CN217646123U - Zeolite adsorption temperature and pressure changing system for recovering dry ammonium fluoride - Google Patents
Zeolite adsorption temperature and pressure changing system for recovering dry ammonium fluoride Download PDFInfo
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- CN217646123U CN217646123U CN202221031814.8U CN202221031814U CN217646123U CN 217646123 U CN217646123 U CN 217646123U CN 202221031814 U CN202221031814 U CN 202221031814U CN 217646123 U CN217646123 U CN 217646123U
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Abstract
The utility model relates to a recovery drying system, in particular to a zeolite adsorption temperature and pressure varying system for recovering and drying ammonium fluoride, which comprises a fan, a pressure varying subsystem and a temperature varying subsystem which are connected in sequence; the pressure swing subsystem comprises a pressure swing adsorption tank set, a vacuum pump, a heat exchanger, a gas-liquid separator, a product tank and a gas replenishing tank; the upper end of the pressure swing adsorption tank set is connected with a gas replenishing tank, and the lower end of the pressure swing adsorption tank set is sequentially connected with a vacuum pump, a heat exchanger, a gas-liquid separator and a product tank; the temperature change subsystem comprises a temperature change adsorption tank set, a vacuum pump, a heat exchanger, a product tank and a hot steam pipeline; the upper end of the temperature swing adsorption tank set is connected with a vacuum pump, a heat exchanger and a product tank in sequence, and the lower end is connected with a hot steam pipeline. Compared with the prior art, the utility model discloses combine pressure swing adsorption and temperature swing adsorption to carry out the recovery drying process of ammonium fluoride tail gas, can effectively retrieve the ammonium fluoride in the tail gas.
Description
Technical Field
The utility model relates to a retrieve drying system, concretely relates to zeolite adsorption temperature and pressure changing system for retrieving dry ammonium fluoride.
Background
Ammonium fluoride, an inorganic compound of formula NH 4 And F, an ionic compound which is white crystalline powder, is easy to deliquesce, is soluble in water and methanol, is slightly soluble in ethanol and is insoluble in acetone, and is mainly used as a glass etching agent, a wood and wine-brewing preservative, a disinfectant, an analytical reagent, a zirconium spot reagent, a fiber mordant and a reagent for extracting rare elements.
At present, ammonium fluoride tail gas of an ammonium fluoride production plant can contain 50 percent (volume fraction) of ammonium fluoride, and a small amount of butanol and water vapor are mixed, so that the tail gas can meet the requirement of direct tail gas emission in the emission standard of pollutants for synthetic resin industry (GB 31572-2015); however, a large amount of ammonium fluoride is converted and wasted in the treatment process, i.e., raw materials are wasted, and the treatment cost is increased.
Chinese patent CN111410210A discloses a method for recovering ammonium fluoride from ammonium fluoride waste water, comprising the following steps: s1, adding hydrofluoric acid into ammonium fluoride wastewater, adjusting the pH of the wastewater to 5-6, and adding NH in the wastewater 3 Converted into ammonium fluoride salt and dissolved in the wastewater; s2, pumping the ammonium fluoride wastewater after pH adjustment into an evaporator, wherein the evaporator is in a vacuum environment, carrying out pressure reduction and constant temperature evaporation on the ammonium fluoride wastewater in the evaporator, wherein the evaporation temperature is 50-70 ℃, the evaporation time is 1-5 h, the ammonium fluoride is continuously separated out in the evaporation process to obtain crystallized ammonium fluoride, and the generated condensed water is recycled. However, the patent aims at the recovery of ammonium fluoride in the ammonium fluoride waste water, and cannot provide an effective method for the recovery of ammonium fluoride in the ammonium fluoride tail gas; and at present, there is no system for recovering ammonium fluoride from the production tail gas, so it is urgently needed to provide an effective recovery system for recovering ammonium fluoride tail gas from an ammonium fluoride production plant.
