CN212301342U - Test device for rapidly judging ammonia content of fly ash - Google Patents
Test device for rapidly judging ammonia content of fly ash Download PDFInfo
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- CN212301342U CN212301342U CN202021158339.1U CN202021158339U CN212301342U CN 212301342 U CN212301342 U CN 212301342U CN 202021158339 U CN202021158339 U CN 202021158339U CN 212301342 U CN212301342 U CN 212301342U
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Abstract
The invention discloses a testing device for rapidly judging ammonia content of fly ash, which comprises a distillation flask, an anti-splash water-vapor separator, a condensation pipe, a steam flask and an alkali liquor reagent bottle which are connected with the distillation flask through pipelines, wherein the anti-splash water-vapor separator is arranged above the distillation flask and is communicated with the distillation flask, the condenser pipe is connected above the anti-splash water-vapor separator through a pipeline, and a detection kit is arranged below the condensation pipe and is used for detecting the ammonia content of liquid containing ammonia to be detected. The invention adopts the detection kit to detect the liquid to be detected containing ammonia, avoids complex titration process, simplifies operation steps, and in addition, the detection kit can realize batch production and long-term storage, avoids reagent preparation and calibration in the test process, and shortens the test time, thereby improving the test efficiency and rapidly realizing the judgment of the ammonia-containing range of the fly ash.
Description
Technical Field
The invention relates to the technical field of building material detection, in particular to a testing device for rapidly judging ammonia content of fly ash.
Background
The fly ash is a byproduct of combustion power generation of a coal-fired power plant, is applied to cement, mortar and concrete products for a long time, plays roles in reducing cost and improving efficiency and improves performance, and is an important cementing material. In recent years, in order to respond to national environmental protection requirements and reduce ammonia nitrogen substances discharged to the atmosphere by enterprises such as thermal power plants and the like, the coal-fired power plants successively carry out denitration modification on units, and in the operation of SCR and SNCR, ammonia is used for treating nitrogen oxides in flue gas and simultaneously causing residues of the ammonia nitrogen substances in fly ash, so that the fly ash subjected to denitration modification has the problems of a large amount of bubbles, sharp odor, obviously prolonged or even no coagulation of coagulation time, concrete volume expansion and even serious expansion, internal porosity, strength reduction and the like in the application process of cement concrete, the deterioration of the performance of the cement concrete is caused, and the quality safety and the construction environment safety of a concrete structure are seriously threatened.
Due to the diversity of chemical forms and physical combination forms of ammonia nitrogen substances in the fly ash, the test of the ammonia nitrogen content of the fly ash has a plurality of difficulties. The existing ammonia-containing test method for fly ash mainly comprises the methods of soaking, suction filtration or centrifugal separation and the like for extracting ammonium ions, a formaldehyde method, a distillation-titration method, a Nassner reagent-spectrophotometer method, a salicylic acid photometer, an ion chromatography and the like. The method of infiltration, suction filtration or centrifugal separation has the defects of insufficient extraction and difficult avoidance of Ca2+、Mg2+Interference problems with ions and gels; the formaldehyde method and the distillation-titration method have the problems of insufficient precision and incapability of meeting the test requirement of the fly ash; the method comprises a Nashin reagent-spectrophotometer, a salicylic acid photometer, an ion chromatography, etc. to obtain essenceToo high, the test scope is narrow and not suitable for the problem of fly ash ammonia test. In addition, the methods have the problems of long testing time, complex solution preparation, complex operation and the like in the quantitative testing process.
Disclosure of Invention
Aiming at the problems, the invention provides a testing device for rapidly judging ammonia content of fly ash, aiming at the defects of the existing quantitative test of ammonia content of fly ash, rapidly detecting and judging the ammonia content of fly ash, and providing a basis for quantitative control of ammonia content of denitration fly ash and other building material products.
The invention adopts the following technical scheme:
the utility model provides a test device for judge fly ash ammonia content fast, includes the retort, splashproof vapor separator, condenser pipe, steam bottle and alkali lye reagent bottle that link to each other with the retort through the pipeline, splashproof vapor separator sets up in the retort top and communicates with the retort, and the pipe connection condenser pipe is passed through to splashproof vapor separator top, and the condenser pipe below is equipped with the detect reagent box and is used for detecting the ammonia content that contains ammonia and wait to detect the liquid.
