JPS6218857B2 - - Google Patents

Description

DETAILED DESCRIPTION OF THE INVENTION The present invention relates to an apparatus for simultaneously measuring ash and sulfur in solid fuels such as coal and coke.

Being able to easily and quickly measure the ash and sulfur content in coal and coke is important for quality control at coal preparation plants and for quality control when coal and coke are used as fuel at power plants, cement plants, steel plants, etc. It is extremely important for management.

Devices that use X-rays or radiation have been known to measure the ash and sulfur content in solid fuels, but they measure ash and total sulfur at the same time, and only combustible sulfur is measured. cannot be directly measured, a calibration curve is required for the measurement, and the measurement cannot be performed unless the sample is kept dry.

Further, even with conventional combustion methods using high-frequency furnaces and silicon carbide furnaces, only combustible sulfur cannot be directly measured, and non-combustible sulfur must be measured after preparing ash in advance.

The present invention improves such existing measurement technology, and when measuring the ash and sulfur content in solid fuels such as coal and coke, it is possible to simultaneously measure the ash content and sulfur content, and moreover, it is possible to simultaneously measure the ash content and sulfur content. The present invention aims to provide a measuring device that can determine the combustible sulfur content from the same measurement sample.

In order to achieve this purpose, the measuring device of the present invention includes a gas supply ring for supplying oxygen gas placed on the top of an electronic balance, and an infrared heating furnace surrounding the gas supply ring. The protective tube is integrated and mounted so as to be able to be raised and lowered, and within the protective tube, a support tube with a sample holder at the upper end is set upright on the weight sensing table of the electronic balance, and the gas of the gas supply ring is The upper end of the protection tube to which oxygen gas is supplied from the outlet is connected to a suction pump, and a temperature regulator is capable of controlling the infrared heating furnace to a temperature at which combustible sulfur and non-combustible sulfur in the sample each become sulfur dioxide gas. configured by connecting to.

A measuring device with such a configuration uses an infrared heating furnace to rapidly burn and ash coal or coke in an oxygen stream, and measures the ash content from the change in weight, and also measures the ash content from the amount of sulfur dioxide gas generated. The sulfur content is measured, and when performing such measurements, by setting the ashing temperature at 800 to 900°C and measuring the sulfur dioxide gas generated at that time, the combustible sulfur content can be calculated, and the combustion temperature can also be measured. The non-combustible sulfur content can be calculated by raising the temperature to 1300-1400℃ and measuring the sulfur dioxide gas generated at that time.

Therefore, according to the measuring device of the present invention, ash content and sulfur content can be measured simultaneously with simple operation using a simple device, and combustible sulfur content and non-combustible sulfur content can be determined from the same measurement sample. .

Embodiments of the present invention will be described in detail below with reference to the drawings.

FIG. 1 schematically shows the configuration of the entire apparatus according to the present invention, where 1 indicates the measuring apparatus main body, and 2 indicates a temperature regulator 2. As shown in FIG. The measuring device main body 1 has a second
As shown in detail in the figure, a gas supply ring 5 is placed on the top of the electronic balance 3 through a plate-shaped rubber gasket 4, and a rubber gasket 6 is placed on the outer circumferential step 5a of the gas supply ring 5. A cooling ring 9 is mounted to connect the infrared heating furnace 7 and the protection tube 8 made of quartz glass. Further, a support tube 11 made of quartz glass and having a sample holder 12 made of platinum attached to its upper end is erected on the weight sensing table 3a of the electronic balance 3 via a joint fitting 10. The support tube 11 may be made of alumina.

The gas supply ring 5 has a gas inlet 1 on one side of which oxygen gas is supplied from a cylinder (not shown).
3, provided with a gas outlet 14 on the upper surface thereof, and provided with a gas outlet 15 that opens on the outer circumferential step 5a side to create an airflow along the inner wall of the protective tube 8, and further provides support for the inner circumference thereof. A gas outlet 16 for creating an airflow along the outer wall of the support tube 11 is provided in the tube insertion hole 5b. The gas outlet 15 is
The volatile matter in the coal becomes soot at the beginning of the measurement and tends to adhere to the inner wall of the protection tube, so this is to prevent that adhesion, and the gas outlet 16 prevents the combustion gas from flowing back into the balance section. It is something to do. A spiral cooling pipe 17 provided within the gas supply ring 5 prevents heat transfer to the electronic balance 3, and is provided with a water inlet 18 and a water outlet 19 led out of the ring 5.

The cooling ring 9 prevents heat transfer to the electronic balance 3, is provided with a cooling water inlet 20 and a cooling water outlet 21, and is integrally fixed to the infrared heating furnace 7 by a connecting fitting 22. A protection tube 8 is fitted inside. The infrared heating furnace 7, protection tube 8, and cooling ring 9 integrated as described above are movable up and down along the support 23 shown in FIG. The structure is such that the infrared heating furnace 7, protection tube 8, etc. can be set simply by unloading the device. This configuration is advantageous in that it is not only simple and easy to operate, but also easy to repeat measurements.

As described above, the gasket 4 is provided between the top of the electronic balance 3 and the gas supply ring 5, and the gasket 6 is provided between the gas supply ring 5 and the cooling ring 9.
However, it is not necessary to obtain complete airtightness with these gaskets 4 and 6, and the amount of oxygen gas supplied and the suction pump 24 connected to the protection tube are adjusted so that the inside of the protection tube 8 has a positive pressure. If the suction amount shown in FIG. 1 is set in advance, the inflow of impure gas can be prevented.

