CN113984459A - Method and device for measuring ammonia release in preparation process of magnesium slag and fly ash-based filling paste - Google Patents
Method and device for measuring ammonia release in preparation process of magnesium slag and fly ash-based filling paste Download PDFInfo
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Abstract
A device for measuring ammonia release in the process of preparing magnesium slag and fly ash based filling paste comprises a negative pressure mixing tank body for preparing the filling paste, wherein the negative pressure mixing tank body is connected with a feeding pipe for feeding materials, an air suction interface of the negative pressure mixing tank body is connected with an air suction device through a pipeline, the air suction device is used for sucking air to form negative pressure in the negative pressure mixing tank body and take away ammonia gas volatilized from a liquid phase in the preparation process during air suction, an air outlet of the air suction device is connected with an adsorption column to fix the ammonia gas in an adsorbent, and ammonia release characteristics in the process of preparing the filling paste are obtained by detecting the ammonia nitrogen concentration of the adsorbent. The invention avoids the phenomenon that the paste body is hydrated by adding water to release ammonia gas when the preparation tank is not closed, and can send the air containing the released ammonia gas into the adsorption column through a pipeline, so that the determination is more convenient and simpler, and the accuracy is improved. The method makes correct judgment on underground filling work based on the ammonia gas release rule, and has important guiding significance on underground safe mining.
Description
Technical Field
The invention belongs to the technical field of coal mining, and particularly relates to a method and a device for measuring ammonia release in a preparation process of magnesium slag and fly ash-based filling paste.
Background
The fly ash is the main solid waste discharged by a coal-fired power plant and consists of two parts of fine ash and boiler bottom slag which are captured from flue gas generated after coal combustion, and the discharge mass ratio of the fine ash to the boiler bottom slag is about 3: 1. With the continuous improvement of the emission standard of the waste gas of the coal-fired boiler, reducing agents (liquid ammonia or urea) need to be sprayed into the flue gas in the process of denitration of the boiler flue gas by adopting a Selective Catalytic Reduction (SCR) method and a selective non-catalytic reduction (SNCR) method, and excessive reducing agents are often added for guaranteeing the denitration effect. SO that unreacted ammonia gas and SO in the flue gas3Chemical reaction is carried out to generate ammonium salt (NH)4HSO4And (NH)4)2SO4) Remains in the fly ash.
The fly ash is used as a byproduct of a coal-fired power plant, and a main utilization way of the fly ash at present is to produce building materials, such as concrete as an additive, but the fly ash is too far away from the market, the transportation cost is high, and the building industry is saturated, so that the fly ash has a limit on a disposal way of the fly ash used as a building material raw material. The current common disposal is in situ landfill. But the absorption capacity is limited, and a large amount of fly ash cannot be safely treated. Solid wastes such as fly ash and the like are used as raw materials in the coal filling and mining process and are mixed according to a certain proportion to prepare paste to be filled into a goaf, so that the coal pressing problem of 'three lower' (under a building, under a railway and under a water body) is solved, the parallel operation of filling and mining is realized, the ground settlement control is completed, and the aim of green mining is fulfilled; meanwhile, the technical problem of ash storage of the power plant can be solved, the pollution of the fly ash to the ground environment is reduced, and the effect of preventing coal spontaneous combustion is achieved.
With the continuous and intensive research, the denitration fly ash problem is frequently found in some projects, most prominently, the ammonium salt in the fly ash reacts in the alkaline environment of cement hydration to generate ammonia gas, the ammonia gas is released more in the stirring process, and the discomfort such as dizziness, vomit and the like of operators can be caused seriously, so that the new problem of the denitration fly ash in the application becomes a research hotspot of cement concrete profession for two years. The coal ash is used as a main material for mine filling, the using amount of the coal ash is far larger than that of the coal ash in concrete, residual ammonia in the denitration coal ash releases ammonia due to hydration reaction, and the residual ammonia escapes from the underground closed space, so that the body health of operating personnel and the use safety of industrial equipment are seriously influenced.
Therefore, solving the adverse effect of ammonia gas release of the fly ash filling paste has important significance for realizing safe underground filling of the fly ash paste, and mastering the ammonia gas release rule is the basis for solving the problems.
