CN109395671B - Bypass monitoring device for gas-liquid-solid three-phase reaction and application of bypass monitoring device in carbon dioxide mineral sealing - Google Patents
Bypass monitoring device for gas-liquid-solid three-phase reaction and application of bypass monitoring device in carbon dioxide mineral sealing Download PDFInfo
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- G01N9/002—Investigating density or specific gravity of materials; Analysing materials by determining density or specific gravity using variation of the resonant frequency of an element vibrating in contact with the material submitted to analysis
- G01N2009/006—Investigating density or specific gravity of materials; Analysing materials by determining density or specific gravity using variation of the resonant frequency of an element vibrating in contact with the material submitted to analysis vibrating tube, tuning fork
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Abstract
The invention relates to a bypass monitoring device for gas-liquid-solid three-phase reaction, which comprises a horizontally arranged cylindrical monitoring cavity, an eccentric reducing pipe, a tuning fork densimeter and a pH meter, wherein a densimeter placing pipe is arranged above the monitoring cavity in the vertical direction, the tuning fork densimeter is inserted into the placing pipe, the measuring end of the densimeter extends into the monitoring cavity, a gas phase branch pipe is arranged on the side wall above the densimeter placing pipe, the other end of the gas phase branch pipe is communicated with a three-phase reactor, a discharging pipe is arranged below the monitoring cavity in the vertical direction, and the bottom of the discharging pipe is communicated with the three-phase reactor; the side wall of the monitoring cavity is communicated with the large head section of the eccentric reducing pipe, and the small head section of the eccentric reducing pipe is communicated with the three-phase reactor; a pH meter placing pipe is arranged above the monitoring cavity, and a pH meter is inserted in the monitoring cavity. The device can accurately monitor the solid-liquid ratio value and the pH value of a reaction system, can sample through a sampling port for component analysis, can also realize descaling and cleaning of a tuning fork densimeter and the pH meter, and improves the safety and accuracy of the process.
Description
Technical Field
The invention relates to a bypass monitoring device for gas-liquid-solid three-phase reaction and application thereof in carbon dioxide mineral sealing, and belongs to the technical field of chemical industry.
Background
In the chemical industry, there are many reactions involving gas-liquid-solid three-phase reaction processes, and in these reaction systems, it is generally necessary to accurately analyze the solid-liquid ratio and the composition of the aqueous solution to determine the progress of the reaction. For example, in order to follow the world trend supporting national low-carbon emission reduction strategy, zhao Liang and the like, a method for sealing carbon dioxide in industrial flue gas (such as flue gas of a cement plant, flue gas of a thermal power plant and the like) by using magnesium chloride and preparing light magnesium carbonate and co-producing ammonium chloride is developed. According to the method, the pH value of the solution is regulated by liquid ammonia to absorb carbon dioxide in industrial flue gas, magnesium ammonium carbonate hydrate crystals generated by the reaction are used as intermediate products, and the light magnesium carbonate is prepared by refining magnesium ammonium carbonate hydrate. In the implementation process of the process, the gas-liquid-solid three-phase reaction process needs to be realized in the production of magnesium ammonium carbonate hydrate intermediate products and the refining process of light magnesium carbonate, and the reaction process can be judged by accurately analyzing the solid-liquid ratio value and the aqueous solution component in the process so as to improve the separation efficiency.
So far, the common solid-to-liquid ratio monitoring means is a tuning fork densitometer, and the common pH monitoring means is a pH meter. In order to avoid the influence of bubbles on density measurement, a foam remover with meshes is usually designed to protect a tuning fork of the densitometer, however, in a reaction system with solid formation, the meshes of the foam remover are blocked by solid substances, so that monitoring errors are caused. In addition, densitometers and pH surfaces can scale, creating measurement errors. There is no cleaning scheme for tuning fork densimeter, but the common cleaning scheme for pH meter is a telescopic sheath, and the pH is retracted into the sheath for cleaning during cleaning, and the mechanism has complex structure and poor reliability.
Disclosure of Invention
The invention aims to solve the defects of the prior art and provides a bypass monitoring device for gas-liquid-solid three-phase reaction, which can accurately monitor the solid-liquid ratio value, the pH value and the chemical components of a reaction system.