Preferably, the testing device further comprises capsule belts, and capsule balls are arranged on the capsule belts at equal intervals.
Preferably, the splash-proof water-vapor separator comprises a hollow spherical cavity, the upper end and the lower end of the cavity are respectively provided with a gas outlet and a gas inlet which are communicated with the interior of the cavity, the lower end of the gas outlet extends into the interior of the cavity, the lower end of the gas outlet is provided with a circular arc-shaped splash-proof baffle disc for preventing reaction liquid from boiling over to enter a subsequent pipeline to influence a result, a gas through hole is formed at the joint of the gas outlet and the splash-proof baffle disc, condensed liquid can flow back to the distillation flask through the gas through hole, a circulation loop for continuous distillation extraction and reflux reaction is formed in the distillation flask and the splash-proof water-vapor separator, and ammonia nitrogen substances in the fly ash.
Preferably, the detection kit comprises a hollow box body and a detection chamber arranged inside the box body, a cover body is arranged above the detection chamber, a conveying groove is formed in one side of the cover body, a liquid releasing groove is formed in one end of the conveying groove, the lower end of the liquid releasing groove is communicated with the detection chamber through a pipeline, a puncturing device is arranged above the liquid releasing groove, and a discharge groove is formed in the right side of the upper end face of the liquid releasing groove.
Preferably, the puncturing device comprises a transmission motor fixed above the liquid releasing groove, a transmission turntable is arranged below the transmission motor, the transmission motor drives the transmission turntable to rotate through a bearing, a fan-shaped notch is formed in the transmission turntable and used for placing the capsule ball, and a steel needle is arranged on the groove wall of the liquid releasing groove and used for puncturing the capsule ball.
Preferably, an extrusion clapboard is arranged between the conveying turntable and the inner wall of the liquid releasing groove and used for extruding the punctured capsule balls, one end of the extrusion clapboard is connected to one end of the discharge groove, a stripping clapboard is arranged on the groove wall of the discharge groove, one end of the stripping clapboard is close to the conveying turntable to prevent the capsule balls from being brought into the conveying groove, and the stripping clapboard strips the empty capsule belt stuck on the conveying turntable.
Preferably, the cover body is provided with an ammonia gas through hole and a stirrer, the lower end of the condensation pipe extends into the absorption liquid in the detection chamber through a pipeline, the absorption liquid absorbs ammonia gas, and the stirrer stirs the ammonia-containing liquid to be detected in the detection chamber;
the lower end of the detection chamber is provided with a liquid discharge pipe for discharging the detected detection liquid.
The testing method of the testing device for rapidly judging the ammonia content of the fly ash comprises the following steps:
s1, hermetically connecting a testing device, weighing a certain amount of fly ash, filling the fly ash into a distillation flask, and washing and infiltrating;
s2, filling quantitative absorption liquid into the detection chamber, adding excessive alkaline reaction liquid into the distillation flask, and introducing hot steam generated in the steam flask into the distillation flask to accelerate the reaction and the distillation of ammonia gas;
s3, separating the distillate gas by a splash-proof water-vapor separator, cooling by a condenser pipe, and introducing the distillate gas into an absorption liquid at the bottom of the detection chamber to obtain a liquid to be detected containing ammonia;
and S4, starting the detection kit, putting a capsule belt into the puncturing device, and rapidly testing the ammonia content range of the fly ash according to the color change of the ammonia-containing liquid to be tested and the consumption of capsule balls.
Preferably, the capsule ball is filled with 1.2-12ml of dilute hydrochloric acid reaction reagent with the concentration of 0.005-0.05 mol/L, 0.01-0.1 ml of color indicator of methyl red-methylene blue solution, and the mixed detection reagent is red, and can detect the ammonia content of the fly ash of 50/(M/10) -100/(M/10) ppm, wherein M is the mass of the fly ash and g.
The alkaline reaction solution is sodium hydroxide or potassium hydroxide, the mass concentration is 5-50 wt%, and the mass ratio of the alkaline reaction solution to the fly ash sample is as follows: (5-50): (10-30);
the absorption liquid is boric acid, the mass concentration is 1.5-4 wt%, and the mass ratio of the absorption liquid to the fly ash sample is as follows: (20-200) and (10-30).
