CN114910604B - Online analysis instrument and online analysis method for ammonia-salt ratio - Google Patents
Online analysis instrument and online analysis method for ammonia-salt ratio Download PDFInfo
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- CN114910604B CN114910604B CN202210544306.8A CN202210544306A CN114910604B CN 114910604 B CN114910604 B CN 114910604B CN 202210544306 A CN202210544306 A CN 202210544306A CN 114910604 B CN114910604 B CN 114910604B
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- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
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- G01N1/10—Devices for withdrawing samples in the liquid or fluent state
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Abstract
The invention discloses an ammonia-salt ratio online analyzer, which comprises a main body cabinet, a circulating sampler arranged on the outer side of the main body cabinet, an analyzer host, a pure water module and a NaCl concentration detector which are arranged in the main body cabinet, wherein the analyzer host comprises a pure water pump, a feed pump, a detection cup, a discharge pump, a plunger pump and a six-way valve, the six-way valve is provided with a first outlet, a third outlet, a fifth outlet, a second inlet, a fourth inlet and a sixth inlet, the third outlet and the discharge end of the discharge pump are commonly connected with a liquid level sensor, a PH meter is arranged on the detection cup, and a positive pressure system is arranged in the main body cabinet.
Description
Technical Field
The invention belongs to the technical field of chemical analysis, and particularly relates to an ammonia-salt ratio online analyzer and an ammonia-salt ratio online analysis method.
Background
In the production process of sodium carbonate, ammonia brine and carbon dioxide are subjected to a physical and chemical process in a carbonization tower to realize the conversion of NaCl to NaHCO 3 Is converted to obtain qualified NaHCO 3 Suspension, the chemical reaction of which is NaCl+NH 3 +CO 2 +H 2 O＝NaHCO 3 +NH 4 Cl, the ammonia salt ratio is particularly important in the chemical reaction process, about 10 to 13.5 percent of ammonia in the ammonia salt water is taken away by tail gas discharged from the top of the tower, so that the ammonia salt ratio is maintained to be 1.110 to 1.150, and NH in alkali liquor is discharged 3 With Cl - In a ratio of 1:1, naCl conversion is low if free ammonia in the ammonia brine is too low, and Cl is not only reduced if free ammonia is too high - The concentration and the ammonia conversion rate are reduced, and the phenomenon of tower blockage of the carbonation alkali preparation tower is caused.
The measurement of the ammonia-salt ratio is a complex process, at present, the measurement of the ammonia-salt ratio mainly adopts manual sampling, the manual sampling analysis frequency is high, the workload is very large, the volatilized ammonia gas also has certain harm to human bodies, the detection time is long, and the feedback and the treatment of the problems in each production process cannot be carried out in time, so that an online device capable of carrying out closed sampling and accurate analysis is urgently needed, and data are transmitted to a DCS for production control.
Disclosure of Invention
In order to overcome the defects of the prior art, the invention provides an ammonia-salt ratio online analyzer and an ammonia-salt ratio online analysis method which can realize closed sampling in the production process of sodium carbonate and can realize rapid and accurate online analysis of the ammonia-salt ratio.
In order to achieve the above purpose, the present invention is realized by the following technical scheme:
the utility model provides an ammonia salt is than online analysis appearance, includes the main part cabinet, still including setting up in the circulation sampler in the main part cabinet outside and setting up in the inside analyzer host computer of main part cabinet, pure water module and NaCl concentration detector, the analyzer host computer includes pure water pump, feed pump, detection cup, discharge pump, plunger pump and six-way valve, circulation sampler, naCl concentration detector and feed pump pass through the feeding system that the pipeline formed the sample in proper order with the feed pump, six-way valve is provided with three export and No. 2 of No. 3 export (3) and No. 5) respectively, no. 4) and No. 6 of No. 5 import, and the discharge end of feed pump passes through pipeline connection No. 4 of six-way valve, and the feed end of pure water pump is connected with No. 6 of pure water module delivery port and six-way valve respectively, and No. 2 of six-way valve and No. 5 pass through the quantitative pipe intercommunication, and No. 1 of six-way valve is connected with No. 3 of discharge pump through the pipeline connection No. 3 of six-way valve and No. 6 of discharge pump, and the discharge end of six-way valve is connected with the discharge pump through the discharge end of detection cup through the pipeline connection, and the discharge end of six-way valve is connected with the discharge pump.
Further, the circulation sampler lower part is provided with the circulation sampler import of being connected to the production pipeline that circulates there is ammonia brine, and circulation sampler upper portion is provided with circulation sampler export, be provided with the filtration membrane pipe that is used for filtering impurity and bubble in the circulation sampler, the lower extreme of filtration membrane pipe is close to circulation sampler import, and the upper end of filtration membrane pipe is kept away from circulation sampler import and is connected to the feed end of NaCl concentration detector through the pipe connection.
