20;
introducing mixed gas carrying gas and water vapor into the furnace tube, keeping the mixed gas flowing, continuously heating to heat the thermocouple 23 to 1600 +/-30 ℃, forming slag in the crucible 15, and keeping the temperature for 20min or more;
controlling the temperature in the furnace tube 11 to be reduced through the temperature control module 2, continuously testing the viscosity of the molten slag in the temperature reduction process, and collecting analysis data until the torque exceeds the measuring range of the rheometer or the viscosity value exceeds 300 Pa & s;
and obtaining a viscosity-temperature curve of the coal ash slag according to the viscosity values of the coal ash slag at different temperatures measured by the rheometer 5, and determining the viscosity-temperature characteristic of the coal ash slag in the presence of high-temperature steam.
The carrying gas for the viscosity-temperature characteristic test is argon; the volume fraction of the water vapor in the mixed gas of the water vapor and the carrier gas is 0%, 10%, 20% and 30%; the cooling rate of the rheometer test in the cooling process is 1 ℃/min.
The components of the slag sample used are shown in table 1;
TABLE 1 (wt%)
| SiO2 | Al2O3 | Fe2O3 | CaO | |
| Coal ash 1 | 37.72 | 37.72 | 11.74 | 12.82 |
FIG. 3 shows the viscosity-temperature curves of the fly ash slag under Ar, Ar +10% steam, Ar +20% steam and Ar +30% steam conditions, measured by the above method; as can be seen from the figure: as the percentage of water vapor content in the atmosphere increases, the viscosity of the slag increases slightly at the same temperature; the increase of the water vapor content percentage in the atmosphere does not change the type of the slag, the viscosity of the slag is rapidly increased when the temperature is reduced to the critical viscosity temperature in the cooling process of the slag, the characteristics of the crystallized slag are presented, but the increase of the water vapor content percentage in the atmosphere causes the increase of the critical viscosity temperature, and the water vapor is beneficial to the formation of the crystallized slag.
Example 2
The difference from the embodiment 1 is that: the slag sample compositions used are shown in table 2.
TABLE 2 (wt%)
| SiO2 | Al2O3 | Fe2O3 | CaO | |
| Coal ash 2 | 50.29 | 25.15 | 11.74 | 12.82 |
FIG. 4 shows the viscosity-temperature curves of the fly ash slag under Ar, Ar +10% steam, Ar +20% steam and Ar +30% steam conditions, measured by the above method; as can be seen from the figure: as the percentage of water vapor content in the atmosphere increases, the viscosity of the slag increases slightly at the same temperature; the increase of the water vapor content percentage in the atmosphere does not change the type of the molten slag, the viscosity of the molten slag is rapidly increased when the temperature of the molten slag is reduced to the critical viscosity temperature in the cooling process, the characteristics of the crystallized slag are presented, the increase of the water vapor content percentage in the atmosphere causes the increase of the critical viscosity temperature, the water vapor is beneficial to the formation of the crystallized slag, and particularly, the critical viscosity temperature is obviously increased when the water vapor content percentage reaches 30%.
