CN210875372U - Low-loss organic amine solution purification device - Google Patents
Low-loss organic amine solution purification device Download PDFInfo
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- CN210875372U CN210875372U CN201921569569.4U CN201921569569U CN210875372U CN 210875372 U CN210875372 U CN 210875372U CN 201921569569 U CN201921569569 U CN 201921569569U CN 210875372 U CN210875372 U CN 210875372U
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Abstract
The utility model discloses a low-loss organic amine solution purification device, which comprises an ion exchange bed, wherein an inert gas cylinder, a fifth liquid storage tank and a second liquid adding pump are arranged at an upper end feed inlet of the ion exchange bed through pipelines, a lower end feed inlet of the ion exchange bed is connected with a first liquid adding pump through a pipeline, and a material pumping port of the first liquid adding pump is connected with the first liquid storage tank through a pipeline; a discharge port at the lower end of the ion exchange bed is connected with a second liquid storage tank, a third liquid storage tank and a fourth liquid storage tank through pipelines, and a multiple total reflection infrared spectrum analyzer is installed on the discharge pipeline at the lower end of the ion exchange bed; and a discharge port at the upper end of the ion exchange bed is connected with a fourth liquid storage tank through a pipeline. The utility model discloses be convenient for the staff is through multiple total reflection infrared spectroscopy analysis appearance D1 real-time detection result control flap, and it is poor to the actual running conditions response to have avoided prior art to adopt the operation procedure of solidification, can not independently optimize the shortcoming of operational parameter.
Description
Technical Field
The utility model belongs to the technical field of solution purification device, in particular to low-loss organic amine solution purification device.
Background
The petrochemical and environmental protection industries often use chemical absorption methods based on organic amine absorbents to separate acidic gases such as hydrogen sulfide and carbon dioxide from raw material gases, for example, a Methyldiethanolamine (MDEA) solution is used to remove hydrogen sulfide gas in a deacidification process of natural gas or coal gasification synthesis gas, and Monoethanolamine (MEA) is used to remove carbon dioxide in a carbon dioxide capture process of power plant flue gas. Impurities in raw material gas participate in reaction or organic amine per se undergoes degradation reaction to cause the problems of deterioration, deterioration and the like of an organic amine solution, effective components in the solution are continuously reduced, the absorption capacity is continuously reduced, even if organic amine raw materials are supplemented on time, the stable operation of a device cannot be guaranteed, side reactions caused by the impurities and products degraded by the organic amine are mainly accumulated in the solution in the form of heat-stable salts, the components of the heat-stable salts mainly comprise formate, acetate, oxalate, sulfate, nitrate, sulfide and the like, and the problem of corrosion aggravation, solution foaming, device performance fluctuation and the like caused by the increase of the concentration of the heat-stable salts. It is therefore generally necessary to ensure that the heat-stable salt concentration is less than 1.0 wt.%. Methods for inhibiting the generation of heat-stable salts include inert gas protection, addition of additives into solutions and the like, but because of the factors of various impurities in raw material gas, low chemical stability of organic amines and the like, the methods have a very limited effect on inhibiting the degradation of organic amines. The method of directly replacing the amine liquid is expensive and the waste liquid may cause environmental problems due to the accumulation of heat-stable salts.
How to remove heat stability salt is one of the key technologies for ensuring the continuous operation of the desulfurization and decarburization systems, and the conventional purification methods of mechanical filtration and activated carbon adsorption cannot remove the heat stability salt existing in an ionic state. The methods currently used include: (1) the heat recovery method is characterized in that organic impurities are changed into high-boiling inorganic salt by adding alkali, and organic amine components with low boiling point are recovered by a distillation method, but the method has high energy consumption and low recovery rate, and the alkali with high concentration is introduced into a system; (2) electrodialysis, which separates impurity ions by utilizing the selective permeability of membrane technology to different ions, has the disadvantages of poor separation effect and easy pollution of the membrane; (3) the ion exchange method is a widely used method at present, and utilizes the characteristic that ion exchange resin has selective adsorption effect on different ions to separate impurity ions from organic amine solution, and realizes the regeneration of resin adsorption capacity by adding alkali, thereby achieving the purpose of resin recycling.
