CN110411791B - A particulate matter collection device for analyzing trace element high temperature enrichment performance - Google Patents
A particulate matter collection device for analyzing trace element high temperature enrichment performance Download PDFInfo
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- CN110411791B CN110411791B CN201910658524.2A CN201910658524A CN110411791B CN 110411791 B CN110411791 B CN 110411791B CN 201910658524 A CN201910658524 A CN 201910658524A CN 110411791 B CN110411791 B CN 110411791B
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- G01N1/00—Sampling; Preparing specimens for investigation
- G01N1/02—Devices for withdrawing samples
- G01N1/22—Devices for withdrawing samples in the gaseous state
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- G01N1/00—Sampling; Preparing specimens for investigation
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- G01N2001/2282—Devices for withdrawing samples in the gaseous state with cooling means
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Abstract
The invention discloses a particulate matter collecting device for analyzing high-temperature enrichment performance of trace elements, which is suitable for collecting ash samples under the high-temperature condition of a high-temperature sedimentation furnace and is used for analyzing the enrichment characteristics of volatile elements (As, Se) and the like in high-temperature ash. The device consists of a short hollow pipe, a long hollow pipe, a high-temperature-resistant fine screen, a base, an ash bucket flange, a filter cylinder, a cooling sleeve and a hearth corundum pipe. The long hollow pipe can be embedded into the short hollow pipe; meanwhile, a high-temperature-resistant fine screen is clamped between the two sections of hollow pipes and is used for collecting ash samples; the base is welded to the long hollow tube, the fixable device remains upright, and gas entering the device is vented. When collecting ash, the device extends into the high temperature zone in the furnace from the bottom of the settling furnace and is fixed at the bottom of the settling furnace. The invention has the advantages that the ash sample can be collected at the temperature of 700-.
Description
Technical Field
The invention belongs to the technical field of heavy metal detection of flue gas, and particularly relates to a particulate matter collecting device for analyzing the high-temperature enrichment performance of trace elements.
Background
Various pollutants which damage the environment can be generated in the coal combustion process, heavy metal trace elements are one of the pollutants, and although the content of the heavy metal trace elements is not large, the heavy metal trace elements enter the atmosphere along with flue gas due to the volatile characteristics (such As Hg, As and Se) of some heavy metal trace elements, so that the environment and human bodies are greatly harmed. The high-temperature ash is collected, the content of the trace heavy metal elements in the ash is measured, the general rule of volatilization of the heavy metal trace elements can be explored, and the method has important significance for controlling the heavy metal trace elements.
In the prior art, the high-temperature ash is collected and the content of trace heavy metal elements in the ash is measured and is usually higher, so that the device capable of sampling at high temperature is designed, and the device has important significance for researching the enrichment characteristic of volatile heavy metal elements in the fly ash and the control method thereof.
Disclosure of Invention
The invention relates to a device for collecting an ash sample at a high temperature, which aims to make up the defect of low ash collecting temperature of the existing sampling device and solve the problem that heavy metal trace elements are re-adsorbed on the surface of particles by gas phase condensation in the process of cooling. By utilizing the device, the high-temperature ash generated in the combustion process of the settling furnace can be collected, so that the enrichment characteristic of heavy metal elements in the high-temperature ash can be accurately analyzed, the high-temperature adsorption mechanism of volatile heavy metals in particles can be researched, and the control method of volatile toxic trace elements can be explored. The device is suitable for collecting ash samples under the high-temperature condition of the laboratory settling furnace, the ash collecting temperature can be controlled to be between 700 and 800 ℃, and the device is a detachable ash collecting device arranged in a hearth.