At present, no device for collecting and measuring the ammonia gas release amount in the stirring process exists, and the structure of the existing ammonia gas collecting device is too complicated, so that multi-part ammonia gas collection and measurement are needed. Therefore, aiming at weak links in the research of the existing ammonia gas release and collection device, the ammonia gas release amount of the paste in the stirring process needs to be measured simply and easily, the ammonia gas release rule of the fly ash paste is proved, and a reduction and control measure is found based on the ammonia gas release rule, so that the method is close to the green and safe mining concept and is of great importance.
Disclosure of Invention
In order to solve the problem of collecting and measuring ammonia released by the filling paste, the invention aims to provide a method and a device for measuring ammonia release in the preparation process of the magnesium slag and fly ash-based filling paste, aims to enable the filling paste to be in a stirred state, collects and measures ammonia dissipated by the filling paste, researches and analyzes the ammonia release rule of the large-proportion magnesium slag and fly ash-based filling paste, and provides a basis for guiding and solving the environmental problem of the large-proportion magnesium slag and fly ash-based filling paste in the application process of high-efficiency mining of coal mines.
In order to achieve the purpose, the invention adopts the technical scheme that:
a device for measuring ammonia release in the process of preparing magnesium slag and fly ash based filling paste comprises a negative pressure mixing tank body for preparing the filling paste, wherein the negative pressure mixing tank body is connected with a feeding pipe for feeding materials, an air suction port of the negative pressure mixing tank body is connected with an air suction device through a pipeline, the air suction device is used for sucking air to form negative pressure in the negative pressure mixing tank body and take away ammonia gas volatilized from a liquid phase in the preparation process during air suction, an air outlet of the air suction device is connected with an adsorption column to fix the ammonia gas in an adsorbent, and ammonia release characteristics in the process of preparing the filling paste are obtained by detecting the ammonia nitrogen concentration of the adsorbent.
Preferably, the upper part of the negative pressure mixing tank body is provided with a detachable cover plate, and the feeding pipe and the air exhaust interface are both arranged on the cover plate.
Preferably, the top end of the feeding pipe is of a bell mouth structure, and the air exhaust interface is provided with a filter disc.
Preferably, a stirring motor is fixed on the cover plate, the output of the stirring motor is connected with a stirring shaft with paddle type blades in the tank, and a regulating valve and a gas flowmeter are arranged on the pipeline.
Preferably, the bottom of the adsorption column is provided with a gas release device, an exhaust port of the air extraction device is connected with the gas release device, and the gas containing ammonia enters the adsorption column in a bubble form and is subjected to mass transfer exchange with the adsorbent in the rising process.
Preferably, the air extraction device is an air extraction pump with the flow rate of 10-20L/min and the vacuum degree of-90 Pa, and the gas release device is an aeration head with the height of 3cm and the diameter of 1.9 cm.
The invention also provides a determination method of a determination device based on ammonia release in the preparation process of the magnesium slag and fly ash-based filling paste, which comprises the following steps:
firstly, adding paste preparation water with a fixed volume into a negative pressure mixing tank body through an adding pipe according to the filling paste proportion;
then, starting an air extraction device to pump the gas in the negative pressure mixing tank into the adsorption column, and maintaining the opening state of the air extraction device;
then, adding a mixed material formed according to the proportion of the filling paste material into a negative pressure mixing tank body through a feeding pipe, and uniformly stirring the mixed material and water, wherein the mixed material comprises magnesium slag or fly ash, aggregate and an additive;
and finally, continuously detecting the ammonia nitrogen concentration in the adsorbent in the adsorption column, and converting the released ammonia amount.
Preferably, the air exhaust device is set to have the flow rate of 10-20L/min and the vacuum degree of-90 Pa.
Preferably, the adsorbent is dilute sulfuric acid with a concentration of 0.1 mol/L.
Preferably, the amount of ammonia released is obtained by:
get V2Adding a mL adsorbent into a 50mL colorimetric tube, diluting to a marked line, adding 1.0mL potassium sodium tartrate solution, uniformly mixing, adding 1.5mL nano reagent, uniformly mixing, standing for 10min, measuring absorbance at a wavelength of 420nm by using a cuvette with an optical path of 20nm and taking water as a reference, subtracting the absorbance of a blank test from the absorbance measured by a water sample, and searching an ammonia nitrogen content C from a calibration curve1Ammonia nitrogen content of adsorbent C2＝C1*50/V2；
The amount of ammonia released C ═ C2*1.2143*V1，V1Is the volume of adsorbent filled.