The ion exchange purifier has ion exchange bed as the center, ion exchange resin filled inside the ion exchange bed container, purifying unit running on the branch line of the technological system, and controlling the flow speed of the solution in the ion exchange bed to control the contact time between the solution and the resin. The device can cause part of the solution to stay in the exchange bed or the pipeline and cannot return to a solution system to be consumed due to the problems of adhesion and adsorption of resin to the solution, overlarge dead volume of the device and the pipeline, unreasonable liquid inlet ratio and residence time and the like.
The existing purification device control program is fixed and cannot respond according to the solution concentration and the operation condition of the purification device. In fact, the concentration of the solution is changed all the time, the adsorption performance of the ion exchange resin is changed along with the time, if the ion exchange resin is operated according to fixed parameters, the performance of a purification system cannot be kept in an optimal state, and the problem of excessive solution discharge can occur.
SUMMERY OF THE UTILITY MODEL
An object of the utility model is to provide a low-loss organic amine solution purifier to solve current purifier control procedure and be fixed, can't make the technical problem who responds according to solution concentration and purifier operational aspect.
In order to achieve the above object, the utility model provides a following technical scheme:
a low-loss organic amine solution purification device comprises an ion exchange bed, wherein an inert gas cylinder, a fifth liquid storage tank and a second liquid adding pump are mounted at a feed inlet at the upper end of the ion exchange bed through pipelines, a first flowmeter is mounted on an air outlet pipeline of the inert gas cylinder, a seventh valve is mounted on a discharge pipeline of the fifth liquid storage tank, a feed inlet at the lower end of the ion exchange bed is connected with a first liquid adding pump through a pipeline, and a material pumping port of the first liquid adding pump is connected with the first liquid storage tank through a pipeline;
a discharge port at the lower end of the ion exchange bed is connected with a second liquid storage tank, a third liquid storage tank and a fourth liquid storage tank through pipelines, and a multiple total reflection infrared spectrum analyzer is installed on the discharge pipeline at the lower end of the ion exchange bed;
the ion exchange bed is characterized in that an upper end discharge port of the ion exchange bed is connected with a fourth liquid storage tank through a pipeline, a third valve is installed on a feed pipeline of the second liquid storage tank, a fourth valve is installed on a feed pipeline of the third liquid storage tank, the fourth liquid storage tank is connected with a lower end discharge port pipeline of the ion exchange bed and is provided with a fifth valve, and the fourth liquid storage tank is connected with an upper end discharge port pipeline of the ion exchange bed and is provided with a second valve.
Furthermore, a second flowmeter is installed on a discharge pipeline of the second liquid adding pump, and a material pumping port of the second liquid adding pump is connected with a third liquid storage tank and a sixth liquid storage tank through pipelines.
Furthermore, a sixth valve is installed on a discharge pipeline of the third liquid storage tank, and an eighth valve is installed on a discharge pipeline of the sixth liquid storage tank.
Furthermore, a third flow meter and a first valve are arranged on a discharge pipeline of the first liquid adding pump.
Further, the liquid storage tank is a raw liquid tank, the liquid storage tank is a waste liquid tank, the liquid storage tank is a circulating alkali liquid tank, the liquid storage tank is a purified liquid tank, and the liquid storage tank is a deionized water tank.
Further, the sixth liquid storage tank is a clean alkali liquid tank.
Further, the top parts of the second liquid storage tank and the fourth liquid storage tank are provided with gas discharge ports.
Compared with the prior art, the beneficial effects of the utility model are that: this low-loss organic amine solution purifier passes through multiple total reflection infrared spectroscopy analysis appearance D1 real-time detection ion exchange bed X1 discharge solution in organic amine concentration, the staff of being convenient for passes through the opening or closing of multiple total reflection infrared spectroscopy analysis appearance D1 real-time detection result control flap, it is poor to the actual motion condition response to have avoided prior art to adopt the operation procedure of solidification, can not independently optimize the shortcoming of operational parameter, and, further, the utility model discloses can also combine amine solution measurement and purifier operation procedure function of independently adjusting together, can be with the amine loss informationization of purifier operation main step, reduce the loss through optimizing operational parameter, reduce the running cost.
