CN115015344B - System and method for full-automatic online measurement of pH of suspended reaction liquid in reaction kettle - Google Patents
System and method for full-automatic online measurement of pH of suspended reaction liquid in reaction kettle Download PDFInfo
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- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N27/00—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means
- G01N27/26—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means by investigating electrochemical variables; by using electrolysis or electrophoresis
- G01N27/28—Electrolytic cell components
- G01N27/30—Electrodes, e.g. test electrodes; Half-cells
- G01N27/302—Electrodes, e.g. test electrodes; Half-cells pH sensitive, e.g. quinhydron, antimony or hydrogen electrodes
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D29/00—Filters with filtering elements stationary during filtration, e.g. pressure or suction filters, not covered by groups B01D24/00 - B01D27/00; Filtering elements therefor
- B01D29/01—Filters with filtering elements stationary during filtration, e.g. pressure or suction filters, not covered by groups B01D24/00 - B01D27/00; Filtering elements therefor with flat filtering elements
- B01D29/03—Filters with filtering elements stationary during filtration, e.g. pressure or suction filters, not covered by groups B01D24/00 - B01D27/00; Filtering elements therefor with flat filtering elements self-supporting
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D29/00—Filters with filtering elements stationary during filtration, e.g. pressure or suction filters, not covered by groups B01D24/00 - B01D27/00; Filtering elements therefor
- B01D29/62—Regenerating the filter material in the filter
- B01D29/66—Regenerating the filter material in the filter by flushing, e.g. counter-current air-bumps
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N27/00—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means
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- G01N27/00—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means
- G01N27/26—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means by investigating electrochemical variables; by using electrolysis or electrophoresis
- G01N27/28—Electrolytic cell components
- G01N27/30—Electrodes, e.g. test electrodes; Half-cells
- G01N27/38—Cleaning of electrodes
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- G—PHYSICS
- G05—CONTROLLING; REGULATING
- G05B—CONTROL OR REGULATING SYSTEMS IN GENERAL; FUNCTIONAL ELEMENTS OF SUCH SYSTEMS; MONITORING OR TESTING ARRANGEMENTS FOR SUCH SYSTEMS OR ELEMENTS
- G05B19/00—Programme-control systems
- G05B19/02—Programme-control systems electric
- G05B19/04—Programme control other than numerical control, i.e. in sequence controllers or logic controllers
- G05B19/05—Programmable logic controllers, e.g. simulating logic interconnections of signals according to ladder diagrams or function charts
- G05B19/058—Safety, monitoring
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- G—PHYSICS
- G05—CONTROLLING; REGULATING
- G05D—SYSTEMS FOR CONTROLLING OR REGULATING NON-ELECTRIC VARIABLES
- G05D21/00—Control of chemical or physico-chemical variables, e.g. pH value
- G05D21/02—Control of chemical or physico-chemical variables, e.g. pH value characterised by the use of electric means
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Abstract
The invention discloses a system and a method for full-automatic online measurement of pH of a suspension reaction liquid in a reaction kettle, which comprises a measuring device for measuring the suspension reaction liquid in the reaction kettle, wherein a real-time circulating system is formed between the measuring device and the reaction kettle, the whole measurement is controlled by an automatic system, a PLC program is used for controlling the whole process, and the system comprises the steps of online extracting and filtering a reaction solution with suspension particles, online measuring the pH and uploading numerical values, automatically washing a pH electrode, automatically injecting a buffer solution to protect the pH electrode, automatically controlling the flow of alkali (acid) added into the reaction kettle to adjust the pH value of the reaction liquid, and automatically indicating the process.
Description
Technical Field
The invention belongs to the technical field of solution detection, and particularly relates to a system and a method for full-automatic online measurement of pH of a suspension reaction solution in a reaction kettle.
Background
The existing online pH value detection device aims at that a reaction system is a pure solution system, cannot contain colloid and suspended particles, and only considers the temperature and concentration of the solution of the reaction system and the related influence of other ions;
the pH measurement reflects an ion diffusion dynamic balance process, the composition, state, flowing speed, environment and the like of materials in a reaction kettle have great influence on the industrial online pH value measurement result, particularly when suspended particles or colloidal substances exist in a reaction system product, because of the influence of liquid junction potential and flowing potential, the pH value is difficult to accurately measure in the research of colloid chemistry and analytical chemistry, and the online direct measurement of the pH value of a solution with suspended particles in the reaction kettle is more difficult.
And current on-line measuring pH device is directly installed or will detect the electrode and go deep into reation kettle depths installation on being detected the trunk line of liquid in production technology, lacks the calibration and washing and the maintenance link of electrode, causes the online pH to measure inaccurately and the loss of electrode great in the actual production, has shortened the life of pH electrode greatly, and this is undoubtedly also not little cost-consuming.