In order to achieve the purpose, the invention adopts the following technical scheme: a particulate matter collection device for analyzing high temperature enrichment performance of trace elements, comprising:
the cooling sleeve is sleeved on the periphery of the lower end of the hearth corundum tube;
the ash bucket flange is provided with a conical inner cavity, and the filter cylinder is sleeved on the inner periphery of the ash bucket flange;
the bottom end of the inner periphery of the short hollow pipe is provided with an expanded diameter cavity, the inner diameter of the expanded diameter cavity is larger than that of one end of the short hollow pipe, which is far away from the expanded diameter cavity, and the inner periphery of the expanded diameter cavity is in clearance fit with the outer periphery of the long hollow pipe;
the long hollow tube is sleeved in the diameter expanding cavity, and the high-temperature-resistant fine screen is clamped and fixed between the diameter expanding cavity and the top end of the long hollow tube;
the base is welded at the bottom end of the long hollow pipe and is provided with a hollow channel and a conical outer peripheral outline, and the outer peripheral section of the base is matched with the inner periphery of the ash bucket flange;
the short hollow pipe, the high-temperature-resistant fine screen mesh, the long hollow pipe and the base are sequentially assembled and then are arranged in the conical inner cavity of the ash bucket flange, and the conical inner cavity of the ash bucket flange faces the hearth corundum pipe and is fixed with the bottom end of the hearth corundum pipe.
Furthermore, the short hollow pipe, the high-temperature-resistant fine screen and the long hollow pipe are made of high-temperature-resistant materials.
Furthermore, the high-temperature-resistant fine screen is circular, and the paving diameter of the high-temperature-resistant fine screen is larger than the outer diameter of the long hollow pipe.
Further, the mesh number of the high-temperature-resistant fine screen is not less than 800 meshes.
Preferably, the short hollow tube and the long hollow tube are adhered by high-temperature-resistant glue.
Preferably, the bottom end of the ash bucket flange is communicated with the cyclone separator, the condenser, the ash bag dust collector and the induced draft fan in sequence.
Preferably, the cooling sleeve is communicated with a water inlet pipe and a water outlet pipe of the circulating cooling water system.
The invention has the beneficial effects that:
the invention can collect ash samples under the conditions of 700 plus 800 ℃, adopts a high-temperature resistant screen to replace a common fiber filter cartridge, advances the ash interception position to the front of a sampling gun with water cooling or a bottom water cooling disc, and collects bottom ash before the temperature of flue gas is not reduced. Compared with the traditional ash collection method, the method can obtain the bottom ash sample with higher temperature, and overcomes the problem that the trace elements of the gaseous heavy metals in the flue gas are re-adsorbed on the particles in the condensation process. Meanwhile, the device is simple in installation among all accessories, convenient and fast to operate, and the corundum tube can be used by directly extending the device into the hearth.
Drawings
FIG. 1 is a schematic structural diagram of the present invention.
FIG. 2 is a schematic view of the apparatus after it has been placed in the furnace.
Detailed Description
The invention is further described below with reference to the accompanying drawings.
Example 1
Referring to fig. 1, the particulate matter collecting device for analyzing the high-temperature enrichment performance of trace elements comprises a short hollow tube 1, a long hollow tube 2, a high-temperature-resistant fine screen 3, a base 4, an ash bucket flange 6, a filter cylinder 9, a cooling sleeve 7 and a hearth corundum tube 5, wherein the cooling sleeve 7 is sleeved on the periphery of the lower end of the hearth corundum tube 5; the ash bucket flange 6 is provided with a conical inner cavity, and the filter cartridge 9 is sleeved on the inner periphery of the ash bucket flange 6; the bottom end of the inner periphery of the short hollow pipe 1 is provided with an expanding cavity 1.2, the top end of the long hollow pipe 2 is sleeved in the expanding cavity 1.2, the high-temperature-resistant fine screen 3 is clamped and fixed between the expanding cavity 1.2 and the top end of the long hollow pipe 2, the inner diameter of the expanding cavity 1.2 is larger than that of one end 1.1, far away from the expanding cavity, of the short hollow pipe 1, and the inner periphery of the expanding cavity 1.2 is in clearance fit with the outer periphery of the long hollow pipe 2; the base 4 is a hollow conical tube and is welded at the bottom end of the long hollow tube 2.
