CN216747423U - Device for measuring chloride ions in polymeric ferric sulfate solution - Google Patents
Device for measuring chloride ions in polymeric ferric sulfate solution Download PDFInfo
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- CN216747423U CN216747423U CN202220211308.0U CN202220211308U CN216747423U CN 216747423 U CN216747423 U CN 216747423U CN 202220211308 U CN202220211308 U CN 202220211308U CN 216747423 U CN216747423 U CN 216747423U
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Abstract
The utility model belongs to the technical field of analysis and detection, and relates to a device for measuring chloride ions in a polymeric ferric sulfate solution, which comprises a reaction tank, a filter, a precipitation reaction tank, a burette and a potassium chromate replenishing pipe; the reaction tank is arranged above the filter and is communicated with the filter; the bottom of the filter is provided with a filtering outlet; the sedimentation reaction tank is arranged below the filter; the burette and the potassium chromate replenishing pipe are arranged in parallel, and one end of the burette and one end of the potassium chromate replenishing pipe are both arranged in the precipitation reaction tank; and an ammonia water replenishing pipe with one end extending into the reaction tank is arranged on the reaction tank. The utility model can carry out blank test check, reduce the measurement error, improve the measurement accuracy, has high detection speed and ensures the safe and economic operation of the unit.
Description
Technical Field
The utility model belongs to the technical field of analysis and detection, relates to a chloride ion determination device, and particularly relates to a chloride ion determination device in a polymeric ferric sulfate solution.
Background
In the operation of the high-efficiency ultra-supercritical unit, the content of chloride ions such as high mixing, water supply and the like in a water vapor system often exceeds the standard, great hidden danger is brought to the safe operation of the unit, and through repeated searching and analysis, the condition that the coagulant used in the deep treatment of the regenerated water carries a large amount of chloride ions is judged.
Polyferric sulfate, a novel efficient inorganic polymeric flocculant, is prepared by taking iron oxide as a raw material, and dissolving, oxidizing, hydrolyzing and polymerizing by sulfuric acid to obtain product polyferric sulfate; however, in the actual production process of the polymeric ferric sulfate, partial hydrochloric acid is adopted, and chloride ions in the hydrochloric acid are accumulated in the polymeric ferric sulfate solution and enter a unit thermodynamic system along with the treatment of regenerated water. Chloride ions are corrosive anions which have the greatest harm to thermal equipment and are main corrosive ions for promoting pitting corrosion of a water wall, accidents such as boiler tube explosion, blade fracture of a steam turbine, and austenitic steel grain boundary corrosion of a superheater and a reheater can be caused when the content of the chloride ions in water vapor exceeds the standard, so that not only are safety accidents frequent, but also energy conservation and consumption reduction are not facilitated, and the safe and economic operation of a unit is seriously influenced. Therefore, the content of chloride ions in a water vapor system such as thermal power plant thermal equipment is an important monitoring index.
The existing chloride ion detection method can measure the content of chloride ions in a solution, but has the following problems when measuring in a polymeric ferric sulfate solution: (1) the coagulant polyferric sulfate solution is a reddish-brown solution, the disclosed chloride ion determination method is to determine a colorless solution, and the color of the solution influences the determination result; (2) most of the existing chloride ion measurement is carried out by using a potentiometric titration instrument, but the measurement accuracy is not checked in the detection process, so that the measurement result has large error and low accuracy.
SUMMERY OF THE UTILITY MODEL
Aiming at the technical problems existing in the determination of chloride ions in the existing polymeric ferric sulfate solution, the utility model provides the device for determining chloride ions in the polymeric ferric sulfate solution, which can reduce determination errors by eliminating interfering ions, performing blank test checking and the like, improve determination accuracy, realize high detection speed and ensure the safe and economic operation of a unit.
In order to achieve the purpose, the utility model adopts the technical scheme that:
a device for measuring chloride ions in a polymeric ferric sulfate solution comprises a reaction tank, a filter, a precipitation reaction tank, a burette and a potassium chromate replenishing pipe; the reaction tank is arranged above the filter and is communicated with the filter; the bottom of the filter is provided with a filtering outlet; the sedimentation reaction tank is arranged below the filter and communicated with the filtering outlet; the burette and the potassium chromate replenishing pipe are arranged in parallel, and one end of the burette and one end of the potassium chromate replenishing pipe are both arranged in the precipitation reaction tank; and an ammonia water replenishing pipe with one end extending into the reaction tank is arranged on the reaction tank.
Further, a stirrer with one end extending into the reaction tank is arranged above the reaction tank; the stirrer and the ammonia water replenishing pipe are arranged in parallel.