Technical proposal
The bypass monitoring device for the gas-liquid-solid three-phase reaction comprises a horizontally arranged cylindrical monitoring cavity, an eccentric reducing pipe, a tuning fork densimeter and a pH meter, wherein a densimeter placing pipe is arranged above the monitoring cavity in the vertical direction, the bottom of the densimeter placing pipe is communicated with the monitoring cavity, a tuning fork densimeter is inserted into an inlet at the top of the densimeter placing pipe, and a measuring end of the tuning fork densimeter stretches into the monitoring cavity; a gas phase branch pipe is arranged on the side wall above the densimeter placing pipe, one end of the gas phase branch pipe is communicated with the densimeter placing pipe, and the other end of the gas phase branch pipe is communicated with the gas-liquid-solid three-phase reactor through a ball valve and a pipeline; a discharging pipe is arranged in the vertical direction below the monitoring cavity, the top of the discharging pipe is communicated with the monitoring cavity, and the bottom of the discharging pipe is communicated with the gas-liquid-solid three-phase reactor; the side wall of one side of the monitoring cavity is communicated with the large head section of the eccentric reducing pipe, and the small head section of the eccentric reducing pipe is communicated with the gas-liquid-solid three-phase reactor through a pipeline and a peristaltic pump; a pH meter placing pipe is arranged above the monitoring cavity and communicated with the monitoring cavity, and a pH meter is inserted into the pH meter placing pipe; and a sampling port is arranged below the monitoring cavity in an inclined manner.
Further, the axis of the eccentric reducing pipe is perpendicular to the axis of the densitometer placement pipe.
Further, the ratio of the inner diameter of the small head section to the inner diameter of the large head section of the eccentric reducing pipe is 1: (2-2.5).
Further, the length of the big head section of the eccentric reducing pipe is not less than 30cm.
Further, the height of the densitometer-placed tube is not less than 50cm.
Further, the gap between the tuning fork densimeter and the wall of the densimeter placing pipe is 10-20mm.
Further, the measuring end of the tuning fork densimeter is positioned in the monitoring cavity opposite to the large head section of the eccentric reducing pipe.
The device is applied to carbon dioxide mineral sequestration. In the process of sealing and storing the magnesium method carbon dioxide minerals, the production of magnesium ammonium carbonate hydrate intermediate products and the gas-liquid-solid coexistence in the process of refining light magnesium carbonate, the reaction mixture is introduced into the device, so that the real-time and stable separation of a gas phase and a solid-liquid phase can be realized, the interference of low-density bubbles on the density measurement of the liquid-solid mixture can be eliminated after the separation, and the accurate monitoring of the solid-liquid ratio value can be realized.
The application method comprises the following steps:
(1) Pumping the gas-liquid-solid three-phase mixture into an eccentric reducing pipe from a gas-liquid-solid three-phase reactor through a peristaltic pump, and enabling a gas phase to move upwards and a liquid phase and a solid phase to move downwards along the pipe wall when the gas-liquid-solid three-phase mixture flows in a big head section in the eccentric reducing pipe, so that separation of the gas phase from the liquid phase and the solid phase is realized;
(2) After entering the monitoring cavity, the separated gas phase enters a densimeter placing pipe in the vertical direction above the monitoring cavity, and then flows out of a gas phase branch pipe to return to the gas-liquid-solid three-phase reactor; collecting the liquid phase and solid phase mixture separated from the eccentric reducing pipe in a monitoring cavity, and enabling the measuring end of the tuning fork densimeter to penetrate through the densimeter placing pipe and extend into the liquid phase and solid phase mixture in the monitoring cavity to perform density measurement; the pH meter extends into the mixture of the liquid phase and the solid phase in the monitoring cavity through a pH meter placing pipe on the monitoring cavity to measure the pH; the mixture of the liquid phase and the solid phase is discharged through a sampling port obliquely below the monitoring cavity, and component detection is carried out;
(3) After the measurement is finished, the mixture of the liquid phase and the solid phase returns to the gas-liquid-solid three-phase reactor through a discharging pipe below the monitoring cavity;
(4) After the reaction in the gas-liquid-solid three-phase reactor is finished, discharging a reaction mixture, pumping 1-5% of dilute hydrochloric acid into the gas-liquid-solid three-phase reactor, pumping the dilute hydrochloric acid into a monitoring cavity through a peristaltic pump, and cleaning a measuring end of a tuning fork densimeter and a measuring end of a pH meter.