Further, the inlet and the outlet of the six-way valve are sequentially and evenly arranged at intervals according to the sequence of inlet-outlet-inlet, the six-way valve is provided with an initial position and a first rotation position, an included angle between the initial position and the first rotation position of the six-way valve along the anticlockwise direction is 60 degrees, a six-way inlet (6) of the six-way valve is communicated with a first outlet (1) when the six-way valve is positioned at the initial position, a four-way inlet (4) is communicated with a five-way outlet (5), a two-way inlet (2) is communicated with a three-way outlet (3), a two-way inlet (2) of the six-way valve is communicated with a first outlet (1) when the six-way valve is positioned at the first rotation position, a four-way inlet (4) is communicated with a three-way outlet (3), and a five-way outlet (5) is communicated with a six-way inlet (6).
Further, a liquid level sensor is connected to a third outlet (3) of the six-way valve and a discharging end of the discharging pump, a displacement sample inlet is arranged on the left side of the liquid level sensor, a detected material interface is arranged above the liquid level sensor, a discharging port is arranged below the liquid level sensor, the third outlet (3) of the six-way valve is connected with the displacement sample inlet of the liquid level sensor through a pipeline, the discharging end of the discharging pump is connected with the detected material interface of the liquid level sensor through a pipeline, and the discharging port of the liquid level sensor is connected to a discharging pipe.
Further, a stirring device is arranged in the detection cup.
Further, a PH meter for measuring PH value is arranged on the detection cup.
Further, a positive pressure system is arranged in the main body cabinet, and the positive pressure system comprises a pressure reducing valve and a flowmeter.
Further, the detection solution is sulfuric acid.
Still further still include display screen, PLC controller, PCB control panel and for its power that supplies power, can export the data to the DCS system through the signal line.
The invention also provides an online analysis method of the ammonia-salt ratio, which comprises the following steps:
(1) Cleaning with pure water: starting a pure water pump, wherein the six-way valve is at an initial position, sucking pure water through a feeding end of the pure water pump, pumping the pure water into a six-way inlet (6) of the six-way valve, feeding the pure water into a detection cup through a first outlet (1), after pumping a certain amount of pure water, starting a stirring device in the detection cup to stir the pure water, cleaning the detection cup, starting a discharge pump to pump out the pure water for cleaning in the detection cup, enabling the pure water to enter a liquid level sensor through a detected material interface of the liquid level sensor, discharging the pure water into a discharge pipe through a discharge port of the liquid level sensor, completing pure water cleaning, and closing the discharge pump;
(2) Replacement of samples: after the pure water is cleaned in the step (1), starting a feed pump, sucking and filtering the pure water through a filter membrane pipe in a circulating sampler to obtain a sample, wherein the six-way valve is at an initial position, the sample is pumped into a No. four inlet (4) of the six-way valve through the feed pump after passing through a NaCl concentration detector, enters the liquid level sensor from a replacement sample inlet of the liquid level sensor through a No. five outlet (5), a quantitative pipe and a No. two inlet (2), the liquid level sensor detects whether the sample enters or not, the sample entering the liquid level sensor is discharged into a discharge pipe through a discharge port of the liquid level sensor, the replacement of the sample is completed, and the replacement time of the sample is controlled to be 25-40 seconds;
(3) Quantification of samples: after the replacement of the sample in the step (2) is finished, a quantifying pipe connected with a fifth outlet (5) and a second inlet (2) is filled with the sample, the six-way valve is rotated anticlockwise by 60 degrees, the six-way valve is positioned at a first rotation position, the sample in the quantifying pipe is controlled in the quantifying pipe, the volume of the sample in the quantifying pipe is calculated through the volume of the quantifying pipe, and the next quantifying of the sample for detecting the ammonia content is completed;
(4) And (3) detecting NaCl concentration: in the quantitative process of the sample in the step (3), after the six-way valve rotates anticlockwise for 60 degrees and is positioned at the first rotation position for 2-3 seconds, the feeding pump is closed, and the NaCl concentration detector is started to measure the NaCl concentration of the sample remained in the NaCl concentration detector;
(5) Dilution of the sample: after the quantification of the sample is finished in the step (3), the six-way valve is positioned at a first rotation position, the pure water pump is started again to pump pure water, the pure water enters through the six-way inlet (6) and flows into the fifth-way outlet (5), a quantified sample for ammonia content detection in a quantifying pipe which is communicated with the fifth-way outlet (5) and the second-way inlet (2) is flushed into the second-way inlet (2), the quantified sample reaches the detecting cup through the first-way outlet (1), a certain amount of pure water is pumped in once, the pure water dilutes the sample at the same time, and the pure water pump is turned off after the dilution of the sample is finished;
(6) Sample ammonia content detection: after the dilution of the sample is finished in the step (5), starting a plunger pump, sucking sulfuric acid with a certain concentration from a detection solution, dripping the sulfuric acid into the detection cup through a pipeline and a feeding end of the detection cup, wherein a PH meter is always in a detection state in the process of dripping the sulfuric acid into the detection cup, detecting a jump point to be an end point, closing the plunger pump, calculating the ammonia content in the sample through the dripped sulfuric acid, and rotating a six-way valve to an initial position after the ammonia content is detected;
(7) Ammonia-to-salt ratio calculation and result transmission: and (3) calculating the ratio of the NaCl concentration measured in the step (4) to the ammonia content measured in the step (6) through data analysis, namely obtaining the ammonia-salt ratio, and outputting the ammonia-salt ratio data to a DCS (distributed control system) through a signal line by using a signal of 4-20mA so as to carry out production control.