The invention has the beneficial effects that:
1. the invention adopts the detection kit to detect the liquid to be detected containing ammonia, avoids complex titration process, simplifies operation steps, and in addition, the detection kit can realize batch production and long-term storage, avoids reagent preparation and calibration in the test process, and shortens test time, thereby improving test efficiency and rapidly realizing judgment of the ammonia-containing range of the fly ash.
2. The invention adopts excessive alkali liquor reaction and an anti-splash separator, ensures the extraction sufficiency of ammonia nitrogen substances in the fly ash and improves the efficiency; the detection reagent in the capsule ball directly reacts with the ammonium borate, the reaction is rapid, the color development is sensitive, so the influence factors are few, the reaction is sensitive, the reliability of data is high, the test range is wide, and the applicability is stronger.
Drawings
In order to more clearly illustrate the technical solutions of the embodiments of the present invention, the drawings of the embodiments will be briefly described below, and it is apparent that the drawings in the following description only relate to some embodiments of the present invention and are not limiting on the present invention.
FIG. 1 is a schematic structural diagram of a testing apparatus according to the present invention;
FIG. 2 is a schematic perspective view of the detection kit of the present invention;
FIG. 3 is a top view of the detection kit of the present invention;
FIG. 4 is a schematic view of the lancing device (without a drive motor) according to the present invention;
FIG. 5 is a schematic structural view of the gelatin capsule band of the present invention;
FIG. 6 is a schematic cross-sectional view of the splash separator of the present invention;
shown in the drawings
1-a distillation flask, 2-a steam flask, 3-a steam valve, 4-a steam pipeline, 5-a sealing plug, 6-an alkali liquor reagent bottle, 7-an alkali liquor pump, 8-an alkali liquor valve, 9-a distillate gas pipeline, 10-a splash-proof water-vapor separator, 11-a condenser pipe, 12-a condensate water inlet, 13-a condensate water outlet, 14-a suck-back prevention one-way valve, 15-a box body, 16-a detection chamber, 17-a cover body, 18-a stirrer, 19-an ammonia through hole, 20-a steel needle, 21-a conveying tank, 22-a conveying turntable, 23-a stripping baffle, 24-a liquid release groove, 25-a transmission motor, 26-a liquid discharge pipe, 27-a capsule belt, 28-an extrusion baffle, 29-a discharge tank and 30-a capsule ball;
101-splash baffle disc, 102-gas inlet, 103-gas outlet, 104-gas through hole, 105-cavity.
Detailed Description
In order to make the objects, technical solutions and advantages of the embodiments of the present invention clearer, the technical solutions of the embodiments of the present invention will be clearly and completely described below with reference to the drawings of the embodiments of the present invention. It is to be understood that the embodiments described are only a few embodiments of the present invention, and not all embodiments. All other embodiments, which can be derived by a person skilled in the art from the described embodiments of the invention without any inventive step, are within the scope of protection of the invention.
Unless otherwise defined, technical or scientific terms used herein shall have the ordinary meaning as understood by one of ordinary skill in the art to which this disclosure belongs. The use of the word "comprising" or "comprises", and the like, in this disclosure is intended to mean that the elements or items listed before that word, include the elements or items listed after that word, and their equivalents, without excluding other elements or items. "upper", "lower", "left", "right", and the like are used merely to indicate relative positional relationships, and when the absolute position of the object being described is changed, the relative positional relationships may also be changed accordingly.
The invention is further illustrated with reference to the following figures and examples.
As shown in fig. 1 to 6, a test device for rapidly determining ammonia content in fly ash comprises a distillation flask 1, an anti-splash water-vapor separator 10 and a condensation pipe 11, wherein the distillation flask 1 is sealed by a sealing plug 5, an opening above the distillation flask 1 is provided with a steam flask 2 and an alkali liquor reagent flask 6 which are communicated with the interior of the distillation flask 1 through a pipeline, the steam flask 2 is a closed flask body, the exterior of the closed flask body heats the flask body of the steam flask 2by using heating methods such as electricity or fuel, and the like, so that distilled water in the steam flask 2 generates steam, the steam is introduced into the interior of the distillation flask 1 through a steam pipeline 4 to accelerate the reaction between the fly ash and the alkali liquor and the distillation of ammonia gas, and a steam valve 3 is arranged on the steam pipeline;
an alkali liquor pump 7 and an alkali liquor valve 8 are arranged on a pipeline between the alkali liquor reagent bottle 6 and the steam bottle 2, and alkali liquor in the alkali liquor reagent bottle 6 is pumped into the distillation flask 1 through the alkali liquor pump 7 to react with the fly ash in the test process; the alkali liquor is sodium hydroxide or potassium hydroxide, the mass concentration is 5-50 wt%, and the mass ratio of the alkali liquor to the fly ash is as follows: (5-50): (10-30).