The invention has the beneficial effects that:
(1) The invention provides a bypass monitoring device for gas-liquid-solid three-phase reaction, which can accurately monitor the solid-liquid ratio value and the pH value of a reaction system and can sample through a sampling port for component analysis;
(2) The device can realize scale removal and cleaning of the tuning fork densimeter and the pH meter, avoid long-time monitoring, and improve the safety and accuracy of the process due to measurement errors caused by scale covering the surface of the sensor;
(3) The device can realize real-time sampling of the closed reaction tank and rapid analysis and judgment of the reaction process;
(4) The device can be applied to the production of magnesium ammonium carbonate hydrate intermediate products in a magnesium method carbon dioxide mineral recycling process, and the real-time and stable separation of gas phase and liquid-solid phase in a gas-liquid-solid three-phase mixture in the light magnesium carbonate refining process, and can eliminate the interference of low-density bubbles on the density measurement of the liquid-solid mixture after separation, so that the accurate monitoring of the solid-liquid ratio value is realized, and the judgment of the solid-liquid separation time is accurately carried out.
Drawings
FIG. 1 is a schematic diagram of a bypass monitoring device for gas-liquid-solid three-phase reaction according to the present invention;
wherein, 1-monitoring the cavity; 2-densitometer placement tube; 3-gas phase branch pipes; 4-a discharging pipe; 5-eccentric reducing pipe; 6-placing a tube by a pH meter; 7-pH meter; 8-sampling port; 9-peristaltic pump; 10-tuning fork densitometer; 11-ball valve; 12-a gas-liquid-solid three-phase reactor.
Detailed Description
The invention will be further described with reference to the drawings and the specific embodiments.
Example 1
Referring to fig. 1, a bypass monitoring device for gas-liquid-solid three-phase reaction comprises a horizontally arranged cylindrical monitoring cavity 1, an eccentric reducing pipe 5, a tuning fork densimeter 10 and a pH meter 7, wherein a densimeter placing pipe 2 is arranged above the monitoring cavity 1 in the vertical direction, the bottom of the densimeter placing pipe 2 is communicated with the monitoring cavity 1, the tuning fork densimeter 10 is inserted into the inlet at the top of the densimeter placing pipe 2, and the measuring end of the tuning fork densimeter 10 extends into the monitoring cavity 1; a gas phase branch pipe 3 is arranged on the side wall above the densimeter placing pipe 2, one end of the gas phase branch pipe 3 is communicated with the densimeter placing pipe 2, and the other end is communicated with a gas-liquid-solid three-phase reactor 12 through a ball valve 11 and a pipeline; a discharging pipe 4 is arranged in the vertical direction below the monitoring cavity 1, the top of the discharging pipe 4 is communicated with the monitoring cavity 1, and the bottom of the discharging pipe is communicated with a gas-liquid-solid three-phase reactor 12 through a ball valve 11 and a pipeline; the side wall of one side of the monitoring cavity 1 is communicated with the large head section of the eccentric reducing pipe 5, and the small head section of the eccentric reducing pipe 5 is communicated with the gas-liquid-solid three-phase reactor 12 through a pipeline and a peristaltic pump 9; a pH meter placing pipe 6 is arranged above the monitoring cavity 1, the pH meter placing pipe 6 is communicated with the monitoring cavity 1, and a pH meter 7 is inserted into the pH meter placing pipe 6; the inclined lower part of the monitoring cavity 1 is provided with a sampling port 8.
The axis of the eccentric reducing pipe 5 is perpendicular to the axis of the densimeter placing pipe 2; the ratio of the inner diameter of the small head section to the inner diameter of the large head section of the eccentric reducing pipe 5 is 1:2.5; the length of the big head section of the eccentric reducing pipe is 30cm; the height of the densitometer placing tube is 50cm; the gap between the tuning fork densimeter and the wall of the densimeter placing pipe is 10mm, and the position of the measuring end of the tuning fork densimeter in the monitoring cavity is opposite to the big head section of the eccentric reducing pipe.