Drawings
The accompanying drawings, which form a part of the present application, are included to provide a further understanding of the invention, and are incorporated in and constitute a part of this specification, illustrate embodiments of the invention and together with the description serve to explain the invention and not to limit the invention. In the drawings:
fig. 1 is a schematic view of the organic amine solution purification device of the present invention.
In the figure: x1 is an ion exchange bed, D1 is a multiple total reflection infrared spectrometer, C1 is an inert gas cylinder, F1 is a first flow meter, F2 is a second flow meter, F3 is a third flow meter, P1 is a first liquid adding pump, P2 is a second liquid adding pump, T1 is a first liquid storage tank, T2 is a second liquid storage tank, T3 is a third liquid storage tank, T4 is a fourth liquid storage tank, T5 is a fifth liquid storage tank, T6 is a sixth liquid storage tank, V1 is a first valve, V2 is a second valve, V3 is a third valve, V4 is a fourth valve, V5 is a fifth valve, V6 is a sixth valve, V7 is a seventh valve, and V8 is an eighth valve.
Detailed Description
The present invention will be described in detail below with reference to the accompanying drawings in conjunction with embodiments. It should be noted that the embodiments and features of the embodiments in the present application may be combined with each other without conflict.
The following detailed description is exemplary in nature and is intended to provide further details of the invention. Unless otherwise defined, all technical terms used herein have the same meaning as commonly understood by one of ordinary skill in the art to which this application belongs. The terminology used herein is for the purpose of describing particular embodiments only and is not intended to be limiting of example embodiments in accordance with the invention.
Referring to fig. 1, the present invention provides a technical solution: a low-loss organic amine solution purification device comprises an ion exchange bed X1, wherein the ion exchange bed X1 comprises a top cover, a bottom cover and a filter screen connected with the top cover and the bottom cover, ion exchange resin is filled in the ion exchange bed X1, the ion exchange resin contained in the ion exchange bed X1 is cation exchange resin, anion exchange resin or anion-cation mixed ion exchange resin, the filter screen of the top cover and the bottom cover can ensure that the resin cannot flow out of the ion exchange bed X1, an inert gas cylinder C1, a fifth liquid storage tank T5 and a second liquid adding pump P2 are arranged at a feed inlet at the upper end of the ion exchange bed X1 through pipelines, gas contained in an inert gas cylinder C1 is inert gas such as nitrogen, argon or helium, a first flow meter F1 is arranged on an outlet pipeline of the inert gas cylinder C1, a seventh valve V7 is arranged on a discharge pipeline of the fifth liquid storage tank T5, and a second flow meter F2 is arranged on a discharge pipeline of the second liquid adding pump P2, a material pumping port of the second liquid adding pump P2 is connected with a third liquid storage tank T3 and a sixth liquid storage tank T6 through pipelines, a discharge pipeline of the third liquid storage tank T3 is provided with a sixth valve V6, a discharge pipeline of the sixth liquid storage tank T6 is provided with an eighth valve V8, a lower end feed port of the ion exchange bed X1 is connected with a first liquid adding pump P1 through a pipeline, a material pumping port of the first liquid adding pump P1 is connected with a first liquid storage tank T1 through a pipeline, a discharge pipeline of the first liquid adding pump P1 is provided with a third flow meter F3 and a first valve V1, a lower end discharge port of the ion exchange bed X1 is connected with a second liquid storage tank T2, a third liquid storage tank T3 and a fourth liquid storage tank T4 through pipelines, an upper end discharge port of the ion exchange bed X1 is connected with a fourth liquid storage tank T4 through a pipeline, a lower end discharge pipeline of the ion exchange bed X1 is provided with a multiple total reflection spectrum analyzer D1, a detection window D1 of the ion exchange bed X1 is embedded into, the surface of the window is directly contacted with the waste liquid, the concentration of organic amine in the liquid flowing through the window can be measured, the measuring result can determine the duration and the repetition times of each step in the subsequent purification process, the material of the infrared spectrum window D1 of the multiple total reflection infrared spectrum analyzer is monocrystalline silicon, zinc selenide, diamond or calcium fluoride, a third valve V3 is arranged on a feeding pipeline of a second liquid storage tank T2, a fourth valve V4 is arranged on a feeding pipeline of a third liquid storage tank T3, a fifth valve V5 is arranged on a discharge port pipeline at the lower end of a fourth liquid storage tank T4 which is connected with an ion exchange bed X1, and a second valve V2 is arranged on a discharge port pipeline at the upper end of an ion exchange bed X1 which is connected with a fourth liquid storage tank T.