Therefore, a system and a method for full-automatic online measurement of the pH of a suspension reaction solution in a reaction kettle are provided.
Disclosure of Invention
The invention aims to provide a system and a method for fully-automatically measuring the pH value of a suspension reaction liquid in a reaction kettle on line, which aim to solve the technical problems that the prior technologies for measuring the pH value on line are mostly single pH value measurement, or only comprise an electrode washing process after measurement, and do not solve a series of problems of solution pretreatment, measurement result use, electrode maintenance, acid or alkali addition, process control and the like in a whole way, namely, all links of the whole process of pH measurement and reaction control are not connected in series by an industrial automatic control technology, so that the labor cost is reduced, and the labor productivity is improved to the maximum extent.
In order to solve the technical problems, the specific technical scheme of the system for full-automatic online measurement of the pH of the suspension reaction liquid in the reaction kettle is as follows: including reation kettle, be equipped with in the reation kettle and carry out filterable filter head to suspension reaction liquid, its filter head is connected on the liquid suction pipe, but install the drawing liquid pump of positive and negative extraction on the liquid suction pipe, the solution inflow pipe is connected to the liquid suction pipe other end, the solution inflow pipe runs through the setting on the lateral wall of big container, be equipped with the small container in the big container, be equipped with the pH meter probe in the small container, the pH meter probe can reciprocate through the elevating gear who is connected with it, be connected with the lateral conduit on the solution inflow pipe, solution flows into the small container simultaneously through the lateral conduit, the pH meter probe can be in the small container measuring solution flow and the instant condition of reflection solution, its reation kettle, pH meter probe, drawing liquid pump, elevating gear all are connected with control system, be equipped with the solution outflow pipe on the big container, when solution reaches solution outflow pipe height, flow back to reation kettle through the pipeline.
Further, the filter head includes the frame string bag, the inner chamber of frame string bag is equipped with the balancing weight that makes things convenient for the filter head to sink into the reation kettle solution, and the peripheral cladding of frame string bag has the filter screen.
Furthermore, a cleaning water pipe is arranged in the large container, a plurality of water spraying pipe ports are formed in the cleaning water pipe, the water spraying pipe ports penetrate through and extend into the small container, the top end of the cleaning water pipe is connected with a cleaning water pump pipe, the cleaning water pump pipe is connected with a cleaning water pump, and the cleaning water pump is connected with a control system.
Furthermore, be equipped with the drinking-water pipe that is used for extracting washing back water in the small container, its drinking-water pipe other end is connected the water pump pipe that draws water, and the other end of water pump pipe is connected the water pump that draws water, the water pump that draws water is connected with control system.
Further, the pH meter probe comprises a pH electrode and a transmitter, the transmitter is used for transmitting the pH measured value to a control system, and a pH electrode glass ball is arranged at the bottom end of the pH electrode.
Furthermore, a buffer solution pipe is arranged in the small container, the other end of the buffer solution pipe is connected with a buffer solution water pump pipe, the other end of the buffer solution water pump pipe is connected with a buffer solution water pump, the buffer solution water pump is connected with a control system to pump buffer solution, the buffer solution enters the small container through the buffer solution water pump pipe and the buffer solution pipe, and the part above the pH electrode glass ball is immersed in the buffer solution water pump pipe and the buffer solution pipe to protect the pH electrode.
Further, the control system is a PLC controller and a DCS center.
Further, the lifting device and the large container are installed on the support base.
Furthermore, elevating gear includes electric push rod, and electric push rod fixes on electric push rod base, and electric push rod base is connected on the support, and the leg joint is on the support base, and the connecting rod is connected to the flexible end of electric push rod, and the other end of connecting rod is connected the pH meter probe.