Compared with the prior art, the invention has the following beneficial effects:
(1) According to the ammonia-salt ratio online analyzer provided by the invention, the NaCl concentration detector and the detection cup are arranged in the main cabinet, the NaCl concentration in the sample is detected through the NaCl concentration detector after the sample is sampled through the circulating sampler, then the same batch of sample is sent into the detection cup, a certain amount of 0.1mol/L sulfuric acid is added into the sample of the detection cup and is combined with the PH meter to measure the ammonia content, the ratio of the NaCl concentration to the ammonia content is calculated through data analysis, and then the result is immediately output to the DCS system through a signal line in a 4-20mA signal mode, so that production control is performed, the online analysis of the ammonia-salt ratio is realized.
(2) The pure water cleaning can avoid the influence of residues in the detection cup on the detection result, the replacement of the sample ensures the freshness of the sample, the state of the sample is consistent with the state of ammonia brine in the production pipeline as much as possible, and the accuracy of the ammonia content detection result is ensured.
(3) According to the invention, through improving the flow passage structure of the six-way valve, the inlet and the outlet are uniformly arranged at intervals, pure water cleaning and sample replacement of the detection cup can be finished through the six-way valve, then the flow passage can be switched through rotating the six-way valve, quantification of a sample required by detecting the ammonia content can be finished through a quantifying pipe connecting the second inlet (2) and the fifth outlet (5), micro quantification of 150 mu L each time can be realized, and the sample in the quantifying pipe is flushed into the detection cup through pumping of 20mL of pure water, so that sample dilution is finished, the detection result is accurate, meanwhile, less detection solution is consumed, and high detection precision is ensured.
(4) After the detection is started, the feeding pump starts to pump the sample and replace the sample, at the moment, whether the sample is pumped or not is detected by detecting whether the sample enters the liquid level sensor from the sample inlet, if the sample is blocked by crystallization, the sample cannot be pumped, so that whether the sampling end is blocked by crystallization can be judged, the smooth progress of the analysis process is ensured, the detection accuracy is further improved, the discharging end of the discharging pump is connected with the detected material interface above the liquid level sensor, the liquid level sensor is equivalent to a three-way joint, and thus the sample entering from the sample inlet and the waste liquid in the detection cup pumped by the discharging end of the discharging pump can be discharged by sharing a discharging pipe, so that the main machine structure of the analyzer is more compact and reasonable.
(5) The ammonia water flows in from the inlet of the circulating sampler at the lower part of the circulating sampler and flows back to the production pipeline from the outlet of the circulating sampler at the upper part of the circulating sampler, and the ammonia water is sampled by the filtering membrane pipe positioned in the circulating sampler and the suction of the feeding pump, so that the normal operation of the production process is ensured, the ammonia water in the circulating sampler is always in a flowing state, the freshness of the sample is ensured, the ammonia water is extremely volatilized out of ammonia gas, and the ammonia water belongs to toxic and harmful gas, so that the closed circulating sampler is adopted, and meanwhile, the ammonia water contains more impurities and bubbles and needs to be filtered, the filtering membrane pipe is arranged in the circulating sampler, so that the sample is a cleaner sample, the detection is facilitated, the impurities and the bubbles in the ammonia water can be effectively removed through the filtration, and the detection and analysis accuracy is improved while the sampling is ensured to be fast and continuous.
(6) Through circulation sampler and charge-in pump once sampling, test NaCl concentration and ammonia content respectively, guaranteed the synchronism of detection sample to ensured the accuracy of testing result, can realize timely, accurate control to production process.
(7) The online analyzer provided by the invention eliminates various interferences through means of pure water flushing of a detection cup, replacement of a sample, quantification and dilution of the sample, setting of a liquid level sensor and the like, can ensure the accuracy of a measured value, realizes micro quantitative sampling through a six-way valve, and greatly reduces the required detection solution, namely sulfuric acid, so that the rapid detection and analysis can be ensured, the detection accuracy is ensured, and the detection accuracy can reach +/-1%.
(8) The online analyzer provided by the invention is provided with the positive pressure system, the sampling is performed by adopting the closed pressure sampling, the ammonia volatilization is prevented, meanwhile, solution crystallization blockage is not easy to be caused, compressed air is filled into the main cabinet, so that the air pressure in the main cabinet is kept at positive pressure, the effect of protecting the instrument is achieved, some corrosive gases are prevented from entering, faults in the working process of the analyzer are avoided, and the service life of the analyzer is prolonged.