SUMMERY OF THE UTILITY MODEL
The utility model aims at solving at least one of the problems and providing a zeolite adsorption temperature and pressure changing system for recovering dry ammonium fluoride, which realizes the high-efficiency, high-quality and simple recovery of the dry ammonium fluoride in the production tail gas.
The purpose of the utility model is realized through the following technical scheme:
a zeolite adsorption temperature and pressure changing system for recovering dry ammonium fluoride comprises a fan, a pressure changing subsystem and a temperature changing subsystem which are connected in sequence;
the pressure swing subsystem comprises a pressure swing adsorption tank set, a vacuum pump, a heat exchanger, a gas-liquid separator, a product tank and a gas supplement tank; the upper end of the pressure swing adsorption tank set is connected with a gas supplement tank, and the lower end of the pressure swing adsorption tank set is sequentially connected with a vacuum pump, a heat exchanger, a gas-liquid separator and a product tank;
the temperature-changing subsystem comprises a temperature-changing adsorption tank group, a vacuum pump, a heat exchanger, a product tank and a hot steam pipeline; the upper end of the temperature swing adsorption tank set is sequentially connected with a vacuum pump, a heat exchanger and a product tank, and the lower end of the temperature swing adsorption tank set is connected with a hot steam pipeline;
the ammonium fluoride tail gas firstly enters a pressure swing adsorption tank set of a pressure swing subsystem through a fan to carry out pressure swing adsorption, then enters a temperature swing adsorption tank set of the temperature swing subsystem to carry out temperature swing adsorption, and the treated residual gas is discharged to the air; and (4) desorbing the pressure swing adsorption tank group and the temperature swing adsorption tank group after the adsorption is finished, and recovering the generated gas to the product tank.
Preferably, the pressure swing adsorption tank set comprises two pressure swing adsorption tanks arranged in parallel. When the pressure swing adsorption device is used, the two pressure swing adsorption tanks are alternately used, and when one of the two pressure swing adsorption tanks is used for adsorption, the other pressure swing adsorption tank is used for desorption, so that the whole pressure swing adsorption device can be continuously operated.
Preferably, the pressure swing adsorption tank set is vacuumized by a vacuum pump to perform pressure reduction desorption. The pressure swing adsorption and the decompression desorption are carried out by utilizing the characteristic that the equilibrium adsorption quantity of the adsorbent is increased along with the increase of the component partial pressure in the pressure swing adsorption.
Preferably, the thermal swing adsorption tank group comprises two thermal swing adsorption tanks arranged in parallel. When the temperature swing adsorption device is used, the two temperature swing adsorption tanks are alternately used, and when one of the temperature swing adsorption tanks is used for adsorption, the other temperature swing adsorption tank is used for desorption, so that the whole temperature swing adsorption device can be continuously operated.
Preferably, the temperature swing adsorption tank set is subjected to temperature rise desorption through hot steam in a hot steam pipeline. Normal temperature adsorption and temperature rising desorption are adopted by utilizing the characteristic that the equilibrium adsorption capacity of the adsorbent is reduced along with the temperature rise in the temperature changing adsorption. The hot steam piping connected in this application can use the utility piping in the plant to reduce equipment investment and energy consumption.
Preferably, the hot steam is water vapor. The water vapor is the most common heating medium in the industry and can be conveniently connected into an industrial production system.
Preferably, the adsorbent filled in the pressure swing adsorption tank group and the temperature swing adsorption tank group adopts zeolite molecular sieve adsorbent. The zeolite molecular sieve adsorbent has higher selectivity and larger unit adsorption quantity for target gas in the mixed gas, and can be used for drying water vapor and other impurity gases in the ammonium fluoride mixed gas.
Preferably, the flow rate of the fan is 300-400m 3 /h。
Preferably, the gas replenishing tank replenishes the pressure swing adsorption tank with an inert gas to increase the pressure (usually, the pressure needs to be adjusted when the desorption is changed to the adsorption), and the inert gas can be a gas which does not affect the adsorption, such as nitrogen, helium, and the like.