The splash-proof water-vapor separator 10 is arranged above the distillation flask 1 and is communicated with the interior of the distillation flask 1 through a distillate gas pipeline 9, the upper part of the splash-proof water-vapor separator 10 is connected with a condensation pipe 11 through a pipeline, a condensation water inlet 12 and a condensation water outlet 13 are arranged on the condensation pipe 11 and are used for the inlet and outlet of condensation water, and a detection kit is arranged below the condensation pipe 11 and is used for detecting the ammonia content of liquid to be detected containing ammonia.
The detection kit comprises a hollow box body 15 and a detection chamber 16 arranged in the box body 15, wherein a cover body 17 is arranged on the end surface above the detection chamber 16, an ammonia gas through hole 19 and a stirrer 18 are arranged on the cover body 17, an absorption pipeline is arranged at the lower end of the condensation pipe 11, a suck-back prevention check valve 14 is arranged on the absorption pipeline to prevent liquid in the pipeline from suck back, the lower end of the absorption pipeline extends into absorption liquid placed in the detection chamber 16, the absorption liquid absorbs ammonia, and the stirrer 18 stirs ammonia-containing liquid to be detected in the detection chamber 16;
the stirrer 18 comprises a motor arranged on the cover body 17, the motor drives a stirring rod arranged in the detection chamber 16 to rotate through a shaft, and in the test process, the stirring rod enables the liquid containing ammonia to be tested to be fully mixed with the reaction reagent in the capsule ball 30;
a drain pipe 26 is provided at the lower end of the detection chamber 16 for discharging the detection liquid after detection.
The box body 15 and the detection chamber 16 can be made of one transparent material of polymethyl methacrylate, polystyrene and polycarbonate, so that the color change of the ammonia-containing liquid to be detected in the detection chamber 16 can be observed conveniently.
According to the actual detection requirement, quantitative absorption liquid can be placed in the detection chamber 16, then ammonia gas is introduced to form ammonia-containing liquid to be detected, and the ammonia-containing liquid to be detected can also be directly placed for detection.
A conveying groove 21 is formed in one side of the cover body 17 and used for placing a capsule belt 27, a liquid releasing groove 24 is formed in one end of the conveying groove 21, and preferably, the conveying groove 21 can be obliquely arranged on the upper end face of the box body 15 (the end far away from the liquid releasing groove 24 is higher);
the liquid releasing groove 24 is funnel-shaped, the lower end of the liquid releasing groove is communicated with the inside of the detection chamber 16 through a pipeline, a puncturing device is arranged above the liquid releasing groove, a discharge groove 29 is arranged on the right side of the upper end face of the liquid releasing groove 24, and the capsule belt punctured by the puncturing device is discharged from the discharge groove 29.
The puncturing device comprises a transmission motor 25 fixed above the liquid releasing groove 24, the transmission motor 25 is fixed on the upper end face of the box body 15 through a support, the transmission motor 25 is connected with a transmission turntable 22 arranged below the transmission motor 25 through a shaft so as to drive the transmission turntable 22 to rotate, a fan-shaped notch is arranged on the transmission turntable 22 and used for positioning and clamping a capsule ball 30, the transmission turntable 22 rotates for a circle to realize transmission of one capsule ball, and a steel needle 20 is arranged on the groove wall of the liquid releasing groove 24 and used for puncturing the capsule ball 30;
an extrusion clapboard 28 is arranged between the conveying turntable 22 and the inner wall of the liquid releasing groove 24 and is used for extruding capsule balls 30 which are punctured by the steel needles 20, the left end of the extrusion clapboard 28 is fixed on the groove wall of the liquid releasing groove 24, the right end of the extrusion clapboard 28 is connected with the left end of the discharge groove 29, the middle part of the extrusion clapboard is fixed on the groove wall of the liquid releasing groove 24 through a bracket, a stripping clapboard 23 is arranged on the groove wall of the discharge groove 29, one end of the stripping clapboard 23 is abutted against the conveying turntable 22, and the stripping clapboard 23 strips the empty capsule belt 27 which is stuck on the conveying turntable 22.