A process control method of a system for measuring the pH value of a suspension reaction solution on line comprises the following steps:
s1, suspended particles and colloidal substances are selectively filtered in a reaction system, a liquid pump pumps reaction solution in a reaction kettle to a large container on a bracket base and a small container arranged in an inner cavity of the large container through a pipeline, junction potential of the system is reduced, and solution property requirements required by pH measurement are met;
s2, in the whole reaction process, automatically controlling the liquid pump to rotate forwards and backwards according to a PLC program so as to wash a filter head connected with the liquid pump through a liquid pumping pipe, keeping the filter head not to be blocked, keeping normal liquid pumping, and enabling pumped liquid to flow back into the reaction kettle from an outlet of the large container after flowing through the large container and the small container to form an external kettle circulating system;
s3, measuring the real-time flowing solution in the small container on line by using a pH meter probe so as to control the pH value of the whole reaction system and process;
s4, measuring the pH value, if the pH value is far away from the end point of the reaction, controlling the flow meter to add alkali or acid at a constant speed through the PLC, controlling the flow meter to slowly add alkali or acid before the pH value approaches the process pH value, gradually moving to the process, staying for a few minutes at the target pH value, observing the change of the pH value until the reaction system reaches the stable target pH value, and controlling the probe of the pH meter and the flow meter to stop by the PLC;
s5: after the probe and the flowmeter of the pH meter stop working, a liquid pump is started to reversely pump the reaction solution in the large container and the small container back to the reaction kettle;
s6: after the solution is pumped, starting an electric push rod on a bracket base to push upwards, pushing a pH electrode connected with the electric push rod through a connecting rod, starting a cleaning water pump to pump clean water to pass through a cleaning water pump pipe inlet in a large container, dividing the cleaning water pump pipe inlet into two water spray pipe ports through a pipeline to wash a pH meter probe, wherein the water spray pipe ports penetrate and extend into a small container, starting the water pump by a PLC (programmable logic controller) to pump the cleaning water for cleaning the electrode through the pipe ports, and controlling the electric push rod to return to the original position;
s7: and (4) starting a buffer solution water pump by a program to pump the buffer solution in the storage bottle, injecting the buffer solution into the small container through the buffer solution water pump pipe and the buffer solution pipe, and immersing the pH electrode glass ball and the part above into the small container to protect the pH electrode.
Compared with the prior art, the invention has the beneficial effects that:
(1) The design of the novel reaction liquid extraction filter head and the positive and negative rotation operations of the liquid extraction pump are alternately performed in the clearance of liquid extraction and back flushing, so that suspended particles cannot be adsorbed around the filter head, the extracted liquid is stable and uniform, the pH value of colloid and suspension generated in chemical production is measured on line, and the problem in industrial production is solved.
(2) The device for completely measuring the pH system on line is designed delicately, so that the measurement is standardized and systematized, the accuracy of the pH measurement is ensured, the service life of the test electrode is prolonged, and the cost is reduced.
(3) After the suction filtration liquid enters the large container, the filtrate enters the small container through the ingenious design of the branched pipe to construct a real-time circulating system of reaction liquid systems in the reaction kettle and the measuring container, so that the extraction of the reaction liquid, the measurement of the pH value, the adjustment of the pH value of the reaction liquid in the reaction kettle and the determination of the process are ensured in real time and on line.
(4) The whole process is controlled by a PLC program, and comprises the steps of online extracting and filtering reaction solution with suspended particles, online measuring pH and uploading numerical values, automatically flushing a pH electrode, automatically injecting buffer solution to protect the pH electrode, automatically controlling the flow of alkali (acid) added into a reaction kettle to adjust the pH value of the reaction solution, and automatically indicating the process. The intelligent control method is accurate and convenient, and can save labor and time cost.
(5) The whole system does not contain metal materials, can be applied to the online accurate measurement of the pH value and related data of a strong acid and strong base reaction system, and can be widely applied to colloid and suspension reaction systems and other related chemical reaction parameters and data test problems of chemical systems.
Drawings
FIG. 1 is a schematic view of the structure of the present invention;
FIG. 2 is a structural cross-sectional view of the present invention;
FIG. 3 is a top view of the construction of the macro-container of the present invention;
FIG. 4 is a schematic view of a filter head according to the present invention;
FIG. 5 is a cross-sectional view of the filter head construction of the present invention;
the notation in the figure is: 1. a filter head; 101. a filter screen; 102. a frame net bag; 103. a counterweight block; 2. cleaning the water pipe; 3. a water pumping pipe; 4. a solution inflow tube; 5. a branch line; 6. a small container; 7. a large container; 8. a pH electrode glass sphere; 9. water spraying pipe mouth; 10. a solution outflow pipe; 11. cleaning the water pump pipe; 12. a water pump pipe; 13. a buffer solution water pump pipe; 14. a pH electrode; 15. buffering the solution pipe; 16. an electric push rod; 17. a support; 18. an electric push rod base; 19. a bracket base; 20. a connecting rod.
Detailed Description
In order to better understand the purpose, structure and function of the present invention, the following describes a system for fully automatic online measurement of pH of a reaction solution suspended in a reaction kettle in detail with reference to the accompanying drawings.