Further, a control valve is arranged between the reaction tank and the filter.
Further, the filter is also provided with a washing water inlet.
Furthermore, the device for measuring chloride ions in the polymeric ferric sulfate solution also comprises a pH meter with one end arranged in the precipitation reaction tank.
Furthermore, the device for measuring chloride ions in the polymeric ferric sulfate solution also comprises a sulfuric acid replenishing pipe, one end of which extends into the precipitation reaction tank; the sulfuric acid replenishing pipe is parallel to the burette.
Furthermore, the device for measuring chloride ions in the polymeric ferric sulfate solution also comprises a sodium hydroxide replenishing pipe, one end of which extends into the precipitation reaction tank; the sodium hydroxide replenishing pipe is parallel to the burette.
Furthermore, a drain pipe communicated with the inner part of the sedimentation reaction tank is arranged at the bottom of the sedimentation reaction tank.
Furthermore, a valve is arranged on the water drain pipe.
The utility model has the beneficial effects that:
1. the measuring device provided by the utility model comprises a reaction tank, a precipitation reaction tank, a filter and a burette; the device combining precipitation, separation, filtration and titration is adopted, manual titration is adopted, and meanwhile a blank test is carried out, so that errors are eliminated, and the accuracy is improved; meanwhile, the technical blank of the existing project in the national standard for acceptance of polymeric ferric sulfate is filled, the operation steps are simple, the popularization is easy, and the difficulty is low.
2. By adopting the device, the content of chloride ions in a polymeric ferric sulfate solution can be detected in time, the quality of coagulant drugs can be improved, and the coagulant drugs can be processed in time when the chloride ions exceed the standard, so that unqualified flocculant containing a large amount of chloride ions is prevented from entering makeup water treatment equipment, the frequency of corrosion accidents is greatly reduced, unsafe events such as non-stop of a unit and the like caused by leakage of four pipes of a boiler, pipe explosion, serious salt accumulation of blades of a steam turbine and the like due to serious corrosion are effectively prevented, the corrosion of water vapor system equipment by the chloride ions is avoided, and the safe and economic operation of the unit is ensured.
3. The chloride ion measuring device provided by the utility model is simple to operate, can be used for rapidly measuring the content of chloride ions, so that the phenomenon that over-standard chloride ions enter a thermodynamic system to cause scaling corrosion is prevented, and the device has high popularization value.
4. The method can ensure that the water quality is qualified after measurement, prolong the operation period of water treatment equipment, improve the period water production, reduce the regeneration times and save a large amount of acid and alkali waste every year; meanwhile, the scale formation, corrosion and salt deposition of a thermodynamic system are effectively prevented, the pipe replacement cost is saved, and great economic benefits are generated.
Drawings
FIG. 1 is a schematic view of an apparatus according to the present invention;
wherein:
1-ammonia water replenishing pipe; 2-a stirrer; 3-a reaction tank; 4-a filter; 5-burette; 6-potassium chromate replenishing pipe; 7-sulfuric acid replenishing pipe; 8-a pH meter; 9-sodium hydroxide replenishing pipe; 10-a precipitation reaction tank; 11-a valve; 12-a drain pipe; 13-control valve.
Detailed Description
The present invention will now be described in detail with reference to the accompanying drawings and examples.
Examples
Referring to fig. 1, the device for measuring chloride ions in a polymeric ferric sulfate solution provided in this embodiment includes a reaction tank 3, a filter 4, a precipitation reaction tank 10, a burette 5 and a potassium chromate replenishing pipe 6; the reaction tank 3 is arranged above the filter 4 and is communicated with the filter 4; the bottom of the filter 4 is provided with a filtering outlet; the precipitation reaction tank 10 is arranged below the filter 4 and is communicated with the filtering outlet; the burette 5 and the potassium chromate replenishing pipe 6 are arranged in parallel, and one end of the burette 5 and one end of the potassium chromate replenishing pipe 6 are both arranged in the precipitation reaction tank 10.
In this embodiment, the reaction tank 3 is provided with an ammonia water replenishing pipe 1 having one end extending into the reaction tank 3. A stirrer 2 with one end extending into the reaction tank 3 is arranged above the reaction tank 3; the stirrer 2 is arranged in parallel with the ammonia water replenishing pipe 1. A control valve 13 is arranged between the reaction tank 3 and the filter 4. The filter 4 is also provided with a washing water inlet.