Claims (7)
1. A device for measuring the viscosity-temperature characteristics of coal ash slag in the presence of high-temperature steam is characterized in that: the support frame (16) is fixed on the ground, a first lifting device (6) is installed on the support frame (16), a fixed platform (8) is installed on the first lifting device (6), a second lifting device (22) is installed above the fixed platform (8), the rheometer (5) is fixed on the second lifting device (22), a furnace tube (11) is installed below the fixed platform (8), a support (12) prepared by coiling a Peltier metal tube is installed in the furnace tube (11), a crucible (15) is installed below the support (12), a gas channel (9) is arranged on the upper portion of the furnace tube (11), a thermocouple (23) is arranged outside the crucible inside the furnace tube (11), cold medium inlets and outlets are connected to two ends of the Peltier metal tube, an inlet of the gas channel (9) is connected with the water vapor generator (4), a rotating rod through hole is arranged at a position, between the furnace tube (11) and the rheometer (5), a lifting hook (7) of the rheometer (5) is connected, a gap is reserved between the rotating rod through hole and the rotating rod (10), a rotor (14) at the bottom of the rotating rod (10) is located inside a crucible (15), the lower part of a furnace tube (11) is located in a cavity inside a box-shaped furnace body (17) prepared from heat insulation materials (18), a heating device (19) is installed in the cavity inside the furnace body (17), a water injection pump (3) and a gas cylinder (20) are connected with a water vapor generator (4), a refrigerant body control valve, a thermocouple (23), the heating device (19) is connected with a temperature control module (2) through electric signals, the temperature control module (2), a rheometer (5), a first lifting device (6) and a second lifting device (22) are connected with a computer (1).
2. The apparatus according to claim 1, wherein the viscosity-temperature characteristics of the fly ash slag in the presence of the high-temperature steam are determined by: a protective cover (21) is arranged on the outer side of the rheometer (5), the protective cover (21) is fixed on the fixed platform (8), and the second lifting device (22) and the rheometer (5) are both arranged in the protective cover (21).
3. The apparatus according to claim 1, wherein the viscosity-temperature characteristics of the fly ash slag in the presence of the high-temperature steam are determined by: the support (12) is a cylindrical barrier bar support formed by coiling a hollow platinum tube with an opening at the upper part and the inside, and the crucible (15) is fixed below the support (12) and is positioned in the support.
4. A method for measuring the viscosity-temperature characteristics of coal ash slag in the presence of high-temperature steam is characterized by comprising the following steps: the method of claim 1, comprising the steps of:
(1) crushing the coal ash slag, and placing the crushed coal ash slag in a crucible (15);
(2) the temperature of the furnace tube (11) is controlled to rise through the temperature control module (2);
(3) after the temperature of a thermocouple (23) in the furnace tube (11) reaches 800 ℃, starting a water injection pump (3) and a water vapor generator (4), and opening the carrying gas in the gas cylinder (20);
(4) introducing mixed gas carrying gas and water vapor into the furnace tube, keeping the mixed gas flowing, continuously heating to heat the thermocouple (23) to 1600 +/-30 ℃, forming slag in the crucible (15), and keeping the temperature for 20min or more;
(5) controlling the temperature in the furnace tube (11) to be reduced through the temperature control module (2), continuously testing the viscosity of the molten slag in the temperature reduction process, and collecting analysis data until the torque exceeds the measuring range of the rheometer or the viscosity value exceeds 300 Pa & s;
(6) and (3) obtaining a viscosity-temperature curve of the coal ash slag according to the viscosity values of the coal ash slag at different temperatures measured by the rheometer (5), and determining the viscosity-temperature characteristic of the coal ash slag in the presence of high-temperature steam.
5. The method for determining the viscosity-temperature characteristics of coal ash slag in the presence of high temperature steam as claimed in claim 4, wherein: in the step (3), the carrier gas is one or more of non-reaction gas, reducing gas and oxidizing gas, wherein the non-reaction gas is Ar and N2The reducing gas is CO + CO2 and N2+ H2, and the oxidizing gas is air.
6. The method for determining the viscosity-temperature characteristics of the coal ash slag in the presence of high-temperature water vapor is characterized in that in the step (4), the volume fraction of the water vapor in the mixed gas is 5% ~ 30%.
7. The method for determining the viscosity-temperature characteristics of coal ash slag in the presence of high temperature steam as claimed in claim 4, wherein: in the step (5), the temperature reduction process of the rheometer (5) is continuous procedure temperature reduction.
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Cited By (1)
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| CN112857959A (en) * | 2021-01-21 | 2021-05-28 | 中国科学院山西煤炭化学研究所 | Preparation device and preparation method of coal ash slag sample |
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