Referring to fig. 1, the first liquid storage tank T1 is a raw liquid tank, the second liquid storage tank T2 is a waste liquid tank, the third liquid storage tank T3 is a circulating alkali liquid tank, the fourth liquid storage tank T4 is a purifying liquid tank, the fifth liquid storage tank T5 is a deionized water tank, the sixth liquid storage tank T6 is a purifying alkali liquid tank, gas discharge ports are formed at the tops of the second liquid storage tank T2 and the fourth liquid storage tank T4, and the sixth liquid storage tank T6 contains alkali solution such as sodium hydroxide and potassium hydroxide required for regeneration of ion exchange resin.
Referring to fig. 1, the device is initially in a state where the first valve V1-the eighth valve V8, the first flowmeter F1-the third flowmeter F3 are all closed, and the device is started and then sequentially and cyclically operated according to the following steps:
1) purifying: the organic amine solution to be purified is contained in a first liquid storage tank T1, the circulation is started, a first liquid adding pump P1, a first valve V1 and a second valve V2 are manually started, the amine solution is added from the bottom of an ion exchange bed X1, the solution entering an ion exchange bed X1 is purified and then enters a fourth liquid storage tank T4 from the top, and after the purification process is operated for a period of time, the device returns to the initial state;
2) inert gas purging: manually opening an inert gas cylinder C1, a first flow meter F1 and a fifth valve V5, blowing inert gas from the top of the ion exchange bed X1, discharging the amine solution remained in the ion exchange bed X1 into a fourth liquid storage tank T4, and returning the device to the initial state;
3) washing with water: manually opening a seventh valve V7 to enable deionized water in a fifth liquid storage tank T5 to be added into an ion exchange bed X1 from the top, closing the seventh valve V7 after reaching a certain liquid level, manually opening a third valve V3 to discharge waste liquid to a second liquid storage tank T2 after the deionized water soaks ion exchange resin in the ion exchange bed X1 for a period of time, if the multiple total reflection infrared spectrometer D1 monitors that the concentration of an amine solution in the water washing waste liquid is high, closing the third valve V3, and simultaneously opening a fifth valve V5 to enable high-concentration waste liquid to flow into the fourth liquid storage tank T4, and enabling the device to be recovered to the initial state;
4) inert gas purging: manually opening an inert gas bottle C1 and a first flowmeter F1, manually controlling to open a third valve V3 or a fifth valve V5 according to the test result of the multiple total reflection infrared spectrometer D1, if the amine concentration in the previous step is lower than a set value, opening the third valve V3 to discharge waste liquid into a second liquid storage tank T2, otherwise, opening the fifth valve V5 to discharge the waste liquid into a fourth liquid storage tank T4; the time of gas purging is controlled by a multiple total reflection infrared spectrum analyzer D1, if the amine concentration in the previous step is higher than a set value, the purging time is prolonged, then the steps (3) and (4) of water washing and inert gas purging are repeated until the amine concentration in the discharged waste liquid is lower than the set value, and the system recovers the initial state;
5) pre-regeneration: manually starting a second liquid adding pump P2, opening a sixth valve V6 and a third valve V3, injecting circulating alkali liquor in a third liquid storage tank T3 from the top of an ion exchange bed X1, leaching ion exchange resin from top to bottom for pre-regeneration, allowing generated liquid to flow into a second liquid storage tank T2, and recovering the device to the initial state; the multiple total reflection infrared spectrometer D1 records the amine concentration in the effluent liquid at the bottom of the ion exchange bed X1, if the amine concentration is higher, the judgment value of the multiple total reflection infrared spectrometer D1 on the amine concentration in the water washing step in the next purification cycle is reduced, and the time of water washing and inert gas purging is prolonged;