The device for measuring the chloride ions in the polymeric ferric sulfate solution also comprises a pH meter 8, one end of which is arranged in the precipitation reaction tank 10. A sulfuric acid replenishing pipe 7 with one end extending into the precipitation reaction tank 10; the sulfuric acid replenishing pipe 7 is parallel to the burette 5. A sodium hydroxide replenishing pipe 9 with one end extending into the precipitation reaction tank 10; the sodium hydroxide replenishing pipe 9 is parallel to the burette 5.
In this embodiment, the bottom of the precipitation reaction tank 10 is provided with a drain pipe 12 communicated with the interior of the precipitation reaction tank 10, and the drain pipe 12 is provided with a valve 11.
In the embodiment, the reaction tank 3 is a container with an opening at the top, the filter 4 is a conical container with a downward tip, the bottom of the reaction tank 3 is communicated with the top of the filter 4, a control valve 13 is arranged at the communication position of the reaction tank 3 and the filter 4, so that a reaction product in the reaction tank 3 can conveniently flow into the filter 4, and the reaction tank 3 is communicated with the filter 4 below the reaction tank 3 through the control valve 13; the bottom of the filter 4 is provided with a filtering outlet, the cross section inside the filter 4 is provided with a filtering layer which can adopt filter paper, the side wall of the upper part of the filter 4 is provided with a washing water inlet communicated with the inside of the filter 4, and the washing water inlet is externally connected with a high-purity water pipeline. The washing water inlet is arranged above the filter layer.
The top of the reaction tank 3 is provided with a stirrer 2 and an ammonia water replenishing pipe 1 which are parallel, and the bottom of the stirrer 2 is arranged in the reaction tank 3 and is used for stirring the solution in the reaction tank 3; one end of the ammonia water replenishing pipe 1 extends into the reaction tank 3, the other end of the ammonia water replenishing pipe is arranged outside the reaction tank 3, and 25% of ammonia water is filled in the ammonia water replenishing pipe 1.
In this embodiment, the sedimentation reaction tank 10 is open at the topThe container (2) is characterized in that a burette 5, a potassium chromate replenishing pipe 6, a sulfuric acid replenishing pipe 7 and a sodium hydroxide replenishing pipe 9 which are parallel to each other are arranged in a precipitation reaction tank 10; and the tops of the four solution pipes are arranged outside the precipitation reaction tank 10, and the bottoms of the four solution pipes are arranged in the precipitation reaction tank 10. The burette 5 was filled with 1 ml-1 mg CL-AgNO of3In the standard solution, a potassium chromate replenishing pipe 6 is filled with 10% potassium chromate solution, and a sulfuric acid replenishing pipe 7 is filled with 0.1mol/L sulfuric acid solution; the sodium hydroxide replenishment pipe 9 was filled with a 0.1mol/L sodium hydroxide solution.
The measurement apparatus provided in this example was based on the principle of chloride ion measurement and the measurement procedure as follows.
The determination principle is as follows: measuring chloride ions in the coagulant polyferric sulfate solution, firstly carrying out decoloration treatment to eliminate interfering ions, then adding ammonia water to react iron ions in the coagulant polyferric sulfate solution with the ammonia water to generate ferric hydroxide precipitate, and filtering to remove the iron ions; the final chloride ion in solution was 1 mg CL to 1 ml CL-AgNO of3And (3) titrating the standard solution, wherein in a neutral solution with the pH value of about 7, chloride ions react with silver nitrate at normal temperature to generate AgCl precipitate, and excessive silver nitrate reacts with potassium chromate to generate red silver chromate precipitate, so that the solution is orange, namely the titration end point. And calculating to obtain the content of chloride ions in the coagulant polyferric sulfate solution. The specific chemical reaction is as follows:
Fe3++3NH3·H2O＝Fe(OH)3↓+3NH4+
Cl-+Ag+→ AgCl ↓ (white)
2Ag++CrO4 2-→Ag2CrO4↓ (red).