Drawings
FIG. 1 is a schematic diagram of an ammonia-to-salt ratio on-line analyzer according to the present invention;
FIG. 2 is a schematic diagram of the analyzer body of FIG. 1;
FIG. 3 is a schematic diagram of the piping communication at the time of replacement of a sample in the case of performing an on-line analysis;
FIG. 4 is a schematic diagram of the quantification of a sample in an on-line analysis and the communication of tubing in a dilution;
fig. 5 is a schematic diagram of the circulation sampling device in fig. 1.
In fig. 1-5: 1-a main body cabinet; 2-cycle sampler; 21-a filtration membrane tube; 22-a recirculating sampler inlet; 23-recirculating the sampler outlet; 3-a pure water module; a 4-NaCl concentration detector; 5-a pure water pump; 6-a feed pump; 7-detecting cup; 8-a discharge pump; 9-a plunger pump; a 10-six-way valve; 11-metering tube; 12-a liquid level sensor; 13-PH meter; 14-positive pressure system; 141-a pressure reducing valve; 142-a flow meter; 15-discharging pipe; 16-analyzer mainframe.
Detailed Description
For the purpose of making apparent the objects, technical solutions and advantages of the present invention, the present invention will be further described in detail with reference to the accompanying drawings and examples, it being understood that the specific examples described herein are for illustration only and are not intended to limit the present invention.
The utility model provides an ammonia salt ratio on-line analyzer as shown in fig. 1-5, including main part cabinet 1, still including setting up in the inside analyzer host computer 16 of main part cabinet 1, pure water module 3 and NaCl concentration detector 4 of main part cabinet 1 and setting up, analyzer host computer 16 includes pure water pump 5, feed pump 6, detection cup 7, discharge pump 8, plunger pump 9 and six-way valve 10, the feeding system that forms the sample is connected gradually through the pipeline with feed pump 6 to circulating sampler 2, naCl concentration detector 4, six-way valve 10 is provided with respectively and exports (1), export (3) and five exports (5) and import (2) No. two, import (4) No. four and import (6) No. six, and the discharge end of feed pump 6 is through pipeline connection six-way valve 10's No. four import (4), and the discharge end of pure water pump 5 respectively with pure water module 3 delivery port and six-way valve 10 six-way valve 6 feed system, six-way valve 10 is connected through pipeline connection, no. two export (10) and six-way valve 10 are through pipeline connection 5) have the feed pump 3 to detect the end (7) and the discharge end is through the feed pump 15 respectively with the feed pump end (10) and is connected through the feed pump end (7) and is connected to the discharge end (10) and is connected with the feed pump end (10) and is connected through the feed pump end).
Wherein the lower part of the circulating sampler 2 is provided with a circulating sampler inlet 22 connected to a production pipeline through which ammonia brine flows, the ammonia brine in the production pipeline enters the circulating sampler 2 from the circulating sampler inlet 22, the upper part of the circulating sampler 2 is provided with a circulating sampler outlet 23, ammonia brine flows back to the production pipeline through which the ammonia brine flows from the circulating sampler outlet 23, the circulating sampler 2 is internally provided with a filtering membrane pipe 21 for filtering impurities and bubbles, the specific structure can be seen in fig. 5, the lower end of the filtering membrane pipe 21 is close to the circulating sampler inlet 22, the upper end of the filtering membrane pipe 21 is far away from the circulating sampler inlet 22 and is connected to the feeding end of the NaCl concentration detector 4 through a pipeline, the discharging end of the NaCl concentration detector 4 is connected with the feeding end of the feeding pump 6 through a pipeline, the inlet and the outlet of the six-way valve 10 are sequentially and evenly arranged at intervals in the order of inlet-outlet-inlet, the six-way valve 10 is provided with an initial position and a first rotation position, the first rotation position of the six-way valve 10 is arranged in the anticlockwise direction of the initial position, an included angle between the initial position of the six-way valve 10 and the first rotation position in the anticlockwise direction is 60 degrees, the six-way valve 10 is communicated with the first outlet (1) when the six-way valve 10 is in the initial position, the four-way inlet (4) is communicated with the five-way outlet (5), the two-way valve (2) is communicated with the three-way outlet (3), the specific structure can be seen in figure 3, the six-way valve 10 is anticlockwise rotated by 60 degrees, the six-way valve 10 is in the first rotation position, the specific structure can be seen in figure 4, when the six-way valve 10 is in the first rotation position, a second inlet (2) of the six-way valve 10 is communicated with a first outlet (1), a fourth inlet (4) is communicated with a third outlet (3), and a fifth outlet (5) is communicated with a sixth inlet (6).