The particulate matter collection device of this implementation device use as follows: firstly, measuring the sampling temperature in the hearth by using a thermocouple at a position 500-600mm deep from the outlet of the sedimentation furnace to obtain the extension length of the thermocouple when the sampling temperature is above 700 ℃, and ensuring that the device of the embodiment samples at the position above 700 ℃; secondly, the device of the embodiment is connected as shown in fig. 1, the long hollow tube 2 and the short hollow tube 1 are both made of high temperature resistant materials, the length of the long hollow tube 2 is 500-600mm, and the length of the short hollow tube 1 is 50-60 mm; the outer diameter of the short hollow tube 1 is 16mm and is larger than the outer diameter of the long hollow tube 2, the inner diameter of the bottom end of the short hollow tube 1 is the same as the outer diameter of the long hollow tube 2 by 13mm, the inner diameter of the other end of the short hollow tube 1 is the same as the inner diameter of the long hollow tube 2 by 10mm, after the round high-temperature-resistant fine screen 3 is placed in the bottom end of the short hollow tube 1, the specification of the high-temperature-resistant fine screen 3 is 800 meshes, then the long hollow tube 2 is embedded into the short hollow tube 1, the high-temperature-resistant fine screen 3 is fixed, and the paving diameter of the high-temperature-resistant fine screen 3 is slightly larger than the outer diameter of the long hollow tube 2; coating a layer of high-temperature-resistant glue at the joint of the two sections of hollow pipes;
referring to FIG. 2, then, according to the extension length determined in the first step, the connected device is extended into a hearth corundum tube 5 from the outlet of a settling furnace, if the whole length is not enough to reach the determined extension length, a base 4 is welded at the lower end of a long hollow tube 2 to be raised to ensure the sampling temperature, the base 4 is a hollow frustum, a filter cylinder 9 is placed in an ash bucket flange 6, a particulate matter collecting device 10 and the base 4 are placed into the ash bucket flange 6 at the bottom end of the settling furnace to compact the filter cylinder 9, the particulate matter collecting device 10 can enable the device to be upright, a cooling sleeve 7 is sleeved on the periphery of the bottom end of the hearth tube 5, the ash bucket flange 6 is connected with the hearth corundum tube 5 through bolts, the device is fixed in the hearth corundum tube 5, the cooling sleeve 7 is communicated with a circulating cooling water system through a water pipe 8, the deformation of the ash bucket flange 6 caused by high-temperature smoke is prevented, and the filter cylinder 9 in the ash bucket flange 6 is prevented from being ablated by the high-temperature smoke, the bottom end of the ash bucket flange 6 is sequentially communicated with a cyclone separator, a condenser, an ash bag dust remover and an induced draft fan. The filter cartridge 9 is used for filtering particles with the diameter smaller than the pores of the high-temperature-resistant fine screen 3, and prevents the induced draft fan from being blocked during air suction.
After the experiment is finished, the ash bucket flange 8 is disassembled, the high-temperature-resistant fine screen 3 is taken out to collect the first ash sample, and the filter cylinder 9 is taken out to collect the second ash sample.
Comparative example
Experimental study on deposition characteristics of coal ash from east Junjie, Urbusao, Zutai et al and O published in Li2/CO2Experimental study on distribution characteristics of trace elements in fine ash particles during pulverized coal combustion2And after quenching the water-cooled sampling tube, removing particles with the particle size of more than 10 mu m by a cyclone separator, or after quenching and cooling by a bottom water-cooled disc, filtering the solution in a separation ash bucket provided with a filter cylinder, and intercepting bottom ash to obtain an ash sample to be detected.
Comparison of effects
In the experiment, hollyriver lignite is combusted at 1000 ℃ and 1100 ℃, sample ash is collected by an ash collecting device of a comparative example and an ash collecting device listed in example 1 respectively, and the measurement of trace heavy metal is carried out, wherein the sample treatment and heavy metal concentration measurement method refers to the volatilization characteristics and models of high-arsenic lignite and low-arsenic bituminous coal co-combustion arsenic published by Liuhui Min, Wangchun et al, and the measurement is carried out by adopting microwave digestion and hydride atomic fluorescence spectrometry.
Referring to GB/T3058-2008 'determination method for arsenic in coal', the digestion method of the coal sample of the Huolin river lignite is to mix and burn the coal sample and the Aishi agent, dissolve the burned sample with hydrochloric acid, add deionized water to a constant volume of 100ml, and measure. The ash collecting device of the comparative example and the ash collecting device listed in example 1 were used to collect an ash sample, and the ash sample was digested by a SpeedWaveMWS-4 type microwave digestion instrument of Berghof, germany, to obtain the heavy metal content in the coal sample. Weighing 0.1g of solid ash sample, putting the solid ash sample into a digestion tank, sequentially adding 5ml of concentrated nitric acid and 2ml of hydrofluoric acid, digesting according to a coal ash digestion program given by an instrument, adding deionized water after digestion to reach a constant volume of 100ml, and measuring. The digested coal and ash samples were tested for arsenic and selenium concentration in liquid samples using an automated hydride generation atomic fluorescence spectrometer (PSA 10.055Millennium Excalibur, uk). And calculating the mass of the heavy metal in the unit ash sample through calculation. In order to reduce the measurement error, each sample is tested for 3 times, the relative deviation is within +/-10 percent, the data is considered to be valid, QA & QC verification is carried out in the measurement process, and the average value of the 3 valid test data is taken as a test result.