Compared with the prior art, the invention has the beneficial effects that:
1. this device is equipped with on the apron and throws the feeder tube, and opens air exhaust device before the preparation, and the ammonia that the very first time will release is pumped completely to the adsorption column, avoids influencing the accurate survey in later stage.
2. The device is provided with the air exhaust device, and the ammonia release characteristic of the preparation of the filling paste can be obtained only by measuring the ammonia nitrogen concentration of the adsorbent conveyed to the adsorption column by the air exhaust device, so that the measurement is more convenient and simpler.
3. The detachable stirring motor is fixedly installed on the cover plate, the adjustable gas flowmeter is arranged at the air exhaust interface, and the detachable stirring motor can be replaced and adjusted according to actual conditions.
Drawings
FIG. 1 is a schematic diagram of the present invention.
In the figure: the device comprises a negative pressure mixing tank body 1, a cover plate 2, a cover plate chuck 3, an O-shaped sealing element 4, an adding pipe 5, a stirring motor 6, a stirring shaft 7, a paddle type blade 8, a filter disc 9, an air suction interface 10, a regulating valve 11, a gas flowmeter 12, an air suction device 13, a gas release device 14 and an adsorption column 15.
Detailed Description
The embodiments of the present invention will be described in detail below with reference to the drawings and examples.
As shown in figure 1, the device for measuring ammonia release in the process of preparing the magnesium slag and fly ash-based filling paste comprises a negative pressure mixing tank body 1, wherein the negative pressure mixing tank body 1 is used for preparing the filling paste and is connected with an adding pipe 5, and the adding pipe 5 is used for adding materials, water and other preparation materials. The interface 10 of bleeding of the negative pressure blending tank body 1 passes through the tube coupling air exhaust device 13, air exhaust device 13 is arranged in bleeding and forms the negative pressure in the negative pressure blending tank body 1 to take away the ammonia that prepares the in-process and volatilize from the liquid phase when bleeding, adsorption column 15 is connected to air exhaust of air exhaust device 13, sends into adsorption column 15 with the gas that contains ammonia, makes the ammonia fix in the adsorbent, through the ammonia nitrogen concentration that detects the adsorbent, can acquire the ammonia release characteristic that fills the lotion and prepare the in-process.
In one embodiment of the invention, the top of the negative pressure mixing tank body 1 is provided with a detachable cover plate 2, and a cover plate chuck 3 and an O-shaped sealing element 4 are used for ensuring the sealing with the negative pressure mixing tank body 1. The feeding pipe 5 and the air exhaust interface 10 can be both arranged on the cover plate 2, namely, the feeding pipe 5 and the air exhaust interface 10 can be both positioned at the top of the negative pressure mixing tank body 1.
In one embodiment of the invention, the top end of the feeding pipe 5 is of a bell mouth structure, so that materials can be conveniently added and air can be conveniently brought in.
In one embodiment of the invention, a stirring motor 6 is fixed on the cover plate 2, the output of the stirring motor 6 is connected with a stirring shaft 7 with paddle type blades 8 positioned in the tank, and a regulating valve 11 and a gas flowmeter 12 are arranged on a pipeline.
In one embodiment of the invention, the air extraction port 10 is provided with a filter 9 to filter out the influence of the interfering substances during the air extraction process.
In one embodiment of the present invention, the bottom of the adsorption column 15 is provided with a gas releasing device 14, the exhaust port of the gas extracting device 13 is connected with the gas releasing device 14, and the gas containing ammonia enters the adsorption column 15 in the form of bubbles and is subjected to mass transfer exchange with the adsorbent during the rising process.
In one embodiment of the present invention, the air pumping device 13 may be an air pump with a flow rate of 10 to 20L/min and a vacuum degree of-90 Pa, and the gas releasing device 14 may be an aeration head with a height of 3cm and a diameter of 1.9 cm.