In order to detect whether the circulation sampler 2 is blocked by crystallization or not and reduce the number of three-way connectors for connecting pipelines, the pipeline arrangement in the analyzer main machine 16 is more compact and reasonable, a third outlet (3) of the six-way valve 10 and the discharge end of the discharge pump 8 are commonly connected with a liquid level sensor 12, a displacement sample inlet is arranged on the left side of the liquid level sensor 12, a detected material interface is arranged above the liquid level sensor 12, a discharge port is arranged below the liquid level sensor, the third outlet (3) of the six-way valve 10 is connected with the displacement sample inlet of the liquid level sensor 12 through a pipeline, the discharge end of the discharge pump 8 is connected with the detected material interface of the liquid level sensor 12 through a pipeline, the discharge port of the liquid level sensor 12 is connected to a discharge pipe 15, a stirring device is arranged in the detection cup 7, the stirring device adopts a stirring rod driven by a micro motor, and stirring blades are arranged on the stirring rod; the PH meter 13 for measuring PH value is arranged on the detection cup 7; the positive pressure system 14 is arranged in the main body cabinet 1, the positive pressure system 14 comprises a pressure reducing valve 141 and a flowmeter 142, the analyzer adopts closed pressure sampling to prevent ammonia from volatilizing and simultaneously not easily causing solution crystallization blockage, compressed air is filled into the main body cabinet 1, so that the air pressure in the main body cabinet 1 is kept at positive pressure, the function of protecting an instrument is achieved, and corrosive gases are prevented from entering; the detection solution is sulfuric acid.
It should be noted that, whether the communication between the sixth inlet (6) and the first outlet (1), the fourth inlet (4) and the fifth outlet (5), and the second inlet (2) and the third outlet (3) of the six-way valve 10 in the initial position of the six-way valve 10 in fig. 3, or the communication between the second inlet (2) and the first outlet (1), the fourth inlet (4) and the third outlet (3), and the fifth outlet (5) and the sixth inlet (6) of the six-way valve 10 in the first rotation position of the six-way valve 10 in fig. 4 is indicated by a flow passage inside the six-way valve 10, all of which are indicated by dotted lines, and the other of which are indicated by a pipeline, the second inlet (2) and the fifth outlet (5) of the six-way valve 10 are connected by a metering tube 11, and are also indicated by solid lines.
The ammonia-salt ratio on-line analyzer provided by the invention is also provided with a display screen, a PLC (programmable logic controller), a PCB (printed circuit board) control board and a 24V switching power supply for supplying power to the same, and can output data to a DCS (distributed control system) through a signal line in a form of 4-20mA signals.
The invention provides an ammonia-salt ratio on-line analyzer, wherein a circulating sampler 2 is connected to a production pipeline through which ammonia brine flows for sampling, a pure water module 3 is connected with pure water, and the on-line analyzer mainly comprises the steps of pure water cleaning, sample replacement, sample quantification, naCl concentration detection, sample dilution, sample ammonia content detection, ammonia-salt ratio calculation, result transmission and the like during specific operation:
(1) Pure water cleaning
The step mainly aims at eliminating the interference caused by residues possibly remained in the detection cup 7 after the last sampling, detection and analysis, and particularly comprises the following steps of starting the pure water pump 5, wherein the six-way valve 10 is in an initial position, sucking pure water through a feed end of the pure water pump 5 and driving the pure water into a six-way inlet (6) of the six-way valve 10, referring to fig. 3, the six-way inlet (6) of the six-way valve 10 is communicated with the first outlet (1) during the initial position, the first outlet (1) is connected with the feed end of the detection cup 7 through a pipeline, the pure water enters the detection cup 7 through the first outlet (1), starting a stirring device in the detection cup 7 to stir the pure water after a certain amount of pure water is pumped in, cleaning the detection cup 7 is performed, the pure water for cleaning in the embodiment is 25-40 mL, then starting the discharge pump 8, and the discharge pump 8 pumps the pure water for cleaning in the detection cup 7, the discharge end of the discharge pump 8 can be directly connected to the discharge pipe 15 (the direct connection between the discharge end of the discharge pump 8 and the discharge pipe 15 is not shown), in this connection state, pure water for cleaning pumped by the discharge end of the discharge pump 8 is directly discharged through the discharge pipe 15, but in order to reduce the three-way joint for connection between the pipelines, the pipeline arrangement in the analyzer main unit 16 is more reasonable, the structure is more compact, the discharge end of the discharge pump 8 is connected to the inspected material interface of the liquid level sensor 12 through the pipeline, at this time, pure water for cleaning pumped by the discharge end of the discharge pump 8 enters the liquid level sensor 12 through the inspected material interface of the liquid level sensor 12 and is discharged to the discharge pipe 15 through the discharge port of the liquid level sensor 12, and finally, pure water cleaning is completed, and the discharge pump 8 is closed, so that interference possibly caused by the previous sampling, detection and analysis can be eliminated.