The detection kit comprises a power switch which respectively controls the on-off of the stirrer 18 and the transmission motor 25, a controller is arranged between the power switch and the transmission motor 25, the transmission turntable 22 rotates one circle by pressing a key once, the transmission motor 25 is a 42BYGHW hybrid stepping motor, the controller comprises an 80C52 singlechip, a driving chip UM2003 and keys (the prior art is not repeated, and the components can be purchased in the market)
The capsule belt 27 is made of a corrosion-resistant plastic material insoluble in the liquid containing ammonia to be detected, capsule balls 30 are arranged on the capsule belt at equal intervals, and the capsule balls 30 are connected by the plastic belt.
6.0ml of dilute hydrochloric acid reaction reagent with the concentration of 0.005mol/L and 0.1ml of color indicator of methyl red-methylene blue solution are filled in the capsule ball 30; or 3.0ml of dilute hydrochloric acid reaction reagent with the concentration of 0.01mol/L and 0.05ml of color indicator of methyl red-methylene blue solution are filled in the capsule ball 30; the mixed detection reagent is red, and the ammonia content of the fly ash of 50ppm can be detected by a single capsule ball 30; when n capsule balls 30 are used, the ammonia content of the fly ash can be detected between 50(n-1)/(M/10) -50n/(M/10) ppm, wherein M is the mass of the fly ash, and g;
1.2ml of dilute hydrochloric acid reaction reagent with the concentration of 0.05mol/L and 0.01ml of color indicator of methyl red-methylene blue solution are filled in the capsule ball 30; or 12ml of dilute hydrochloric acid reaction reagent with the concentration of 0.005mol/L and 0.1ml of color indicator of methyl red-methylene blue solution are filled in the capsule ball 30; the mixed detection reagent is red, and the ammonia content of the fly ash of 100ppm can be detected by a single capsule ball 30; when n capsule balls 30 are used, the ammonia content of the fly ash can be detected, wherein the ammonia content is between 100(n-1)/(M/10) -100n/(M/10) ppm, M is the mass of the fly ash, and g;
when the capsule belt 27 is used, firstly, the plastic belt at the lower end of the capsule ball 30 is wound around the transmission turntable 22 and is led out from the discharge groove 29, and the capsule ball 30 is just positioned at the fan-shaped notch;
during the conveying process, the capsule ball 30 is firstly punctured by the steel needle 20, the punctured capsule ball 30 is squeezed between the conveying turntable 22 and the groove wall of the liquid releasing groove 24, the reaction reagent in the capsule ball 30 is released into the liquid releasing groove 24 below, and finally flows into the detection chamber 16;
the arc-shaped extrusion partition plate 28 between the groove wall of the liquid releasing groove 24 and the conveying rotary disc 22 again extrudes residual reaction reagent in the capsule balls 30, and the extruded clean capsule balls 30 enter the discharge groove 29 to be discharged under the blockage of the stripping partition plate 23.
The testing method of the testing device for rapidly judging the ammonia content of the fly ash comprises the following steps:
s1, hermetically connecting a testing device, weighing 10-30g of coal ash by mass M, filling into a distillation flask 1, and washing and infiltrating;
s2, filling a boric acid solution with the mass concentration of 1.5-4 wt% into the detection chamber 16, adding a NaOH solution with the mass concentration of 5-50 wt% into the distillation flask 1, introducing hot steam in the steam flask 2 into the distillation flask 1 to accelerate the reaction and the distillation of ammonia gas, and distilling for 10 min;
s3, separating the distillate gas by a splash-proof water-vapor separator 10, cooling by a condenser tube 11, and introducing boric acid solution in a detection chamber 16 to obtain ammonia-containing solution to be detected;
s4, starting the detection kit, putting a capsule belt 27 (3 ml of dilute hydrochloric acid reaction reagent with the concentration of 0.01mol/L and 0.05ml of a color indicator of methyl red-methylene blue solution) into the puncturing device, rotating the transmission turntable 22 for one circle to puncture one capsule ball 30, and stirring the mixture to be detected to have no color change if the ammonia-containing liquid is light red, which indicates that the ammonia-containing range of the fly ash is less than 50/(M/10) ppm;
if the pink color in the solution to be tested containing ammonia gradually becomes light until the solution is converted into yellow green, the ammonia containing range of the fly ash is more than 50/(M/10) ppm;
and the capsule balls 30 are punctured continuously until the solution turns into light pink and does not change color within 1min, and the number of the punctured capsule balls 30 is n, so that the ammonia content of the fly ash is 50(n-1)/(M/10) -50n/(M/10) ppm.