6) regeneration: manually starting a second liquid adding pump P2, an eighth valve V8 and a fourth valve V4, injecting the alkaline liquor in a sixth liquid storage tank T6 from the top of an ion exchange bed X1 through the second liquid adding pump P2, washing impurity ions adsorbed on the surface of the resin from top to bottom to regenerate the resin, collecting the washed waste liquor into a third liquid storage tank T3 as circulating alkaline liquor, and recovering the device to the initial state; the multiple total reflection infrared spectrum analyzer D1 records the amine concentration in the circulating alkali liquor flowing out from the bottom of the ion exchange bed X1, if the amine concentration is higher, the amount of the amine solution flowing into the ion exchange bed X1 is increased by combining the result of the third flow meter F3 in the next circulation, the subsequent inert gas purging time is prolonged, the judgment value of the multiple total reflection infrared spectrum analyzer D1 on the amine concentration in the water washing step in the next purification circulation is reduced, and the water washing time and the inert gas purging time are prolonged;
7) inert gas purging: manually opening an inert gas cylinder C1, a first flow meter F1 and a third valve V3, discharging the alkali liquor remained in the ion exchange bed X1 into a second liquid storage tank T2, and restoring the device to the initial state;
8) and (5) completing the circulation and starting the next circulation.
This low-loss organic amine solution purifier passes through multiple total reflection infrared spectrum appearance D1 real-time detection ion exchange bed X1 discharge solution in organic amine concentration, and the staff of being convenient for passes through the opening or closing of multiple total reflection infrared spectrum appearance D1 real-time detection result control valve, has avoided prior art to adopt the operating procedure of solidification to respond poorly to the actual operating conditions, can not independently optimize the shortcoming of operational parameter. Furthermore, the utility model can also set the first valve V1-the seventh valve V7 as the electric control valve, the multiple total reflection infrared spectrum analyzer D1 detects and adds the input purification device control device, and each electric control valve can be automatically controlled correspondingly according to the detected concentration; the utility model discloses can combine amine solution measurement and purifier operation procedure function independently adjusted together, can reduce the loss through optimizing operating parameter with purifier operation main step's amine loss informationization, reduce the running cost.
Example 1:
the ion exchange bed X1 is filled with type II anion exchange resin, the multiple total reflection infrared spectrometer D1 adopts a silicon window, the reflection times on the window are 20 times, an inert gas cylinder C1 is a nitrogen cylinder, the first liquid storage tank T1 is filled with methyldiethanolamine solution to be purified, the concentration is 30 wt%, and the sixth liquid storage tank T6 is filled with 5 wt% potassium hydroxide aqueous solution.
After the system is started, the method comprises the following steps:
1) purifying: the organic amine solution to be purified is contained in a first liquid storage tank T1, the circulation is started, a first liquid adding pump P1, a first valve V1 and a second valve V2 are manually started, the amine solution is added from the bottom of an ion exchange bed X1, and the solution entering an ion exchange bed X1 is purified and then enters a fourth liquid storage tank T4 from the top; the linear velocity of the methyldiethanolamine solution flowing through the surface of the resin is 1 cm/min; the purification step lasts for 0.5 hour, and the device returns to the initial state;
2) inert gas purging: manually opening an inert gas cylinder C1, a first flow meter F1 and a fifth valve V5, blowing inert gas from the top of the ion exchange bed X1, discharging the amine solution remained in the ion exchange bed X1 into a fourth liquid storage tank T4, and returning the device to the initial state when the blowing continuous default value is 2 minutes;
3) washing with water: manually opening a seventh valve V7 to enable deionized water in a fifth liquid storage tank T5 to be added into an ion exchange bed X1 from the top, closing the seventh valve V7 after reaching a certain liquid level, manually opening a third valve V3 to discharge waste liquid to a second liquid storage tank T2 after the deionized water soaks ion exchange resin in the ion exchange bed X1 for a period of time, if the concentration of an amine solution in the water washing waste liquid is higher than 3% by a multiple total reflection infrared spectrometer D1, closing the third valve V3, simultaneously opening a fifth valve V5 to enable high-concentration waste liquid to flow into the fourth liquid storage tank T4, and enabling the device to be recovered to an initial state;