(2) Sample replacement
Referring to fig. 3 again, after the pure water cleaning is completed in step (1), the feed pump 6 is started, ammonia brine in the production pipeline is sucked and filtered through the filtering membrane pipe 21 in the circulating sampler 2 to obtain a sample, the six-way valve 10 is still at the initial position at this time, the sample is driven into the fourth inlet (4) of the six-way valve 10 by the feed pump 6 after passing through the NaCl concentration detector 4, the fourth inlet (4) of the six-way valve 10 is communicated with the fifth outlet (5) in the initial position, the fifth outlet (5) is communicated with the second inlet (2) through the metering pipe 11, the second inlet (2) is communicated with the third outlet (3), the sample is finally discharged through the third outlet (3), at this time, the sample can be directly discharged into the discharge pipe 15 and discharged (the third outlet (3 is not shown in the direct connection diagram of the discharge pipe 15), but in order to check whether the circulating sampler 2 can normally sample, namely, the sample is discharged through the third outlet (3) and the replacement sample inlet of the liquid level sensor 12 is connected through the pipeline, namely, the sample enters the liquid level sensor 12 through the third outlet (3) and enters the liquid level sensor 12 through the pipeline after being discharged through the third outlet (3) and the liquid level sensor 12, at this time, the fresh sample is discharged from the liquid section is not required to be discharged into the liquid phase 40, and the fresh sample is discharged from the liquid section (No. 25) because the fresh sample is discharged from the liquid is completely through the liquid sample is discharged from the liquid sensor through the filter pipe 21 at this stage and the time and the fresh sample section is discharged from the fresh stage is completely after the liquid is discharged through the liquid is completely after the liquid is discharged.
It should be noted that, in the above step, the discharge port of the liquid level sensor 12 is connected with the discharge pipe 15, and the liquid level sensor 12 is mainly used for detecting whether the sample liquid enters from the replacement sample inlet, at this time, the liquid level sensor detects the liquid, which indicates that the circulation sampler 2 can normally sample without being blocked by crystallization, and the detection and analysis process can be continued, otherwise, if the liquid is not detected, it can be determined that the circulation sampler 2 has been blocked by crystallization, and it is necessary to process the sample again by manual cleaning or the like.
(3) Quantification of samples
After the replacement of the sample in the step (2) is finished, the six-way valve 10 is rotated counterclockwise by 60 degrees, so that the six-way valve 10 is in a first rotation position, at this time, the second inlet (2) is communicated with the first outlet (1), the fourth inlet (4) is communicated with the third outlet (3), the fifth outlet (5) is communicated with the sixth inlet (6), and particularly, as can be seen in fig. 4, in the replacement process of the sample in the step (2), the sample circulation must pass through the quantifying tube 11 connected with the fifth outlet (5) and the second inlet (2), so that the quantifying tube 11 is filled with the sample after the sample is replaced for a period of time, the quantifying tube 11 is not communicated with the fourth inlet (4) and the third outlet (3) when the six-way valve 10 is in the first rotation position, no sample enters the quantifying tube 11, and no sample flows out of the quantifying tube 11, so that the sample in the quantifying tube 11 can be controlled in the quantifying tube 11, and the volume of the sample in the quantifying tube 11 is fixed, and the volume of the sample in the quantifying tube 11 can be calculated to obtain the volume of the sample in the quantifying tube 11, and the ammonia content in the next step of the quantifying tube 11 can be detected.
(4) NaCl concentration detection
In the quantifying process of the sample in the step (3), after the six-way valve 10 rotates counterclockwise for 60 degrees for 2-3 seconds after the first rotation position, the feed pump 6 is turned off, the sample still remains in the NaCl concentration detector 4 at this time, and the NaCl concentration detector 4 is started to measure the NaCl concentration of the sample in the sample.
(5) Dilution of samples
After the quantification of the sample is completed in the step (3), the pure water pump 5 is started again, the six-way valve 10 is at a first rotation position, the feed pump 6 is in a closed state, pure water is pumped into the pure water pump 5, the pure water flows into the fifth outlet (5) through the sixth inlet (6), a quantitative sample for ammonia content detection in the quantifying pipe 11 communicated with the fifth outlet (5) and the second inlet (2) is flushed into the second inlet (2), and the second inlet (2) is communicated with the first outlet (1), so that the pure water and the quantitative sample finally reach the detection cup 7 through the first outlet (1), a certain amount of pure water is pumped in once, the pure water pumped in once is 20mL, the pure water is diluted simultaneously, and the pure water pump 5 is closed after the dilution of the sample is completed.
(6) Sample ammonia content detection
After the sample is diluted in the step (5), the plunger pump 9 is started, sulfuric acid with a certain concentration is sucked into the detection solution and is dripped into the detection cup 7 through a pipeline and the feeding end of the detection cup 7, the sulfuric acid with the concentration of 0.1mol/L is adopted in the embodiment, the PH meter 13 is always in a detection state in the process of dripping the sulfuric acid into the detection cup 7, the detected jump point is the end point, the plunger pump 9 is closed, the ammonia content in the sample is calculated through the dripped sulfuric acid, and the six-way valve 10 is rotated to an initial position after the ammonia content detection is completed.
(7) Ammonia-salt ratio calculation and result transmission
And (3) calculating the ratio of the NaCl concentration measured in the step (4) to the ammonia content measured in the step (6) through data analysis, namely obtaining the ammonia-salt ratio, and outputting the ammonia-salt ratio data to a DCS (distributed control system) through a signal line by using a signal of 4-20mA so as to carry out production control.