Functionally, the apparatus of the present invention can be divided into a filling paste dispensing system I, a gas absorption system III and a gas delivery system II connecting the two. Therefore, the negative pressure mixing tank body 1, the cover plate 2, the cover plate chuck 3, the O-shaped sealing element 4, the adding pipe 5, the stirring motor 6, the stirring shaft 7 and the paddle type blade 8 are all components of a filling paste preparation system I, the filter sheet 9, the air extraction interface 10, the regulating valve 11, the gas flowmeter 12 and the air extraction device 13 are all components of a gas conveying system II, and the gas release device 14 and the adsorption column 15 are components of a gas absorption system III.
The device is provided with the adding pipe 5 and the air extractor 13, so that the phenomenon that the paste body is hydrated to release ammonia gas when the preparation tank is not closed and water is added is avoided, and the air which contains the released ammonia gas in the preparation tank can be sent into the adsorption column 15 by the air extractor 13 through a pipeline, so that the determination is more convenient and simpler, and the accuracy is improved. The method makes correct judgment on underground filling work based on the ammonia gas release rule, and has important guiding significance on underground safe mining.
Based on the above structure, the measurement method of the present invention comprises the steps of:
firstly, adding water for preparing the paste with a fixed volume into the negative pressure mixing tank body 1 according to the filling paste proportion through an adding pipe 5, and automatically adjusting the water consumption according to the mass concentration of the filling paste.
Then, the air extractor 13 is started to pump the air in the negative pressure mixing tank 1 into the adsorption column 15, and the opening state of the air extractor 13 is maintained, wherein the flow rate of the air extractor 13 is set to be 10-20L/min, and the vacuum degree is set to be-90 Pa. When the gas release device 14 is used, the gas containing ammonia forms uniformly distributed micro-bubbles under the action of the gas release device 14, and the bubbles perform mass transfer exchange with the adsorbent in the rising process to fix ammonia in the adsorbent.
And then, adding a mixed material formed according to the proportion of the filling paste material into the negative pressure mixing tank body 1 through a feeding pipe 5, wherein the mixed material comprises magnesium slag or fly ash, aggregate, an additive and the like. The stirring motor 6 is started, the added materials are uniformly stirred with water, the previous preparation mode that materials are uniformly mixed and filled and then stirred with water is changed, the aim is to completely pump the released ammonia gas to the adsorption column 15 in the first time, and the influence on the accurate determination in the later period is avoided. In the preparation process, air enters the negative pressure mixing tank body 1 through the feeding pipe 5 and carries ammonia gas volatilized from the liquid phase out of the tank body.
And finally, continuously detecting the ammonia nitrogen concentration in the adsorbent in the adsorption column 15, and converting the ammonia release amount, wherein the adsorbent can be dilute sulfuric acid with the concentration of 0.1 mol/L.
After reacting for a period of time, taking a certain amount of adsorbent to carry out ammonia nitrogen concentration detection by adopting a Nashiner reagent method, and finally obtaining the quality of ammonia gas released by the filling paste through conversion so as to obtain the ammonia release characteristic prepared by the filling paste.
Specifically, it may take V2Adding a mL adsorbent into a 50mL colorimetric tube, diluting to a marked line, adding 1.0mL potassium sodium tartrate solution, uniformly mixing, adding 1.5mL nano reagent, uniformly mixing, standing for 10min, measuring absorbance at a wavelength of 420nm by using a cuvette with an optical path of 20nm and taking water as a reference, subtracting the absorbance of a blank test from the absorbance measured by a water sample, and searching an ammonia nitrogen content C from a calibration curve1Ammonia nitrogen content of adsorbent C2＝C1*50/V2。
Wherein: c2The ammonia nitrogen content of the adsorbent, namely the ammonium ion concentration in the adsorbent, is mg/L; 50/V2The dilution factor is expressed in liters L.
The mass of the ammonia released by the large-proportion magnesium slag and the fly ash-based filling paste is calculated by the following method:
C＝C2*1.2143*V1
in the formula: c is the mass of ammonia released by the large-proportion magnesium slag and the fly ash-based filling paste, and the unit is mg; 1.2143 is the conversion coefficient of nitrogen to ammonia, V1The unit is the volume of the packed adsorbent in mL.
In conclusion, the device has the advantages of small occupied area, capability of simultaneously preparing a plurality of pastes and performing air extraction, low operation cost, simplicity and convenience in operation, high accuracy and high stability, only needs to measure the ammonia nitrogen content in the adsorbent, does not have the problem of air extraction blockage, and can replace parts according to actual requirements at any time.