Preferably, the system further comprises a control system, wherein the control system comprises a pressure gauge and an organic gas detector which are arranged in the pressure swing adsorption tank group, a thermometer and an organic gas detector which are arranged in the temperature swing adsorption tank group, valves arranged on each connecting passage, and a controller which is respectively and electrically connected with the pressure gauge, the thermometer, the organic gas detector and the valves. Automatic control and automatic switching of the adsorption tank groups are realized through the use of the control system.
Preferably, the controller is a PLC controller.
The utility model discloses a theory of operation does:
the ammonium fluoride tail gas to be treated is sent into a pressure swing adsorption tank set for pressure swing adsorption under the action of a fan, the tail gas after adsorption enters the pressure swing adsorption tank set for temperature swing adsorption, and the tail gas (residual gas) after adsorption meets the emission standard and can be directly discharged into the atmosphere; and then desorption is carried out, the pressure of the pressure swing adsorption tank group is reduced through a vacuum pump to realize desorption, the desorbed gas is treated by a heat exchanger and a gas-liquid separator and then reaches the product tank, the temperature swing adsorption tank group is introduced with hot steam through a hot steam pipeline to raise the temperature to realize desorption, and the desorbed gas enters the product tank after the suction of the vacuum pump and the heat exchange of a condenser.
Compared with the prior art, the utility model discloses following beneficial effect has:
1. the system combines pressure swing adsorption and temperature swing adsorption to recycle the ammonium fluoride tail gas, not only can effectively recycle substantially all ammonium fluoride in the tail gas, but also the recycled ammonium fluoride is in a dry state and has high purity, and the ammonium fluoride can be directly used as a product without further treatment; meanwhile, the treated tail gas can be directly discharged without further treatment. And the cost used for adsorption is low, and the adsorbent can be treated on a large scale and in a large scale, and is suitable for industrial application.
2. The utility model discloses still adopt automatic control technique and monitoring technology simultaneously, convenient operation, operation safe and reliable, the system is equipped with the detector and the safe value of temperature, pressure and key pollution index, and when exceeding safety range, the system will send the warning automatically.
3. The utility model discloses also can handle all kinds of volatile organic gases, the gas emission after the processing accords with the technical index of synthetic resin industrial pollutant emission standard (GB 31572-2015), and the gaseous recoverable apparatus for producing raw materials that is used as of desorption out not only practices thrift the environmental protection cost, but also brings economic benefits.
Drawings
FIG. 1 is a schematic diagram of a system of the present invention;
in the figure: 1-a pressure swing adsorption tank group; 2-a vacuum pump; 3-a heat exchanger; 4-a gas-liquid separator; 5-a product tank; 6-gas make-up tank; 7-temperature swing adsorption tank group; 8-hot steam pipes; 9-a fan.
Detailed Description
The present invention will be described in detail with reference to the accompanying drawings and specific embodiments.
Example 1
A zeolite adsorption temperature and pressure swing system for recovering dry ammonium fluoride, as shown in figure 1, comprises a fan 9, a pressure swing subsystem and a temperature and pressure swing subsystem which are connected in sequence;
the pressure swing subsystem comprises a pressure swing adsorption tank group 1, a vacuum pump 2, a heat exchanger 3, a gas-liquid separator 4, a product tank 5 and a gas supplement tank 6; the upper end of the pressure swing adsorption tank group 1 is connected with a gas supplement tank 6, and the lower end is sequentially connected with a vacuum pump 2, a heat exchanger 3, a gas-liquid separator 4 and a product tank 5;
the temperature change subsystem comprises a temperature change adsorption tank group 7, a vacuum pump 2, a heat exchanger 3, a product tank 5 and a hot steam pipeline 8; the upper end of the temperature swing adsorption tank set 7 is sequentially connected with the vacuum pump 2, the heat exchanger 3 and the product tank 5, and the lower end is connected with the hot steam pipeline 8;
the ammonium fluoride tail gas firstly enters a pressure swing adsorption tank set 1 of a pressure swing subsystem for pressure swing adsorption through a fan 9, then enters a temperature swing adsorption tank set 7 of the temperature swing subsystem for temperature swing adsorption, and the treated residual gas is discharged; and (3) desorbing the pressure swing adsorption tank group 1 and the temperature swing adsorption tank group 7 after the adsorption is finished, and recovering the generated gas to the product tank 5.