As shown in fig. 1, the present invention discloses a system for full-automatic online measurement of pH of a suspension reaction solution in a reaction kettle, which comprises a reaction kettle (not shown in the figure) filled with a suspension reaction solution, wherein the reaction kettle is a reaction kettle in the prior art and is provided with relevant devices such as an alkali (acid) adding flowmeter, etc.; the measuring device is used for automatically extracting and refluxing the suspended reaction liquid in the reaction kettle on line and automatically measuring the pH value in the reaction process;
as shown in fig. 2, the measuring device includes a support base 19, a large container 7 is placed on the support base 19, a small container 6 is arranged in the large container 7, the small container 6 is arranged above an inner cavity of the large container 7, and can be fixed by being attached to an inner wall of one side of the large container 7 or supported by a fixing part, a certain distance is reserved between the bottom end of the small container 6 and the large container 7, so that the small container is in a suspended state, a solution inflow pipe 4 is arranged on one side wall of the large container 7 in a penetrating manner, an outer pipe opening of the solution inflow pipe 4 can be movably connected with a liquid pumping pipe, a liquid pumping pump is arranged on the liquid pumping pipe, and according to the requirement of an online accurate measurement suspension reaction liquid pH system, a filter head 1 for pumping reaction liquid is specially designed for the current situation that colloid and suspension liquid are easy to block by the liquid pumping pump, and the filter head 1 is connected to the other end of the liquid pumping pipe;
as shown in fig. 4 and 5, the filter head 1 is composed of three parts, the first part is a filter screen 101, filter materials with different pore diameters such as resin with better strong acid resistance and strong alkali resistance are selected according to the properties of a suspension solution and the sizes of particles, the pore diameter of the mesh is preferably 100 to 2000 meshes, mesh materials with different pore diameters are selected according to different solution conditions and after a whole system test, the mesh is prevented from being blocked in the using process, the filtering and backflushing effects cannot be achieved, and the filter screen 101 selectively allows particles with certain particle diameters to pass through. The second part is a plastic frame net bag 102 which is used for supporting the filter screen 101 and ensuring a certain three-dimensional space configuration so that the solution can enter the inside. The size of the grid of the frame is not limited, the grid can be within the range from 2 mm to 20 mm, and certain supporting strength support and acid and alkali resistance are required;
the third part is a counterweight material, mainly comprising acid-resistant and alkaline ceramic massive balls and cylindrical materials, and preferably a ceramic column 3, because the filter head 1 is not easy to enter liquid when the solution of suspended particles in the reaction kettle is stirred and rotated vigorously, the design of the counterweight filter head better solves the problem of extracting liquid from the suspended solution, and solves the problem that the colloid and suspension system are not suitable for directly measuring pH in industrial production; if the balance weight is not added, the filter head 1 is difficult to enter the solution to extract the solution under the high-speed stirring of the stirring paddle;
the filter head 1 is connected with a liquid pump and then enters the solution, the liquid pump is controlled by a PLC program to rotate positively and negatively in a pulse mode, the solution is pumped for a period of time and then rotates reversely, and the filter head 1 is washed by the pumped solution. Because the suspended particles are adsorbed around the filter head 1 when the solution is extracted, the further extraction of the solution is blocked, the filter head 1 is not washed to influence the change of the solution components, and the extracted solution is used for back washing the filter head 1, the problem is better solved, the suspended particles can not be attached around the filter head by combining the intermittent and pulse alternate operation of the extracted liquid and the back washing liquid, the extracted liquid is stable and uniform, the intermittent pulse time is controlled by a PLC program, and the time interval of several seconds and several minutes and the time length and frequency of each extraction and back washing can be determined by the program setting;
after a filter head 1 is placed in a reaction kettle, a solution is pumped in the reaction kettle through a liquid pump, and is filtered by the filter head 1 and then sent into a solution inflow pipe 4, the part of the solution inflow pipe 4 extending into a large container 7 is divided into two circulation pipelines, wherein the outflow port of the solution inflow pipe 4 is used as a pipeline to flow the solution into the large container 7, a branch pipeline 5 is branched from the solution inflow pipe 4 and is used for guiding the solution into a small container 6, the pumped solution can timely enter the small container 6, the solution in the large container 7 has the same property and the same pH value, the solution in the small container 6 keeps flowing, the small container 6 where a pH meter probe is positioned is ensured to measure the flowing of the pH solution and reflect the instant state of the solution, and when the small container 6 is full, the solution overflows to the large container 7;
as shown in fig. 1 and fig. 2, a solution outflow pipe 10 is further disposed through a side wall of the large container 7, the solution outflow pipe 10 is located at a certain height on the side wall of the large container 7, and an external connection pipe is connected to the solution outflow pipe and led into the reaction kettle, so that the solution flows back to the reaction kettle through the solution outflow pipe 10 after the large container 7 is filled with the solution, thereby forming a circulation system;