The ammonia-salt ratio online analyzer provided by the invention tests according to an online analysis method of the ammonia-salt ratio, and the process conditions of a production line during the test are as follows: ammonia brine: FNH3 is 102-105tt, TCl - 90-92tt (tt is a common unit in the saline-alkali industry, and the unit is converted into 1 tt=1/20 equivalent concentration=0.85 kg/m) 3 ) The temperature is below 42 ℃, analysis is carried out every two hours from 2 am to 10 pm the next day, and the result is compared with the detection result of manual sampling as follows:
according to the data analysis, the ammonia content detected by the ammonia salt ratio on-line analyzer is less volatile due to the fact that the ammonia content is sampled in a closed environment, and the detected ammonia content is relatively close to the real condition of a production pipeline, so that the monitoring and control of the production process are facilitated.
The above examples are merely illustrative of the preferred embodiments of the present invention and do not limit the spirit and scope of the present invention. Various changes and modifications made to the technical solution of the present invention by those skilled in the art without departing from the design concept of the present invention shall fall within the protection scope of the present invention, and the technical content of the protection of the present invention is fully described in the claims.
Claims (7)
1. The utility model provides an ammonia salt ratio on-line analysis appearance, includes main part cabinet (1), its characterized in that: the device also comprises a circulating sampler (2) arranged at the outer side of the main body cabinet (1), and an analyzer host (16), a pure water module (3) and a NaCl concentration detector (4) which are arranged in the main body cabinet (1);
the lower part of the circulating sampler (2) is provided with a circulating sampler inlet (22) connected to a production pipeline through which ammonia brine flows, the upper part of the circulating sampler (2) is provided with a circulating sampler outlet (23), a filtering membrane pipe (21) for filtering impurities and bubbles is arranged in the circulating sampler (2), the lower end of the filtering membrane pipe (21) is close to the circulating sampler inlet (22), and the upper end of the filtering membrane pipe (21) is far away from the circulating sampler inlet (22) and is connected to the feeding end of the NaCl concentration detector (4) through a pipeline;
the analyzer main machine (16) comprises a pure water pump (5), a feeding pump (6), a detection cup (7), a discharge pump (8), a plunger pump (9) and a six-way valve (10), wherein the circulating sampler (2), the NaCl concentration detector (4) and the feeding pump (6) are sequentially connected through pipelines to form a feeding system of a sample, the six-way valve (10) is respectively provided with a first outlet (1), a third outlet (3) and a fifth outlet (5), and a second inlet (2), a fourth inlet (4) and a sixth inlet (6), the discharge end of the feeding pump (6) is connected with the fourth inlet (4) of the six-way valve (10) through a pipeline, the feeding end and the discharge end of the pure water pump (5) are respectively connected with the water outlet of the pure water module (3) and the six-way valve (10) through the six-way valve (6), the second inlet (2) of the six-way valve (10) is communicated with the fifth outlet (5) through a metering pipe (11), the first outlet (10) of the six-way valve (10) is connected with the discharge end of the plunger pump (7) through the detection cup (7) through the detection pipe (7), and the discharge end of the discharge pump (9) is respectively connected with the discharge end of the discharge pump (15 through the discharge end of the discharge pump (8);
the inlet and the outlet of the six-way valve (10) are sequentially and evenly arranged at intervals according to the sequence of inlet, outlet and inlet, the six-way valve (10) is provided with an initial position and a first rotation position, an included angle between the initial position and the first rotation position of the six-way valve (10) along the anticlockwise direction is 60 degrees, a six-way inlet (6) of the six-way valve (10) is communicated with a first outlet (1) when the six-way valve (10) is positioned at the initial position, a four-way inlet (4) is communicated with a five-way outlet (5), a two-way inlet (2) is communicated with a three-way outlet (3), a two-way inlet (2) of the six-way valve (10) is communicated with a first outlet (1) when the six-way valve (10) is positioned at the first rotation position, a four-way inlet (4) is communicated with a three-way outlet (3), and a five-way outlet (5) is communicated with a six-way inlet (6).
The three-way valve is characterized in that a third outlet (3) of the six-way valve (10) and a discharge end of the discharge pump (8) are connected with a liquid level sensor (12) together, a displacement sample inlet is formed in the left side of the liquid level sensor (12), a detected material interface is formed in the upper side of the liquid level sensor, a discharge outlet is formed in the lower side of the liquid level sensor, the third outlet (3) of the six-way valve (10) is connected with the displacement sample inlet of the liquid level sensor (12) through a pipeline, the discharge end of the discharge pump (8) is connected with the detected material interface of the liquid level sensor (12) through a pipeline, and the discharge outlet of the liquid level sensor (12) is connected to a discharge pipe (15).
2. An ammonia-to-salt ratio on-line analyzer as defined in claim 1, wherein: and a stirring device is arranged in the detection cup (7).