4) inert gas purging: manually opening an inert gas bottle C1 and a first flowmeter F1, manually controlling to open a third valve V3 or a fifth valve V5 according to the test result of the multiple total reflection infrared spectrometer D1, if the amine concentration in the previous step is lower than 3 percent, opening the third valve V3 to discharge the waste liquid into a second liquid storage tank T2, otherwise, opening the fifth valve V5 to discharge the waste liquid into a fourth liquid storage tank T4; the time of gas purging is controlled by a multiple total reflection infrared spectrum analyzer D1, if the amine concentration in the previous step is higher than the set value by 3 percent, the purging time is prolonged, then the steps (3) and (4) of water washing and inert gas purging are repeated until the amine concentration in the discharged waste liquid is lower than the set value, and the system recovers the initial state;
5) pre-regeneration: manually starting a second liquid adding pump P2, opening a sixth valve V6 and a third valve V3, injecting circulating alkali liquor in a third liquid storage tank T3 from the top of an ion exchange bed X1, leaching ion exchange resin from top to bottom for pre-regeneration, allowing generated liquid to flow into a second liquid storage tank T2, and recovering the device to the initial state; the multiple total reflection infrared spectrometer D1 records the amine concentration in the effluent waste liquid at the bottom of the ion exchange bed X1, if the amine concentration is higher than 3%, the judgment value of the multiple total reflection infrared spectrometer D1 on the amine concentration in the water washing step in the next purification cycle is reduced to 2%, and the time of water washing and inert gas purging is prolonged to 2 times of the default value;
6) regeneration: manually starting a second liquid adding pump P2, an eighth valve V8 and a fourth valve V4, injecting the alkaline liquor in a sixth liquid storage tank T6 from the top of an ion exchange bed X1 through the second liquid adding pump P2, washing impurity ions adsorbed on the surface of the resin from top to bottom to regenerate the resin, collecting the washed waste liquor into a third liquid storage tank T3 as circulating alkaline liquor, and recovering the device to the initial state; the multiple total reflection infrared spectrum analyzer D1 records the amine concentration in the circulating alkali liquor flowing out from the bottom of the ion exchange bed X1, if the amine concentration is higher, the amount of the amine solution flowing into the ion exchange bed X1 in the next cycle is increased to be 1.5 times of that in the current cycle by combining with the result of a third flow meter F3, the subsequent inert gas purging time is prolonged to be 2 times of the default value, the judgment value of the multiple total reflection infrared spectrum analyzer D1 on the amine concentration in the water washing step in the next purification cycle is reduced to be 2%, and the water washing time and the inert gas purging time are prolonged to be 2 times of the default time;
7) inert gas purging: manually opening an inert gas cylinder C1, a first flow meter F1 and a third valve V3, discharging the alkali liquor remained in the ion exchange bed X1 into a second liquid storage tank T2, and restoring the device to the initial state;
8) and (5) completing the circulation and starting the next circulation.
The water system and inert gas purge step times for the next cycle are modified as in step 5) or 6) for 3 consecutive cycles, increasing the default time for the duration of these two steps by a factor of 1. If the default time is improved by more than 5 times after a plurality of cycles, the device sends a notice to the operating personnel to carry out equipment overhaul and maintenance.
Example 2:
anion-cation exchange resin is filled in an ion exchange bed X1, a zinc selenide window is adopted as a multiple total reflection infrared spectrometer D1, the number of reflections on the window is 25, an inert gas cylinder C1 is a nitrogen cylinder, monoethanolamine solution to be purified is filled in a first liquid storage tank T1, the concentration of the monoethanolamine solution is 35 wt%, and sodium hydroxide aqueous solution with the concentration of 5 wt% is filled in a sixth liquid storage tank T6.