as shown in fig. 2 and 3, the large container 7 is provided with the cleaning water pipe 2, the cleaning water pipe 2 is divided into a plurality of water spraying pipe openings 9 for spraying clean water, the water spraying pipe openings 9 extend through and are positioned in the small container 6, preferably two water spraying pipe openings 9 are provided in the small container 6 in a bilateral symmetry manner, and the function of multi-way washing is achieved; the cleaning water pipe 2 is externally connected with a spray washing water pump pipe 11, the other end of the spray washing water pump pipe 11 is connected with a spray washing water pump, and the spray washing water pump is placed in a water source to pump clean water;
as shown in fig. 2 and 3, a water pumping pipe 3 and a buffer solution pipe 15 are further arranged in the small container 6, one end of the water pumping pipe 3 extends to be located in the cavity of the small container 6, the other end extends out of the top opening of the small container 6, the water pumping pipe 3 is connected with a water pumping pump pipe 12, the other end of the water pumping pump pipe 12 is connected with a water pumping pump, and the water pumping pump is used for pumping out cleaning water for cleaning the electrodes in the small container 6; the buffer solution pipe 15 is connected with a buffer solution water pump pipe 13, the other end of the buffer solution water pump pipe 13 is connected with a buffer solution water pump, the buffer solution water pump pipe 13 is used for pumping buffer solution, the buffer solution enters the small container 6 through the buffer solution water pump pipe 13, the part above the pH electrode glass ball 8 is immersed in the buffer solution, the pH electrode 14 is protected, the service life is prolonged, pumps with various functions in the application can be summarized into a water pump unit, and the water pump unit is controlled through a PLC (programmable logic controller) of a control system;
as shown in fig. 2, a lifting device is further placed on the support base 19, the lifting device comprises an electric push rod 16, the electric push rod 16 is fixed on an electric push rod base 18, the electric push rod base 18 is connected on a support 17, the support 17 is connected on the support base 19, the telescopic end of the electric push rod 16 is connected with a connecting rod 20, the other end of the connecting rod 20 is connected with a pH meter probe, the pH meter probe adopts a standard component in the prior art, the pH meter probe specifically comprises a pH electrode 14 and a transmitter, the transmitter is used for transmitting a pH measured value to a control system, a pH electrode glass ball 8 is arranged at the bottom end of the pH electrode 14, the pH meter probe is connected with a PLC controller and a DCS center through a lead, and when the pH meter probe is stretched into the small container 6, the pH meter probe can measure the flow of a pH solution in the small container 6 and reflect the instant state of the solution;
the lifting device can also be a component which can achieve the lifting function in other forms, the installation mode is not unique, and the lifting device can also be a mode of being installed and suspended at the top end of the container, so long as the lifting device can drive the pH meter probe to carry out lifting work, the protection range of the application is provided;
the whole processes of online extracting reaction solution, measuring pH, flushing a pH meter probe, protecting the pH meter probe and the like are automatically completed by a designed PLC program, and system control means can be realized based on the prior art.
The specific process is as follows: the solution filtered by the filter head 1 in the reaction kettle is pumped by a water pump and enters the large container 7 through the solution inflow pipe 4, and is divided into two branches, wherein one branch is used as a pipeline to flow the solution into the large container 7 through the outflow port of the solution inflow pipe 4, and the other branch is used for shunting the pumped solution into the small container 6 through the branch pipeline 5, so that the solution in the large container 7 has the same property and the same pH value. The solution in the large container 7 is filled and then flows back to the reaction kettle through the solution outflow pipe 10. So that the solution in the reaction kettle and the solution outside the reaction kettle continuously flow in and out to form a circulating system. The solution enters a small container 6, and then a pH meter probe can test and display the pH value at the moment and upload the pH value to a DCS center in time. The length of the test time needs to be set according to the length of the reaction process time, and the PLC program controls the measurement time and the data uploading of the pH value. Meanwhile, the pH meter probe feeds back the value to the PLC, and the PLC is used for controlling the actions related to the alkali (acid) adding flowmeter and the like in time. When the reaction reaches the end point, the PLC controls the pH meter probe and the flow meter on the reaction kettle to stop working, and the liquid pump is started to reversely pump the reaction solution in the large container 7 and the small container 6 back to the reaction kettle. After the solution is pumped out, the electric push rod 16 is started to push upwards, the pH electrode 14 is pushed upwards by a few centimeters, the cleaning water pump is started to pump clean water to pass through the inlet of the cleaning water pump pipe 11, the cleaning water pump is divided into two water spraying pipe ports 9 through a pipeline to wash the probe of the pH electrode 14 for 5-100 seconds, after the cleaning water is completely washed, the PLC starts the water pumping water pump to pump the cleaning water for cleaning the electrode in the small container 6 through the water pumping water pump pipe 12, and then the electric push rod 16 is controlled to return to the original position. Starting a buffer solution water pump by a program to pump the buffer solution, entering the small container through a buffer solution water pump pipe, and immersing the part above the pH electrode glass ball 8 in the small container to protect the pH electrode 14, wherein the whole process is finished.