More specifically, in the present embodiment:
the tail gas of ammonium fluoride production plant is used as tail gas source, which contains 50% of ammonium fluoride (volume percentage, the same below), 25% of butanol and 15% of water vapor, the rest gas does not affect the discharge and treatment, and the temperature is 240 ℃. The flow rate of the ammonium fluoride tail gas is 350m 3 H, the pressure of the pressure swing adsorption tank group 1 during adsorption is set to be 2 kilograms, the sizes of all the adsorption tanks are consistent and are set to be 5.8m 3 In particular, in this embodiment, in order to improve the recovery rate as much as possible, the adsorbent provided in CN106975444A may be selected, and of course, in other embodiments, a conventional commercially available zeolite adsorbent may also be selected. In other embodiments, the various items of data may be selected and adjusted according to production requirements, standards, requirements, and the like.
The pressure swing adsorption tank group 1 of the embodiment comprises two pressure swing adsorption tanks, and the two pressure swing adsorption tanks are alternately adsorbed and desorbed during use, and the temperature swing adsorption tank group 7 is also provided with two temperature swing adsorbers, and alternately adsorbed and desorbed during use. The tail gas enters one of the pressure swing adsorption tanks for adsorption by the fan 9, the other pressure swing adsorption tank is in the desorption process, the adsorbed gas enters the temperature swing adsorption tank for adsorption, and the adsorbed gas is directly discharged into the air. Then desorbing the fully adsorbed adsorbent, connecting the lower end of the pressure swing adsorption tank set 1 with a vacuum pump 2, vacuumizing the pressure swing adsorption tank set 1 through the vacuum pump 2 to reduce the pressure in the tank for desorption, and enabling the desorbed gas to enter a product tank 5 through a heat exchanger 3 and a gas-liquid separator 4; in order to ensure that the pressure meets the adsorption requirement in the next adsorption, the upper part of the pressure swing adsorption tank set 1 is connected with a gas supplement tank 6, wherein high-pressure inert gas is stored, and sufficient pressure is supplemented to the pressure swing adsorption tank set 1. The lower end of the temperature swing adsorption tank group 7 is connected with a hot steam tank, in the embodiment, water steam which is conventionally used in industry is selected as hot steam to heat the adsorbent for desorption, the upper end of the temperature swing adsorption tank group 7 is connected with a vacuum pump 2, desorbed gas is pumped out through the vacuum pump 2, and the desorbed gas enters the product tank 5 after being condensed by a condenser.
In order to further provide automation performance, a control system is also electrically connected (transmitting electric signals, for example, the signals can be connected through wires or cables) and specifically comprises a PLC controller, a pressure gauge installed in the pressure swing adsorption tank group 1, a temperature gauge installed in the temperature swing adsorption tank group 7, an organic gas detector installed at the discharge outlet of each adsorption tank group, and valves installed on each communication pipeline. The PLC can realize integral automatic control and can give an alarm in time when a problem occurs.
It was determined that when the adsorbent of the present invention was used to treat a synthesis gas of ammonium fluoride and hydrogen, the purity of ammonium fluoride was at least 99%, even 99.9% and 99.99%. When treating ammonium fluoride and water vapor, the saturated adsorption capacity of ammonium fluoride can reach at least 0.014g/g (0.875 mmol/g), and the breakthrough adsorption capacity can reach at least 0.012g/g (0.75 mmol/g). The system can effectively adsorb ammonium fluoride, and then recover to obtain a high-purity product, and meanwhile, the whole process is simple and is suitable for industrial use.