The specific determination steps comprise:
1) diluting solution
Adding a sample to be detected (a coagulant polymeric ferric sulfate solution) into a reaction tank 3, adding high-purity water, and stirring by using a stirrer 2, wherein the mixing ratio of the sample to be detected to the high-purity water is 0.2 ml: 10 ml of water;
2) precipitating iron ions
Dropwise adding 25% ammonia water into the reaction tank 3 through the ammonia water replenishing pipe 1, adding the ammonia water while stirring through the stirrer 2, and enabling iron ions in the sample to be detected to completely react with the ammonia water to generate precipitates; at this time, the control valve 13 is closed;
3) separation washing
After the sediment is completely settled and layered, opening the control valve 13, putting the sediment into the filter 4, introducing high-purity water into a washing water inlet to fully wash the sediment, and after the sediment is filtered by a filter layer, enabling filtrate and washing liquid to flow into a precipitation reaction tank 10 below the filter 4 from a filtering outlet;
4) adjusting the pH
Adding 2 drops of 1% phenolphthalein indicator into a precipitation reaction tank 10, dropwise adding 0.1mol/L sodium hydroxide solution into the precipitation reaction tank 10 through a sodium hydroxide supplementing pipe 9 until the solution is red, and dropwise adding 0.1mol/L sulfuric acid solution into the precipitation reaction tank 10 through a sulfuric acid supplementing pipe 7 until the solution is colorless; when the pH value is adjusted, the method adopts
5) Titration
Adding 10% potassium chromate solution into the precipitation reaction tank 10 through a potassium chromate replenishing pipe 6 (1 ml of potassium chromate solution is added into each 0.2 ml of sample to be detected), and dropwise adding AgNO into the precipitation reaction tank 10 through a burette 53Standard solution, until the solution was orange by dripping, the consumption of AgNO was recorded3The volume of the solution is a ml.
During the titration, in a neutral solution with the pH value of about 7, chloride ions react with silver nitrate at normal temperature to generate AgCL precipitates, and excessive silver nitrate reacts with potassium chromate to generate red silver chromate precipitates, so that the solution is orange, namely the titration end point. At the moment, the pH value of the solution is detected by using the test paper and the pH meter 8 simultaneously, the pH value is about 7 when the solution is dripped, and the accuracy of a measuring result is high.
Simultaneously carrying out blank experiments (without adding a sample to be tested) according to the steps 1) to 5), and recording the consumption of AgNO3Volume of solution a0And (4) milliliters.
6) Computing
And calculating to obtain the content X of the chloride ions in the polymeric ferric sulfate solution. The calculation formula is as follows:
in the above formula:
the content of X-chloride ion is mg/L;
(a-consumption of AgNO by polymeric ferric sulfate solution3The volume of the solution;
a0blank test consumption AgNO3Volume of solution.
Specifically, by adopting the measuring device provided by the utility model, 2 660MW units are subjected to data observation and analysis for nearly 2 years of operation, the content of chloride ions in a water vapor system is greatly reduced, the qualification rate is greatly improved, and through tests, main factors influencing the standard exceeding of the chloride ions in the water vapor system are found, the abnormity that the content of chloride ions such as high mixing, water supply and the like in the water vapor system in the unit operation seriously exceeds the standard is thoroughly solved, and the win-win effects of water vapor quality optimization qualification and safe production are achieved.
The data of one set is taken as an example for detailed description.
1. The change trend of the chloride ion content of the water vapor system of the unit is shown in the table 1.
As can be seen from Table 1, the determination device provided by the utility model is used for determining the content of chloride ions in the flocculating agent polyferric sulfate, prejudging in advance, preventing the flocculating agent containing a large amount of chloride ions from entering the unit, greatly reducing the content of chloride ions in a water vapor system of the unit, and avoiding damage to the unit and corrosion of equipment.
TABLE 1 chloride ion Change trends of the units
2. Save a large amount of drug purchase cost
Before the device and the measuring method are not adopted, the purchased polymeric ferric sulfate is high in cost, after the measuring method of the device is implemented, the polymeric ferric sulfate purchased in each batch is tested for the content of chloride ions, the excessive polymeric ferric sulfate is found, the product is returned in time and is arranged in a blacklist, a manufacturer is forced to improve the production process, the cost is reduced, and the total cost of purchasing medicines is saved by 30 ten thousand yuan per year.
3. The scaling and corrosion rate of the unit is obviously reduced
After the device disclosed by the utility model is used for measurement, the scaling and corrosion of the economizer and the water-cooled wall are obviously reduced. In the overhaul of a 660MW unit, when chemical supervision and inspection are carried out on a thermodynamic system, the scaling and deposition rates of an economizer, a water-cooled wall, a superheater and a reheater are obviously lower than those before the method is implemented, and the scaling amount of the fire facing side of the economizer and the water-cooled wall reaches a class of standard. See table 2 for specific data.
TABLE 2 test data of unit overhaul pipe sample
4. Saves the consumption of acid and alkali
Because the water quality is qualified, the chloride ions prolong the operation period of water treatment equipment and high mixing, improve the periodic water production, reduce the regeneration times and save 15 ten thousand yuan of acid-base waste every year.
5. Saves a large amount of funds for replacing the pipe
After the chloride ion index is qualified, scaling, corrosion and salt accumulation of a thermodynamic system are effectively prevented, pipe replacement caused by four-pipe leakage, severe corrosion of a steam turbine and the like due to scaling and corrosion is avoided, and about 50 ten thousand yuan of pipe cost is saved.