After the system is started, the method comprises the following steps:
1) purifying: the monoethanolamine solution to be purified is contained in a first liquid storage tank T1, the circulation is started, a first liquid adding pump P1, a first valve V1 and a second valve V2 are manually started, amine liquid is added from the bottom of an ion exchange bed X1, and the solution entering an ion exchange bed X1 is purified and then enters a fourth liquid storage tank T4 from the top; the linear velocity of the monoethanolamine solution flowing through the resin surface is 0.5 cm/min; the purification step lasts for 50 minutes, and the device returns to the initial state;
2) inert gas purging: manually opening an inert gas cylinder C1, a first flow meter F1 and a fifth valve V5, blowing inert gas from the top of an ion exchange bed X1, discharging monoethanolamine solution remained in the ion exchange bed X1 into a fourth liquid storage tank T4, and returning the device to the initial state when the default value of blowing is 2 minutes;
3) washing with water: manually opening a seventh valve V7 to enable deionized water in a fifth liquid storage tank T5 to be added into an ion exchange bed X1 from the top, closing the seventh valve V7 after reaching a certain liquid level, manually opening a third valve V3 to discharge waste liquid to a second liquid storage tank T2 after the deionized water soaks the ion exchange resin in the ion exchange bed X1 for a period of time, if the multiple total reflection infrared spectrometer D1 monitors that the concentration of monoethanolamine solution in the water washing waste liquid is higher than 3%, closing the third valve V3, simultaneously opening a fifth valve V5 to enable high-concentration waste liquid to flow into the fourth liquid storage tank T4, and enabling the device to be recovered to the initial state;
4) inert gas purging: manually opening an inert gas bottle C1 and a first flowmeter F1, manually controlling to open a third valve V3 or a fifth valve V5 according to the test result of a multiple total reflection infrared spectrometer D1, if the monoethanolamine solution in the previous step is lower than 3%, opening the third valve V3 to discharge the waste liquid into a second liquid storage tank T2, otherwise, opening the fifth valve V5 to discharge the waste liquid into a fourth liquid storage tank T4; the time of gas purging is controlled by a multiple total reflection infrared spectrum analyzer D1, if the concentration of the monoethanolamine solution in the previous step is higher than the set value by 3%, the purging time is prolonged, then the steps (3) and (4) of water washing and inert gas purging are repeated until the concentration of the monoethanolamine solution in the discharged waste liquid is lower than the set value by 3%, and the system is recovered to the initial state;
5) pre-regeneration: manually starting a second liquid adding pump P2, opening a sixth valve V6 and a third valve V3, injecting circulating alkali liquor in a third liquid storage tank T3 from the top of an ion exchange bed X1, leaching ion exchange resin from top to bottom for pre-regeneration, allowing generated liquid to flow into a second liquid storage tank T2, and recovering the device to the initial state; the multiple total reflection infrared spectrometer D1 records the amine concentration in the effluent liquid at the bottom of the ion exchange bed X1, if the monoethanolamine solution concentration is higher than 3%, the judgment value of the multiple total reflection infrared spectrometer D1 on the monoethanolamine solution concentration in the water washing step in the next purification cycle is reduced to 2%, and the time of water washing and inert gas purging is prolonged to 2 times of the default value;
6) regeneration: manually starting a second liquid adding pump P2, an eighth valve V8 and a fourth valve V4, injecting the alkaline liquor in a sixth liquid storage tank T6 from the top of an ion exchange bed X1 through the second liquid adding pump P2, washing impurity ions adsorbed on the surface of the resin from top to bottom to regenerate the resin, collecting the washed waste liquor into a third liquid storage tank T3 as circulating alkaline liquor, and recovering the device to the initial state; the multiple total reflection infrared spectrum analyzer D1 records the concentration of monoethanolamine solution in the circulating alkali liquor flowing out from the bottom of the ion exchange bed X1, if the concentration of the monoethanolamine solution is higher, the amount of the amine solution flowing into the ion exchange bed X1 in the next cycle is increased to 1.5 times of the previous cycle by combining the result of a third flow meter F3, the subsequent inert gas purging time is prolonged to 2 times of the default value, the judgment value of the multiple total reflection infrared spectrum analyzer D1 on the amine concentration in the water washing step in the next purification cycle is reduced to 2%, and the water washing time and the inert gas purging time are prolonged to 2 times of the default time;
7) inert gas purging: manually opening an inert gas cylinder C1, a first flow meter F1 and a third valve V3, discharging the alkali liquor remained in the ion exchange bed X1 into a second liquid storage tank T2, and restoring the device to the initial state;
8) and (5) completing the circulation and starting the next circulation.