The device is applied to carbon dioxide mineral sealing and storing, and the application method comprises the following steps:
(1) Filling 5 cubes of reaction solution containing 1M ammonium chloride and 0.2M magnesium chloride into an 8-cube gas-liquid-solid three-phase reactor, blowing flue gas containing 15% carbon dioxide at the flow rate of 300 square per hour, simultaneously adding ammonia gas to keep the pH value of the reaction solution at 9, and introducing circulating cooling water to keep the reaction temperature at 60 ℃; starting a peristaltic pump, pumping the gas-liquid-solid three-phase mixture from the gas-liquid-solid three-phase reactor into an eccentric reducing pipe (the pumping flow is 5L/min) through the peristaltic pump, and enabling the gas phase to move upwards and the liquid phase and the solid phase to move downwards along the pipe wall when the gas-liquid-solid three-phase mixture flows in a big head section in the eccentric reducing pipe, so that the separation of the gas phase from the liquid phase and the solid phase is realized;
(2) After entering the monitoring cavity, the separated gas phase enters a densimeter placing pipe in the vertical direction above the monitoring cavity, and then flows out of a gas phase branch pipe to return to the gas-liquid-solid three-phase reactor; collecting the liquid phase and solid phase mixture separated from the eccentric reducing pipe in a monitoring cavity, and enabling the measuring end of the tuning fork densimeter to penetrate through the densimeter placing pipe and extend into the liquid phase and solid phase mixture in the monitoring cavity to perform density measurement; the pH meter extends into the mixture of the liquid phase and the solid phase in the monitoring cavity through a pH meter placing pipe on the monitoring cavity to measure the pH; the mixture of the liquid phase and the solid phase is discharged through a sampling port obliquely below the monitoring cavity, and component detection is carried out;
when bubbling was not performed, the densitometer monitored the reaction solution as a pure solution, the relative density was 1.015, and the pH was 4.457. After bubbling, the relative density was 1.013 and ph was 9.101 before the reaction appeared as a solid. After 0.5 hour of reaction, solids appeared, at which time the relative density reading gradually increased from 1.013 to 1.217, with 29.8% theoretical solids. At this time, 1L of solid-liquid mixture is taken through a sampling port on the device, and is dried after suction filtration, 328 g of solid is obtained, and the solid content is measured to be 27%;
(3) After the measurement is finished, the mixture of the liquid phase and the solid phase returns to the gas-liquid-solid three-phase reactor through a discharging pipe below the monitoring cavity;
(4) After the reaction in the gas-liquid-solid three-phase reactor is finished, discharging a reaction mixture, pumping 1% of dilute hydrochloric acid into the gas-liquid-solid three-phase reactor, pumping the dilute hydrochloric acid into a monitoring cavity through a peristaltic pump, cleaning the measuring end of the tuning fork densimeter and the measuring end of the pH meter, and dissolving the surface scaling of the tuning fork densimeter and the pH meter to realize stable measurement for 18 hours.
Example 2
In the bypass monitoring device for the gas-liquid-solid three-phase reaction, the ratio of the inner diameter of the small head section to the inner diameter of the large head section of the eccentric reducing pipe 5 is 1:2; the length of the big head section of the eccentric reducing pipe is 40cm; the height of the densimeter placing pipe is 60cm; the gap between the tuning fork densitometer and the wall of the densitometer-placing tube was 20mm, and the rest was the same as in example 1.