The sample holder 12 attached to the upper end of the supporter 11 has a sample plate 25 placed therein.
It is formed into a cylindrical shape having a height two to three times that of the sample dish 25. Therefore, even if some of the sample scatters from the sample dish 25, it can be captured in the sample holder 12, so that the measurement can be continued.

As shown in detail in FIG. 3, the auxiliary fuel furnace 30 fixed to the upper part of the infrared heating furnace 7 is constituted by a Kanthal wire furnace or a nichrome wire furnace, and the heating element 31 is connected to a small diameter part in the upper part of the protection tube 8. A refractory castable 32 disposed around the heat generating element 8a and housing the heating element 31 is attached to a furnace cover 34 filled with an insulating refractory wool 33, and a thermocouple 35 reaching the surface of the protective tube 8 is inserted. The auxiliary combustion furnace 30 is
The temperature is always maintained at 800 to 1200°C, preferably about 800 to 1000°C.

The heat-resistant filler 36 filled in the small-diameter portion 8a at the top of the protection tube is made of platinum mesh, platinum wool, quartz glass wool, alumina wool, etc., and is designed to completely burn out the volatile matter generated in the initial stage of combustion. It was established. A connecting tube 37 for leading to the suction pump 24 is connected to the tip of the protective tube 8 via a sliding portion 38 (FIG. 1).

A platinum soaking tube 39 (thickness 0.2
~0.5mm) easily absorbs infrared rays and has high thermal conductivity, so even if soot generated during temperature rise adheres to the top of the protection tube, the soot will be completely combusted when the sulfur content measurement temperature is reached. It is for. That is, the temperature gap between the infrared heating furnace 7 and the auxiliary combustion furnace 30 is eliminated.

The temperature controller 2 detects the temperature of each of the infrared heating furnace 7 and the auxiliary combustion furnace by a thermocouple (not shown) placed near the sample and a thermocouple 35 installed in the auxiliary combustion furnace 30. It is also possible to set a temperature increase program for the infrared heating furnace 7 in advance and perform control according to the program.

In the above-mentioned measuring device, the gas supply ring 5, the cooling ring 9, the spiral cooling pipe 17, and the covers and connecting fittings of each part are preferably made of stainless steel.

Next, a measurement method using the above measuring device will be explained.

Prior to measurement, the infrared heating furnace 7, protection tube 8, etc. were moved upward, and the auxiliary combustion furnace 30 was
Set the temperature to 1050℃. In this state, electronic balance 3
the empty sample plate 2 on the sample holder 12.
5 and after erasing the tare, a sample of coal or coke (0.2 to 1 g) is spread on the sample tray 25 and placed on the sample holder 12. This allows the amount of sample to be determined immediately.

Next, the infrared heating furnace 7, protection tube 8, etc. are lowered and set at the required positions (the state shown in Figure 2), and oxygen gas is flowed at a flow rate of 300 to 1000 ml/min.
The suction pump 24 sucks in an amount of about 30 to 50 ml/min less than the supplied amount, and a switch is turned on to raise the temperature in the infrared heating furnace 7 according to a preset program. The heating rate is 100 from room temperature to 500℃.
-200°C/min, and above that, 200-500°C/min is appropriate. Furthermore, cooling water is allowed to flow through the cooling ring 9 and the spiral cooling pipe 17.

When the temperature reaches the ashing temperature (800 to 900°C) due to the temperature increase, the temperature is maintained for 1 to 3 minutes, and then the oxygen supply is stopped and the suction pump 24 is also stopped. At this point, if the weight is measured using an electronic balance, the weight of the ash can be determined. In addition, the gas sucked by the suction pump 24 is collected in a gas absorption bottle, and the amount of sulfur dioxide gas is measured by titration, or the amount is measured by passing it through an infrared sulfur dioxide gas detector. The amount of combustible sulfur is determined.

After that, while further oxygen is flowing, the suction pump 2
The amount of non-combustible sulfur can be determined by raising the temperature to 1300-1400℃ while performing suction according to step 4, holding it for 1-2 minutes, and then measuring sulfur dioxide gas.
Further, the total sulfur content can also be determined as the sum of the above two sulfur content.

In order to carry out the next measurement, the infrared heating furnace 7 is moved upward to rapidly cool it down, and the operations from tare erasing the sample plate are repeated.

In general, coal has large fluctuations in moisture content, so it is preferable to obtain measured values on an anhydrous basis, but if this is necessary, preheat the sample at 100 to 250°C.
The moisture content can be measured from the weight change during that time, and at the same time, the ash content and sulfur content on an anhydrous basis can be measured.

[Brief explanation of the drawing]

FIG. 1 is a schematic configuration diagram showing the entire embodiment of the present invention, and FIGS. 2 and 3 are enlarged sectional views of the main parts thereof. 2...Temperature controller, 3...Electronic balance, 3a...
Weight sensing stand, 5... Gas supply ring, 7... Infrared heating furnace, 8... Protection tube, 11... Support tube, 12
...Sample holder, 14, 15, 16...Gas outlet.

Claims (1)

[Claims] 1 A gas supply ring for supplying oxygen gas is placed on the top of the electronic balance, and an infrared heating furnace and a protective tube surrounded by it are integrated and placed on this gas supply ring so that they can be raised and lowered. In the protective tube, a support tube with a sample holder at the upper end is installed on the weight sensing table of the electronic balance, and the upper end of the protective tube is supplied with oxygen gas from the gas outlet of the gas supply ring. is connected to a suction pump, and the infrared heating furnace is connected to a temperature controller capable of controlling the temperature at which combustible sulfur and non-combustible sulfur in the sample each become sulfur dioxide gas. Sulfur content measuring device.