Specifically, the process control method of the system for full-automatic online measurement of the pH of the suspension reaction liquid in the reaction kettle comprises the following steps:
s1, suspended particles and colloidal substances are selectively filtered in a reaction system, a liquid pump pumps reaction solution in a reaction kettle to a large container 7 on a bracket base 19 and a small container 6 arranged in an inner cavity of the large container 7 through a pipeline, junction potential of the system is reduced, and solution property requirements required by pH measurement are met;
s2, in the whole reaction process, automatically controlling the liquid pump to rotate forwards and backwards according to a PLC program so as to wash the filter head 1 connected with the liquid pump through the liquid pumping pipe, keeping the filter head 1 not blocked, keeping normal liquid pumping, and enabling the pumped liquid to flow through the large container 7 and the small container 6 and then flow back into the reaction kettle from the outlet of the large container 7 to form an external kettle circulation system;
s3, measuring the solution flowing in the small container 6 in real time on line by using a pH meter probe so as to control the pH value of the whole reaction system and process;
s4, measuring the pH value, if the pH value is far away from the end point of the reaction, controlling the flow meter to add alkali or acid at a constant speed through the PLC, controlling the flow meter to slowly add alkali or acid before the pH value approaches the process pH value, gradually moving to the process, staying for a few minutes at the target pH value, observing the change of the pH value until the reaction system reaches the stable target pH value, and controlling the probe of the pH meter and the flow meter to stop by the PLC;
s5: after the probe and the flowmeter of the pH meter stop working, a liquid pump is started to reversely pump the reaction solution in the large container 7 and the small container 6 back to the reaction kettle;
s6: after the solution is pumped out, starting an electric push rod 16 on a bracket base 19 to push upwards, pushing a pH electrode 14 connected with the electric push rod 16 through a connecting rod 20 upwards, starting a cleaning water pump to pump clean water to pass through an inlet of a cleaning water pump pipe 11 positioned in a large container 7, dividing the clean water into two water spraying pipe ports 9 through a pipeline to wash the pH meter probe, wherein the water spraying pipe ports 9 penetrate and extend to be positioned in a small container 6, and controlling the electric push rod 16 to return to the original position after a PLC (programmable logic controller) starts the water pump to pump the cleaning water for cleaning the electrode through the pipe ports;
s7: the program starts a buffer solution pump to pump the buffer solution in the storage bottle to be injected into the small container 6 through the buffer solution pump pipe 13 and the buffer solution pipe 15, and the pH electrode glass ball 8 and the part above are immersed in the small container to protect the pH electrode 14.
The following examples of pH measurement and system control in a reaction system for synthesizing a polymer material by a reaction applied to a chemical industry are listed:
the particle size of the polymer material synthesized by enterprise reaction is about 30-90 micrometers through analysis and detection in advance, so that a filter screen made of a nylon polymer material is selected, the aperture of a mesh is about 1000-1500 meshes, and the filter screen 101 is formed; the frame net bag 102 of the filter head is made of engineering plastics, the aperture is 2-6 mm, and the filter head has better support strength and acid and alkali resistance; the string bag 2 selects a ceramic column with the weight of 200 g as a balancing weight 103, and the three parts form a filter head 1 which is very suitable for the reaction system;
the filter head 1 is connected with a liquid pump and then is put into the reaction solution which is stirred at high speed in the reaction kettle, the filter head 1 sinks under the suspended particles due to the balance weight, and the reaction solution can be pumped and filtered between the suspended layer and the solution;
when the reaction is carried out for a period of time and the pH value of a reaction system needs to be monitored and controlled, the DCS central system sends an input signal to the PLC, the PLC starts a liquid pump to pump reaction liquid, and starts an online pH meter probe to work;
the solution pumped and filtered by the liquid pump enters a large container 7 through a solution inflow pipe 4 and is divided into two branches, one branch branches the pumped solution into a small container 6 through a branch pipeline 5 to ensure that the pumped solution can enter the small container 6 in time and keep the same property and the same pH value as the solution in the large container 7, and the solution in the large container 7 flows back to the reaction kettle through a solution outflow pipe 10 after being filled with the solution, so that the solution in the reaction kettle and the solution outside the reaction kettle continuously flow in and out to form a circulating system;
the solution enters the small container 6, at which point the pH probe can test and display the pH value at that moment. After starting and measuring for 5 minutes, the pH value of the reaction system is 1.0, at the moment, the liquid pump is controlled by a PLC program to reversely rotate for 5 seconds, the filter head 1 is washed by the extracted solution to disperse suspended particles which surround the filter head 1 and are adsorbed when the solution is extracted, the liquid pump reversely rotates for 5 seconds every 2 minutes within the following reaction measurement time of more than 50 minutes, and the actions of extraction and reverse flushing are repeatedly repeated to ensure that the solution extraction and pH measurement work is smoothly and normally carried out;