It will be appreciated by those skilled in the art that the invention may be embodied in other specific forms without departing from the spirit or essential characteristics thereof. The embodiments disclosed above are therefore to be considered in all respects as illustrative and not restrictive. All changes which come within the scope of the invention or which are equivalent to the scope of the invention are embraced by the invention.
Claims (7)
1. A low-loss organic amine solution purification apparatus comprising an ion exchange bed (X1), characterized in that: an inert gas cylinder (C1), a fifth liquid storage tank (T5) and a second liquid adding pump (P2) are mounted at a feed inlet at the upper end of the ion exchange bed (X1) through pipelines, a first flowmeter (F1) is mounted on a gas outlet pipeline of the inert gas cylinder (C1), a seventh valve (V7) is mounted on a discharge pipeline of the fifth liquid storage tank (T5), a feed inlet at the lower end of the ion exchange bed (X1) is connected with a first liquid adding pump (P1) through a pipeline, and a material pumping port of the first liquid adding pump (P1) is connected with a first liquid storage tank (T1) through a pipeline;
a discharge port at the lower end of the ion exchange bed (X1) is connected with a second liquid storage tank (T2), a third liquid storage tank (T3) and a fourth liquid storage tank (T4) through pipelines, and a discharge pipeline at the lower end of the ion exchange bed (X1) is provided with a multiple total reflection infrared spectrum analyzer (D1);
ion exchange bed (X1) upper end discharge gate has fourth liquid storage pot (T4) through the pipe connection, install third valve (V3) on the feed conduit of second liquid storage pot (T2), install fourth valve (V4) on the feed conduit of third liquid storage pot (T3), install fifth valve (V5) on fourth liquid storage pot (T4) connection ion exchange bed (X1) lower extreme discharge gate pipeline, install second valve (V2) on fourth liquid storage pot (T4) connection ion exchange bed (X1) upper end discharge gate pipeline.
2. The purification apparatus for low-loss organic amine solution as claimed in claim 1, wherein: and a discharge pipeline of the second liquid adding pump (P2) is provided with a second flowmeter (F2), and a material pumping port of the second liquid adding pump (P2) is connected with a third liquid storage tank (T3) and a sixth liquid storage tank (T6) through pipelines.
3. The purification apparatus for low-loss organic amine solution as claimed in claim 2, wherein: a sixth valve (V6) is arranged on a discharge pipeline of the third liquid storage tank (T3), and an eighth valve (V8) is arranged on a discharge pipeline of the sixth liquid storage tank (T6).
4. The purification apparatus for low-loss organic amine solution as claimed in claim 1, wherein: and a third flow meter (F3) and a first valve (V1) are arranged on a discharge pipeline of the first charging pump (P1).
5. The purification apparatus for low-loss organic amine solution as claimed in claim 1, wherein: the liquid storage tank (T1) is a raw liquid tank, the liquid storage tank (T2) is a waste liquid tank, the liquid storage tank (T3) is a circulating alkali liquid tank, the liquid storage tank (T4) is a purified liquid tank, and the liquid storage tank (T5) is a deionized water tank.
6. The purification apparatus for low-loss organic amine solution as claimed in claim 2, wherein: the sixth liquid storage tank (T6) is a clean lye tank.
7. The purification apparatus for low-loss organic amine solution as claimed in claim 1, wherein: the top parts of the second liquid storage tank (T2) and the fourth liquid storage tank (T4) are provided with gas discharge ports.
Priority Applications (1)
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| CN110508331A (en) * | 2019-09-19 | 2019-11-29 | 华能国际电力股份有限公司 | A kind of low-loss Amine Solutions purification device and its application method |
| WO2021052432A1 (en) * | 2019-09-19 | 2021-03-25 | 华能国际电力股份有限公司 | Low-loss organic amine solution purification device and use method thereof |
| CN110508331B (en) * | 2019-09-19 | 2023-08-18 | 华能国际电力股份有限公司 | Low-loss organic amine solution purification device and application method thereof |
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