Claims (10)
1. The device for measuring ammonia release in the process of preparing the magnesium slag and fly ash based filling paste is characterized by comprising a negative pressure mixing tank body (1) with a stirring system and used for preparing the filling paste, wherein the negative pressure mixing tank body (1) is connected with an adding pipe (5) used for adding materials, an air suction interface (10) of the negative pressure mixing tank body (1) is connected with an air suction device (13) through a pipeline, the air suction device (13) is used for sucking air to form negative pressure in the negative pressure mixing tank body (1) and taking away ammonia gas volatilized from a liquid phase in the paste preparation process, an air outlet of the air suction device (13) is connected with an adsorption column (15) to fix the ammonia gas in an adsorbent, and the ammonia release characteristic in the filling paste preparation process is obtained by detecting the ammonia nitrogen concentration of the adsorbent.
2. The device for measuring ammonia release in the process of preparing the magnesium slag and fly ash-based filling paste according to claim 1, wherein a detachable cover plate (2) is arranged at the upper part of the negative pressure mixing tank body (1), and the adding pipe (5) and the air suction port (10) are both arranged on the cover plate (2).
3. The device for measuring ammonia release in the process of preparing the magnesium slag and fly ash-based filling paste according to claim 1 or 2, wherein the top end of the feeding pipe (5) is of a bell mouth structure, and the air suction port (10) is provided with a filter (9).
4. The device for measuring ammonia release in the process of preparing the magnesium slag and fly ash-based filling paste according to claim 2, wherein a stirring motor (6) is fixed on the cover plate (2), the output of the stirring motor (6) is connected with a stirring shaft (7) with a paddle type blade (8) in a tank, and a regulating valve (11) and a gas flowmeter (12) are arranged on the pipeline.
5. The device for measuring ammonia release in the preparation process of the magnesium slag and fly ash-based filling paste according to claim 1, wherein a gas release device (14) is arranged at the bottom of the adsorption column (15), an exhaust port of the air extraction device (13) is connected with the gas release device (14), and the gas containing ammonia enters the adsorption column (15) in the form of bubbles and is subjected to mass transfer exchange with the adsorbent in the rising process.
6. The device for measuring ammonia release in the preparation process of the magnesium slag and fly ash-based filling paste according to claim 5, wherein the air extractor (13) is an air pump with the flow rate of 10-20L/min and the vacuum degree of-90 Pa, and the gas release device (14) is an aeration head with the height of 3cm and the diameter of 1.9 cm.
7. The method for measuring the ammonia release in the process of preparing the magnesium slag and fly ash-based filling paste according to claim 1 is characterized by comprising the following steps of:
firstly, adding water for preparing paste with a fixed volume into a negative pressure mixing tank body (1) through an adding pipe (5) according to the ratio of the filled paste;
then, starting the air extractor (13) to pump the gas in the negative pressure mixing tank body (1) into the adsorption column (15), and maintaining the opening state of the air extractor (13);
then, adding a mixed material formed according to the proportion of the filling paste material into the negative pressure mixing tank body (1) through an adding pipe (5) and uniformly stirring the mixed material with water, wherein the mixed material comprises magnesium slag or fly ash, aggregate and an additive;
and finally, continuously detecting the ammonia nitrogen concentration in the absorbent in the adsorption column (15), and converting the released ammonia amount.
8. The measurement method according to claim 7, wherein the flow rate of the gas-extracting device (13) is set to 10 to 20L/min and the degree of vacuum is set to-90 Pa.
9. The method according to claim 7, wherein the adsorbent is dilute sulfuric acid having a concentration of 0.1 mol/L.
10. The assay of claim 7, wherein the amount of ammonia released is obtained by:
get V2Adding a mL adsorbent into a 50mL colorimetric tube, diluting to a marked line, adding 1.0mL potassium sodium tartrate solution, uniformly mixing, adding 1.5mL nano reagent, uniformly mixing, standing for 10min, measuring absorbance at a wavelength of 420nm by using a cuvette with an optical path of 20nm and taking water as a reference, subtracting the absorbance of a blank test from the absorbance measured by a water sample, and searching an ammonia nitrogen content C from a calibration curve1Ammonia nitrogen content of adsorbent C2＝C1*50/V2；
The amount of ammonia released C ═ C2*1.2143*V1，V1Is the volume of adsorbent filled.
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