3. An ammonia-to-salt ratio on-line analyzer as defined in claim 1, wherein: the detection cup (7) is provided with a PH meter (13) for measuring PH value.
4. An ammonia-to-salt ratio on-line analyzer as defined in claim 1, wherein: a positive pressure system (14) is arranged in the main body cabinet (1), and the positive pressure system (14) comprises a pressure reducing valve (141) and a flowmeter (142).
5. An ammonia-to-salt ratio on-line analyzer as defined in claim 1, wherein: the detection solution is sulfuric acid.
6. An ammonia-to-salt ratio on-line analyzer as defined in claim 1, wherein: the intelligent control system also comprises a display screen, a PLC controller, a PCB control board and a power supply for supplying power to the PLC controller, and can output data to the DCS system through a signal line.
7. An on-line analysis method of ammonia-to-salt ratio according to any one of claims 1 to 6, characterized in that: the method comprises the following steps:
(1) Cleaning with pure water: starting a pure water pump (5), at the moment, a six-way valve (10) is in an initial position, sucking pure water through a feeding end of the pure water pump (5) and pumping the pure water into a six-way inlet (6) of the six-way valve (10), sending the pure water into a detection cup (7) through a first outlet (1), after pumping a certain amount of pure water, starting a stirring device in the detection cup (7) to stir the pure water, cleaning the detection cup (7), starting a discharge pump (8) to pump the pure water for cleaning in the detection cup (7), enabling the pure water to enter a liquid level sensor (12) through a detected material interface of the liquid level sensor (12), discharging the pure water into a discharge pipe (15) through a discharge port of the liquid level sensor (12), and closing the discharge pump (8);
(2) Replacement of samples: after the pure water is cleaned in the step (1), starting a feed pump (6), sucking and filtering the pure water through a filtering membrane pipe (21) in a circulating sampler (2) to obtain a sample, wherein the six-way valve (10) is at an initial position, the sample is driven into a fourth inlet (4) of the six-way valve (10) by the feed pump (6) after passing through a NaCl concentration detector (4), enters the liquid level sensor (12) from a replacement sample inlet of the liquid level sensor (12) through a fifth outlet (5), a quantitative pipe (11) and a second inlet (2), the liquid level sensor (12) detects whether the sample enters or not, the sample entering the liquid level sensor (12) is discharged into a discharge pipe (15) through a discharge port of the liquid level sensor (12), the replacement of the sample is completed, and the replacement time of the sample is controlled to be 25-40 seconds;
(3) Quantification of samples: after the replacement of the sample in the step (2) is finished, a quantifying pipe (11) connected with a fifth outlet (5) and a second inlet (2) is filled with the sample, the six-way valve (10) is rotated anticlockwise by 60 degrees, the six-way valve (10) is positioned at a first rotation position, the sample in the quantifying pipe (11) is controlled in the quantifying pipe (11), the volume of the sample in the quantifying pipe (11) is calculated through the volume of the quantifying pipe (11), and the next quantifying of the sample for detecting the ammonia content is completed;
(4) And (3) detecting NaCl concentration: in the quantitative process of the sample in the step (3), after the six-way valve (10) rotates anticlockwise for 60 degrees and is positioned at the first rotation position for 2-3 seconds, the feeding pump (6) is closed, and the NaCl concentration detector (4) is started to measure the NaCl concentration of the sample remained in the NaCl concentration detector (4);
(5) Dilution of the sample: after the quantification of the sample is finished in the step (3), the six-way valve (10) is positioned at a first rotation position, the pure water pump (5) is started again to pump pure water, the pure water enters through the sixth inlet (6) and flows to the fifth outlet (5), a quantified sample for ammonia content detection in the quantifying pipe (11) communicated with the fifth outlet (5) and the second inlet (2) is flushed into the second inlet (2), the quantified sample reaches the detecting cup (7) through the first outlet (1), a certain amount of pure water is pumped in once, the pure water dilutes the sample at the same time, and the pure water pump (5) is closed after the dilution of the sample is finished;
(6) Sample ammonia content detection: after the sample is diluted in the step (5), starting a plunger pump (9), sucking sulfuric acid with a certain concentration from a detection solution, dripping the sulfuric acid into the detection cup (7) through a pipeline and a feeding end of the detection cup (7), wherein a PH meter (13) is always in a detection state in the process of dripping the sulfuric acid into the detection cup (7), detecting a jump point to be an end point, closing the plunger pump (9), calculating the ammonia content in the sample through the dripped sulfuric acid, and rotating a six-way valve (10) to an initial position after the ammonia content detection is finished;
(7) Ammonia-to-salt ratio calculation and result transmission: and (3) calculating the ratio of the NaCl concentration measured in the step (4) to the ammonia content measured in the step (6) through data analysis, namely obtaining the ammonia-salt ratio, and outputting the ammonia-salt ratio data to a DCS (distributed control system) through a signal line by using a signal of 4-20mA so as to carry out production control.
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