The device is applied to carbon dioxide mineral sealing and storing, and the application method comprises the following steps:
(1) Filling 5 cubes of reaction solution containing 1M ammonium chloride and 0.2M magnesium chloride into an 8-cube gas-liquid-solid three-phase reactor, blowing flue gas containing 15% carbon dioxide at the flow rate of 300 square per hour, simultaneously adding ammonia gas to keep the pH value of the reaction solution at 9.3, and introducing circulating cooling water to keep the reaction temperature at 60 ℃; starting a peristaltic pump, pumping the gas-liquid-solid three-phase mixture from the gas-liquid-solid three-phase reactor into an eccentric reducing pipe (the pumping flow is 35L/min) through the peristaltic pump, and enabling the gas phase to move upwards and the liquid phase and the solid phase to move downwards along the pipe wall when the gas-liquid-solid three-phase mixture flows in a big head section in the eccentric reducing pipe, so that the separation of the gas phase from the liquid phase and the solid phase is realized;
(2) After entering the monitoring cavity, the separated gas phase enters a densimeter placing pipe in the vertical direction above the monitoring cavity, and then flows out of a gas phase branch pipe to return to the gas-liquid-solid three-phase reactor; collecting the liquid phase and solid phase mixture separated from the eccentric reducing pipe in a monitoring cavity, and enabling the measuring end of the tuning fork densimeter to penetrate through the densimeter placing pipe and extend into the liquid phase and solid phase mixture in the monitoring cavity to perform density measurement; the pH meter extends into the mixture of the liquid phase and the solid phase in the monitoring cavity through a pH meter placing pipe on the monitoring cavity to measure the pH; the mixture of the liquid phase and the solid phase is discharged through a sampling port obliquely below the monitoring cavity, and component detection is carried out;
the densitometer and the pH meter were monitored in real time during the reaction. When bubbling was not performed, the densitometer monitored the reaction solution as a pure solution, the relative density was 1.016, and the pH was 4.521. After bubbling, the relative density was 1.014 and ph 9.311 before the reaction had solids. After 0.3 hours of reaction, solids appeared, at which time the relative density reading increased gradually from 1.016 to 1.290 with a theoretical solids content of 38.2%. At this time, 1L of solid-liquid mixture is taken through a sampling port on the device, and is dried after suction filtration, 502 g of solid is obtained, and the measured content is 39%;
(3) After the measurement is finished, the mixture of the liquid phase and the solid phase returns to the gas-liquid-solid three-phase reactor through a discharging pipe below the monitoring cavity;
(4) After the reaction in the gas-liquid-solid three-phase reactor is finished, discharging a reaction mixture, pumping 5% of dilute hydrochloric acid into the gas-liquid-solid three-phase reactor, pumping the dilute hydrochloric acid into a monitoring cavity through a peristaltic pump, cleaning the measuring end of the tuning fork densimeter and the measuring end of the pH meter, and dissolving the surface scaling of the tuning fork densimeter and the pH meter to realize stable measurement for 24 hours.
Example 3
In the bypass monitoring device for the gas-liquid-solid three-phase reaction, the ratio of the inner diameter of the small head section to the inner diameter of the large head section of the eccentric reducing pipe 5 is 1:2.2; the length of the big head section of the eccentric reducing pipe is 60cm; the height of the densimeter placing pipe is 80cm; the gap between the tuning fork densitometer and the wall of the densitometer-placing tube was 15mm, and the rest was the same as in example 1.
The device is applied to carbon dioxide mineral sealing and storing, and the application method comprises the following steps:
(1) Filling 5 cubes of tap water into an 8-cube magnesium ammonium carbonate hydrate reaction kettle, adding 1000 kg of magnesium ammonium carbonate hydrate crude product into the reaction kettle at a flow rate of 25 kg per minute, and simultaneously blowing carbon dioxide-lean tail gas containing 90% of nitrogen; starting a peristaltic pump, pumping the gas-liquid-solid three-phase mixture from the gas-liquid-solid three-phase reactor into an eccentric reducing pipe (the pumping flow is 20L/min) through the peristaltic pump, and enabling the gas phase to move upwards and the liquid phase and the solid phase to move downwards along the pipe wall when the gas-liquid-solid three-phase mixture flows in a big head section in the eccentric reducing pipe, so that the separation of the gas phase from the liquid phase and the solid phase is realized;