when the pH value of the reaction system reaches 3.20, a low alarm line set by a pH meter probe sends out a buzzer, the buzzer feeds back to a DCS control center through a transmitter to start an addition and subtraction flowmeter of the reaction kettle to add alkali for neutralization reaction, when the pH value reaches 3.50, the pH meter probe transmitter feeds back to the DCS center to reduce the flow of the alkali adding flowmeter, slowly add alkali and control the reaction speed. And when the pH value reaches 4.10, the PLC closes the switch of the alkali adding flow meter, stops adding alkali and terminates the reaction. Finally, the pH value of the reaction solution is measured to be 4.12, the target set reaction end point pH value is reached, and the whole reaction and test time is 56 minutes;
when the reaction reaches the end point, the PLC controls the pH meter probe and the flowmeter to stop working, and then the liquid pump is started immediately to reversely rotate for 1 minute to pump the reaction solution in the large container 7 and the small container 6 back to the reaction kettle. After the solution is pumped out, the electric push rod 16 is started to push upwards, the pH electrode 14 is pushed upwards by 3 cm, the cleaning water pump is started to pump clean water to pass through the inlet of the spray water pump pipe, the clean water is divided into two spray water pipe ports 9 through the pipe to wash the probe of the pH meter for 35 seconds, the PLC starts the water pump to pump the cleaning water for cleaning the electrode through the pipe ports, and then the electric push rod 16 is controlled to return to the original position. The program starts the buffer solution pump to pump 50 ml of the buffer solution with pH =4.01 from the storage bottle, and the buffer solution is injected into the small container 6 through the buffer solution pump pipe 13 and the buffer solution pipe 15, and the pH electrode glass ball 8 and the upper part are immersed in the buffer solution pump pipe to protect the pH electrode 14, and then the whole process is completed.
It will be evident to those skilled in the art that the invention is not limited to the details of the foregoing illustrative embodiments, and that the present invention may be embodied in other specific forms without departing from the spirit or essential attributes thereof. The present embodiments are therefore to be considered in all respects as illustrative and not restrictive, the scope of the invention being indicated by the appended claims rather than by the foregoing description, and all changes which come within the meaning and range of equivalency of the claims are therefore intended to be embraced therein. Any reference sign in a claim should not be construed as limiting the claim concerned.
Furthermore, it should be understood that although the present description refers to embodiments, not every embodiment may contain only a single embodiment, and such description is for clarity only, and those skilled in the art should integrate the description, and the embodiments may be combined as appropriate to form other embodiments understood by those skilled in the art.
Claims (9)
1. The utility model provides a system for suspension reaction liquid pH in full-automatic on-line measuring reation kettle, includes reation kettle, its characterized in that, be equipped with in the reation kettle and carry out filterable filter head (1) to suspension reaction liquid, filter head (1) are including frame string bag (102), the inner chamber of frame string bag (102) is equipped with and makes things convenient for filter head (1) to sink balancing weight (103) in the reation kettle solution, the peripheral cladding of frame string bag (102) has filter screen (101), filter head (1) is connected on the liquid suction pipe, but install the drawing liquid pump of positive and negative extraction on the liquid suction pipe, solution inflow pipe (4) is connected to the liquid suction pipe other end, solution inflow pipe (4) run through and set up on the lateral wall of big container (7), be equipped with little container (6) in big container (7), be equipped with the pH meter probe in the little container (6), the pH meter probe can reciprocate through the elevating gear who is connected with it, be connected with lateral conduit (5) on solution inflow pipe (4), solution flows into in little container (6) simultaneously through lateral conduit (5), the pH meter probe can reach the flow state and the flow control reation kettle, the flow control system, be equipped with the flow rate of reaction solution, 10, the reaction solution is in the reation kettle, the flow control system.
2. The system for full-automatic online measurement of the pH of the reaction solution suspended in the reaction kettle according to claim 1, wherein a cleaning water pipe (2) is disposed in the large container (7), the cleaning water pipe (2) is divided into a plurality of water spraying pipe ports (9), the water spraying pipe ports (9) extend through and are located in the small container (6), the top end of the cleaning water pipe (2) is connected with a cleaning water pump pipe (11), the cleaning water pump pipe (11) is connected with a cleaning water pump, and the cleaning water pump is connected with a control system.
3. The system for the full-automatic online measurement of the pH of the reaction solution in suspension in the reaction kettle according to claim 2, wherein a water pumping pipe (3) for pumping the water used for cleaning the small container (6) is arranged in the small container (6), the other end of the water pumping pipe (3) is connected with a water pumping pump pipe (12), the other end of the water pumping pump pipe (12) is connected with a water pumping pump, and the water pumping pump is connected with a control system.