According to the operation steps, the ammonia content range of several kinds of fly ash is measured, the measured ammonia content range is compared with an accurate quantitative result, and the accuracy is verified, wherein the result is shown in table 1.
TABLE 1 test result table for ammonia content range of fly ash
As the optimization of the scheme, the prepared liquid to be tested containing ammonia can be directly placed into the detection chamber, and the ammonia content concentration range of the liquid to be tested containing ammonia can be quickly obtained through the release amount of the capsule ball 30, so that the defects of reagent preparation and calibration, long titration time and the like in the test process are avoided; the detection kit can realize batch production and long-term storage, and improves the testing efficiency.
Although the present invention has been described with reference to a preferred embodiment, it should be understood that various changes, substitutions and alterations can be made herein without departing from the spirit and scope of the invention as defined by the appended claims.
Claims (7)
1. The utility model provides a test device for judge fly ash ammonia content fast, its characterized in that includes retort (1), splashproof vapor separator (10), condenser pipe (11), steam bottle (2) and alkali lye reagent bottle (6) through pipeline and retort (1) inside intercommunication, splashproof vapor separator (10) set up in retort (1) top and with retort (1) inside intercommunication, connect condenser pipe (11) through the pipeline above splashproof vapor separator (10), and condenser pipe (11) below is equipped with the detect reagent box.
2. The test device for rapidly judging the ammonia content of the fly ash according to claim 1, further comprising capsule belts (27), wherein the capsule belts (27) are provided with capsule balls (30) at equal intervals.
3. The testing device for rapidly judging ammonia content of fly ash according to claim 2, wherein the anti-splash water-vapor separator (10) comprises a cavity (105), the upper end and the lower end of the cavity (105) are respectively provided with a gas outlet (103) and a gas inlet (102), the gas outlet (103) extends into the cavity (105), the lower end of the cavity is provided with a splash guard (101), and a gas through hole (104) is arranged at the joint of the gas outlet (103) and the splash guard (101).
4. The device for rapidly determining ammonia content in fly ash according to claim 3, wherein the detection kit comprises a hollow box body (15), a detection chamber (16) arranged inside the box body (15), a cover body (17) is arranged above the detection chamber (16), a conveying groove (21) is arranged on one side of the cover body (17), a liquid releasing groove (24) is arranged at one end of the conveying groove (21), the lower end of the liquid releasing groove (24) is communicated with the detection chamber (16), a puncturing device is arranged above the liquid releasing groove, and a discharge groove (29) is arranged on the right side of the upper end face of the liquid releasing groove (24).
5. The testing device for rapidly judging the ammonia content of the fly ash according to claim 4, wherein the puncturing device comprises a transmission motor (25) fixed above the liquid releasing groove (24), a transmission turntable (22) is arranged below the transmission motor (25), the transmission motor (25) drives the transmission turntable (22) to rotate, and a steel needle (20) is arranged on the wall of the liquid releasing groove (24).
6. The device for rapidly determining the ammonia content in the fly ash as claimed in claim 5, wherein an extrusion baffle (28) is arranged between the transmission turntable (22) and the inner wall of the liquid release groove (24), one end of the extrusion baffle (28) is connected to one end of the discharge groove (29), a stripping baffle (23) is arranged on the wall of the discharge groove (29), and one end of the stripping baffle (23) is close to the transmission turntable (22).
7. The test device for rapidly judging ammonia content of fly ash according to claim 6, wherein the cover body (17) is provided with an ammonia gas through hole (19) and a stirrer (18), and the lower end of the condensation pipe (11) extends into the detection chamber (16) through a pipeline;
a liquid discharge pipe (26) is arranged at the lower end of the detection chamber (16).
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