(2) After entering the monitoring cavity, the separated gas phase enters a densimeter placing pipe in the vertical direction above the monitoring cavity, and then flows out of a gas phase branch pipe to return to the gas-liquid-solid three-phase reactor; collecting the liquid phase and solid phase mixture separated from the eccentric reducing pipe in a monitoring cavity, and enabling the measuring end of the tuning fork densimeter to penetrate through the densimeter placing pipe and extend into the liquid phase and solid phase mixture in the monitoring cavity to perform density measurement; the pH meter extends into the mixture of the liquid phase and the solid phase in the monitoring cavity through a pH meter placing pipe on the monitoring cavity to measure the pH; the mixture of the liquid phase and the solid phase is discharged through a sampling port obliquely below the monitoring cavity, and component detection is carried out;
the degree of the densimeter and the degree of the pH meter are monitored in real time in the reaction process, and when bubbling is not carried out, the densimeter monitors that the reaction liquid is a pure solution, the relative density is 1.0, and the pH value is 6.8. After gradual addition of solids and bubbling, the relative density reading gradually increased from 1.0 to 1.119, with 16.7% theoretical solids. After 1 hour of reaction, the relative density gradually increased to 1.387. Taking 1L of solid-liquid mixture through a sampling port on the device, carrying out suction filtration and drying to obtain 221 g of solid, measuring 16% of measured content, and detecting the solid as pure light magnesium carbonate;
(3) After the measurement is finished, the mixture of the liquid phase and the solid phase returns to the gas-liquid-solid three-phase reactor through a discharging pipe below the monitoring cavity;
(4) After the reaction in the gas-liquid-solid three-phase reactor is finished, discharging a reaction mixture, pumping 3% of dilute hydrochloric acid into the gas-liquid-solid three-phase reactor, pumping the dilute hydrochloric acid into a monitoring cavity through a peristaltic pump, cleaning the measuring end of the tuning fork densimeter and the measuring end of the pH meter, and dissolving the surface scaling of the tuning fork densimeter and the pH meter to realize stable measurement for 24 hours.
Claims (6)
1. The bypass monitoring device for the gas-liquid-solid three-phase reaction is characterized by comprising a horizontally arranged cylindrical monitoring cavity, an eccentric reducing pipe, a tuning fork densimeter and a pH meter, wherein a densimeter placing pipe is arranged above the monitoring cavity in the vertical direction, the bottom of the densimeter placing pipe is communicated with the monitoring cavity, the tuning fork densimeter is inserted into the inlet at the top of the densimeter placing pipe, and the measuring end of the tuning fork densimeter extends into the monitoring cavity; a gas phase branch pipe is arranged on the side wall above the densimeter placing pipe, one end of the gas phase branch pipe is communicated with the densimeter placing pipe, and the other end of the gas phase branch pipe is communicated with the gas-liquid-solid three-phase reactor through a ball valve and a pipeline; a discharging pipe is arranged in the vertical direction below the monitoring cavity, the top of the discharging pipe is communicated with the monitoring cavity, and the bottom of the discharging pipe is communicated with the gas-liquid-solid three-phase reactor; the side wall of one side of the monitoring cavity is communicated with the large head section of the eccentric reducing pipe, and the small head section of the eccentric reducing pipe is communicated with the gas-liquid-solid three-phase reactor through a pipeline and a peristaltic pump; a pH meter placing pipe is arranged above the monitoring cavity and communicated with the monitoring cavity, and a pH meter is inserted into the pH meter placing pipe; a sampling port is arranged below the monitoring cavity in an inclined manner; the ratio of the inner diameter of the small head section to the inner diameter of the large head section of the eccentric reducing pipe is 1: (2-2.5); the axis of the eccentric reducing pipe is perpendicular to the axis of the densimeter placing pipe.
2. The bypass monitoring device for gas-liquid-solid three-phase reaction according to claim 1, wherein the length of the large end section of the eccentric reducing pipe is not less than 30cm.
3. The by-pass monitoring device for gas-liquid-solid three-phase reaction according to claim 1, wherein the height of the densitometer-placed tube is not less than 50cm.
4. The by-pass monitoring device for gas-liquid-solid three-phase reaction according to claim 1, wherein a gap between the tuning fork densitometer and a wall of the densitometer-placing tube is 10-20mm.
5. The by-pass monitoring device for gas-liquid-solid three-phase reactions according to any of claims 1 to 4, characterized in that the measuring end of the tuning fork densitometer is positioned opposite the large head section of the eccentric reducer pipe in the monitoring cavity.
6. Use of a bypass monitoring device according to any one of claims 1 to 5 in carbon dioxide mineral sequestration.
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