4. The system for the full-automatic online measurement of the pH of the reaction liquid suspended in the reaction kettle according to claim 1, wherein the pH meter probe comprises a pH electrode (14) and a transmitter, the transmitter is used for transmitting the pH measurement value to the control system, and a pH electrode glass ball (8) is arranged at the bottom end of the pH electrode (14).
5. The system for the full-automatic online measurement of the pH of the reaction solution suspended in the reaction kettle according to claim 4, wherein a buffer solution pipe (15) is arranged in the small container (6), the other end of the buffer solution pipe (15) is connected with a buffer solution water pump pipe (13), the other end of the buffer solution water pump pipe (13) is connected with a buffer solution water pump, the buffer solution water pump is connected with a control system to pump the buffer solution, the buffer solution enters the small container (6) through the buffer solution water pump pipe (13) and the buffer solution pipe (15), and the part above the pH electrode glass ball (8) is immersed in the buffer solution water pump pipe to protect the pH electrode (14).
6. The system for the full-automatic on-line measurement of the pH of the reaction solution suspended in the reaction kettle according to any one of claims 1 to 5, wherein the control system is a PLC (programmable logic controller) and a DCS center.
7. The system for the full-automatic on-line measurement of the pH of the reaction liquid suspended in the reaction kettle according to claim 5, wherein the lifting device and the large container (7) are installed on a support base (19).
8. The system for full-automatic online measurement of the pH of the reaction solution in suspension in the reaction kettle according to claim 7, wherein the lifting device comprises an electric push rod (16), the electric push rod (16) is fixed on an electric push rod base (18), the electric push rod base (18) is connected on a support (17), the support (17) is connected on a support base (19), the telescopic end of the electric push rod (16) is connected with a connecting rod (20), and the other end of the connecting rod (20) is connected with a pH meter probe.
9. A process control method of a system for on-line measuring pH of a suspended reaction solution using the system of claim 8, comprising the steps of:
s1, suspended particles and colloidal substances are selectively filtered in a reaction system, a liquid pump pumps reaction solution in a reaction kettle to a large container (7) on a bracket base (19) and a small container (6) arranged in an inner cavity of the large container (7) through a pipeline, junction potential of the system is reduced, and solution property requirements required by pH measurement are met;
s2, in the whole reaction process, automatically controlling the liquid pump to rotate forwards and backwards according to a PLC program so as to wash the filter head (1) connected with the liquid pump through the liquid pumping pipe, keeping the filter head (1) from being blocked, keeping normal liquid pumping, and enabling the pumped liquid to flow through the large container (7) and the small container (6) and then flow back into the reaction kettle from an outlet of the large container (7) to form an outside-kettle circulating system;
s3, measuring the real-time flowing solution in the small container (6) on line by using a pH meter probe so as to control the pH value of the whole reaction system and process;
s4, measuring the pH value, if the pH value is far away from the end point of the reaction, controlling the flow meter to add alkali or acid at a constant speed through the PLC, controlling the flow meter to slowly add alkali or acid before the pH value approaches the process pH value, gradually moving to the process, staying for a few minutes at the target pH value, observing the change of the pH value until the reaction system reaches the stable target pH value, and controlling the probe of the pH meter and the flow meter to stop by the PLC;
s5: after the probe and the flowmeter of the pH meter stop working, a liquid pump is started to reversely pump the reaction solution in the large container (7) and the small container (6) back to the reaction kettle;
s6: after the solution is pumped out, an electric push rod (16) on a bracket base (19) is started to be pushed upwards, a pH electrode (14) connected with the electric push rod (16) through a connecting rod (20) is pushed upwards, a cleaning water pump is started to pump clean water to pass through an inlet of a cleaning water pump pipe (11) in a large container (7), the inlet is divided into two water spraying pipe ports (9) through a pipeline to wash a pH meter probe, wherein the water spraying pipe ports (9) penetrate and extend into a small container (6), and a PLC (programmable logic controller) starts the water pumping pump to pump the cleaning water of the cleaning electrode through the pipeline ports and controls the electric push rod (16) to return to the original position;
s7: the program starts a buffer solution water pump to pump the buffer solution in the storage bottle, the buffer solution is injected into the small container (6) through a buffer solution water pump pipe (13) and a buffer solution pipe (15), and the pH electrode glass ball (8) and the part above are immersed in the buffer solution, so that the pH electrode (14) is protected.
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Address after: 230000 Weide Industrial Park at the intersection of Wenshan Road and Changgu Road in Feixi County Economic Development Zone, Hefei City, Anhui Province Patentee after: Anhui Zhongke Weide Digital Technology Co.,Ltd. Address before: 230000 No. 316, Jinxiu Avenue, Taohua Industrial Park, Feixi County, Hefei City, Anhui Province Patentee before: ANHUI WDT INDUSTRIAL AUTOMATION CO.,LTD. |