The arsenic and selenium concentration in the detection liquid sample corresponding to the ash sample II is lower than 5ppb, and a measurement result cannot be obtained. Indicating that the heavy metal in the flue gas is almost intercepted by the high-temperature-resistant screen.
The specific result values are as follows:
TABLE 1 concentration of heavy metals in combustion ash of Huolin river lignite settling furnace
From the above, the heavy metal content in the ash sample measured in example 1 is lower than that in the ash sample measured in the comparative example, mainly because the ash sampling method in the comparative example belongs to low temperature sampling, and the ash-containing flue gas enters the sampling tube before entering the sampling tube due to the N sampling tube2And quenching by a water cooling system, the temperature has been reduced to below 100 ℃. Under the condition, the volatilized heavy metal can be rapidly condensed and adsorbed on the surface of particles, so that the heavy metal element content of the ash sample collected by the filter cylinder is higher than that of the ash sample at the outlet of the actual hearth, and the enrichment characteristic and the reaction mechanism of the volatile heavy metal element in the high-temperature ash can be greatly influenced.
Claims (7)
1. A particulate matter collecting device for analyzing high-temperature enrichment performance of trace elements, comprising:
the cooling sleeve is sleeved on the periphery of the lower end of the hearth corundum tube;
the ash bucket flange is provided with a conical inner cavity, and the filter cylinder is sleeved on the inner periphery of the ash bucket flange;
the bottom end of the inner periphery of the short hollow pipe is provided with an expanded diameter cavity, the inner diameter of the expanded diameter cavity is larger than that of one end of the short hollow pipe, which is far away from the expanded diameter cavity, and the inner periphery of the expanded diameter cavity is in clearance fit with the outer periphery of the long hollow pipe;
the long hollow tube is sleeved in the diameter expanding cavity, and the high-temperature-resistant fine screen is clamped and fixed between the diameter expanding cavity and the top end of the long hollow tube;
the base is welded at the bottom end of the long hollow pipe and is provided with a hollow channel and a conical outer peripheral outline, and the outer peripheral section of the base is matched with the inner periphery of the ash bucket flange;
the short hollow pipe, the high-temperature-resistant fine screen mesh, the long hollow pipe and the base are sequentially assembled and then are arranged in the conical inner cavity of the ash bucket flange, and the conical inner cavity of the ash bucket flange faces the hearth corundum pipe and is fixed with the bottom end of the hearth corundum pipe.
2. The particulate collection device of claim 1 wherein the short hollow tube, the high temperature resistant fine screen, and the long hollow tube are made of high temperature resistant material.
3. The particulate matter collecting device according to claim 1, wherein the high temperature resistant fine mesh screen is circular, and the flattened diameter of the high temperature resistant fine mesh screen is larger than the outer diameter of the long hollow tube.
4. The particulate matter collecting device according to claim 1, wherein the high-temperature-resistant fine screen has a mesh number of not less than 800 meshes.
5. The particulate matter collecting device according to claim 1, wherein the short hollow tube and the long hollow tube are bonded together using a high temperature resistant adhesive.
6. The particulate matter collecting device according to claim 1, wherein the bottom end of the ash bucket flange is communicated with a cyclone separator, a condenser, an ash bag dust collector and an induced draft fan in sequence.
7. The particulate collection device of claim 1, wherein the cooling jacket is in communication with an inlet and an outlet of a recirculating cooling water system.
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CN101637668B (en) * | 2009-01-14 | 2011-07-20 | 中山大学 | Device and method for combined use of molecular imprinting solid phase microextraction and hollow fiber liquid phase microextraction, and application thereof |
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CN103113904B (en) * | 2013-03-13 | 2014-03-26 | 上海理工大学 | Experimental device for coal and biomass pyrolysis experiment |
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