6. Avoid the loss caused by the non-stop of the machine set
After the device disclosed by the utility model is used for measuring, the quality of a coagulant medicine can be improved, the content of chloride ions in a water vapor system is effectively reduced, the occurrence frequency of corrosion accidents is greatly reduced, the huge loss caused by unsafe events such as non-stop of a unit and the like caused by the explosion of four pipes of a boiler, serious salt accumulation of a turbine blade and the like of water vapor system equipment due to serious standard exceeding of the chloride ions is avoided, and the safe operation of the unit is ensured.
7. Simple operation and high popularization value
The chloride ion measuring device provided by the utility model is simple to operate, can be used for rapidly measuring the content of chloride ions, so that the phenomenon that excessive chloride ions enter a thermodynamic system to cause scaling corrosion is prevented, and the chloride ion measuring device has high popularization value.
Adopt above-mentioned device, can in time detect out the chloride ion content in the coagulant polyferric sulfate solution, can in time return goods when the chloride ion exceeds standard, avoided containing a large amount of chloride ion's unqualified flocculating agent, along with the recycled water gets into the feedwater treatment facility, corrode steam system equipment, ensured the safety of unit, economic operation, avoided leaking because of corroding the boiler four-tube that causes seriously, accident such as blow out.
According to the chloride ion measuring device, through a device combining precipitation, separation, filtration and titration, manual titration is adopted, and meanwhile, a blank test is carried out, so that errors are eliminated, and the accuracy is improved; meanwhile, the technical blank of the existing project in the national standard is filled, the operation steps are simple, the popularization is easy, and the difficulty is low.
Claims (9)
1. A device for measuring chloride ions in a polymeric ferric sulfate solution is characterized by comprising a reaction tank (3), a filter (4), a precipitation reaction tank (10), a burette (5) and a potassium chromate replenishing pipe (6); the reaction tank (3) is arranged above the filter (4) and is communicated with the filter (4); the bottom of the filter (4) is provided with a filtering outlet; the sedimentation reaction tank (10) is arranged below the filter (4) and is communicated with the filtering outlet; the burette (5) and the potassium chromate replenishing pipe (6) are arranged in parallel, and one end of the burette (5) and one end of the potassium chromate replenishing pipe (6) are both arranged in the precipitation reaction tank (10); an ammonia water replenishing pipe (1) with one end extending into the reaction tank (3) is arranged on the reaction tank (3).
2. The device for measuring the chloride ions in the polymeric ferric sulfate solution according to claim 1, wherein a stirrer (2) with one end extending into the reaction tank (3) is arranged above the reaction tank (3); the stirrer (2) and the ammonia water replenishing pipe (1) are arranged in parallel.
3. The apparatus for determining chloride ions in polymeric ferric sulfate solution according to claim 2, wherein a control valve (13) is arranged between the reaction cell (3) and the filter (4).
4. The apparatus for detecting chloride ions in polymeric ferric sulfate solution as claimed in claim 3, wherein the filter (4) is further provided with a washing water inlet.
5. The apparatus for measuring chloride ions in a polymeric ferric sulfate solution according to any one of claims 1 to 4, wherein the apparatus further comprises a pH meter (8) having one end disposed in the precipitation reaction tank (10).
6. The apparatus for measuring chloride ion in polymeric ferric sulfate solution according to claim 5, further comprising a sulfuric acid replenishing pipe (7) having one end extended into the precipitation reaction tank (10); the sulfuric acid replenishing pipe (7) is parallel to the burette (5).
7. The apparatus for measuring chloride ion in polymeric ferric sulfate solution according to claim 6, wherein the apparatus further comprises a sodium hydroxide replenishing pipe (9) having one end extending into the precipitation reaction tank (10); the sodium hydroxide replenishing pipe (9) is parallel to the burette (5).
8. The device for detecting the chloride ions in the polymeric ferric sulfate solution as claimed in claim 7, wherein the bottom of the precipitation reaction tank (10) is provided with a drain pipe (12) communicated with the interior of the precipitation reaction tank (10).
9. The apparatus for detecting chloride ion in polymeric ferric sulfate solution as claimed in claim 8, wherein the drain pipe (12) is provided with a valve (11).
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| Application Number | Priority Date | Filing Date | Title |
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| CN202220211308.0U CN216747423U (en) | 2022-01-25 | 2022-01-25 | Device for measuring chloride ions in polymeric ferric sulfate solution |
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| CN202220211308.0U CN216747423U (en) | 2022-01-25 | 2022-01-25 | Device for measuring chloride ions in polymeric ferric sulfate solution |
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