The embodiments described above are intended to facilitate the understanding and use of the invention by those skilled in the art. It will be readily apparent to those skilled in the art that various modifications to these embodiments may be made, and the generic principles described herein may be applied to other embodiments without the use of the inventive faculty. Therefore, the present invention is not limited to the above embodiments, and those skilled in the art should make improvements and modifications within the scope of the present invention according to the disclosure of the present invention.
Claims (10)
1. The zeolite adsorption temperature and pressure changing system for recovering the dry ammonium fluoride is characterized by comprising a fan (9), a pressure changing subsystem and a temperature changing subsystem which are connected in sequence;
the pressure swing subsystem comprises a pressure swing adsorption tank set (1), a vacuum pump (2), a heat exchanger (3), a gas-liquid separator (4), a product tank (5) and a gas supplement tank (6); the upper end of the pressure swing adsorption tank group (1) is connected with a gas supplement tank (6), and the lower end is sequentially connected with a vacuum pump (2), a heat exchanger (3), a gas-liquid separator (4) and a product tank (5);
the temperature-changing subsystem comprises a temperature-changing adsorption tank group (7), a vacuum pump (2), a heat exchanger (3), a product tank (5) and a hot steam pipeline (8); the upper end of the temperature swing adsorption tank group (7) is sequentially connected with a vacuum pump (2), a heat exchanger (3) and a product tank (5), and the lower end is connected with a hot steam pipeline (8);
ammonium fluoride tail gas firstly enters a pressure swing adsorption tank set (1) of a pressure swing subsystem through a fan (9) for pressure swing adsorption, then enters a temperature swing adsorption tank set (7) of a temperature swing subsystem for temperature swing adsorption, and the treated residual gas is discharged; and (3) desorbing the pressure swing adsorption tank group (1) and the temperature swing adsorption tank group (7) after adsorption is finished, and recovering the generated gas into the product tank (5).
2. The zeolite adsorption temperature and pressure swing system for dry ammonium fluoride recovery of claim 1 wherein said bank of pressure swing adsorption tanks (1) comprises two pressure swing adsorption tanks arranged in parallel.
3. The zeolite adsorption temperature and pressure swing system for recovering dry ammonium fluoride of claim 2, wherein the pressure swing adsorption tank set (1) is vacuumized by the vacuum pump (2) for pressure and pressure reduction desorption.
4. The zeolitic adsorptive temperature swing adsorption system for the recovery of dry ammonium fluoride according to claim 1, wherein said set of temperature swing adsorption tanks (7) comprises two temperature swing adsorption tanks arranged in parallel.
5. The zeolite adsorption temperature and pressure swing system for dry ammonium fluoride recovery of claim 4 wherein the thermal swing adsorption tank train (7) is temperature swing desorbed by hot steam in hot steam line (8).
6. The zeolitic adsorption temperature and pressure swing system for recovery of dry ammonium fluoride according to claim 5, wherein said hot steam is steam.
7. The system of claim 1, wherein the adsorbent filled in the pressure swing adsorption tank set (1) and the temperature swing adsorption tank set (7) is zeolite molecular sieve adsorbent.
8. The zeolite adsorption temperature and pressure swing system for dry ammonium fluoride recovery of claim 1 wherein the fan (9) has a flow rate of 300-400m 3 /h。
9. The zeolite adsorption temperature and pressure swing system for recovery of dry ammonium fluoride of claim 1, further comprising a control system comprising a pressure gauge and an organic gas detector disposed in the pressure swing adsorption tank train (1), a temperature gauge and an organic gas detector disposed in the temperature swing adsorption tank train (7), valves disposed in each connection path, and a controller electrically connected to the pressure gauge, the temperature gauge, the organic gas detector, and the valves, respectively.
10. The zeolite adsorption temperature and pressure swing system for recovery of dry ammonium fluoride of claim 9 wherein said controller is a PLC controller.
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| Application Number | Priority Date | Filing Date | Title |
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| CN202221031814.8U CN217646123U (en) | 2022-04-29 | 2022-04-29 | Zeolite adsorption temperature and pressure changing system for recovering dry ammonium fluoride |
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| CN202221031814.8U CN217646123U (en) | 2022-04-29 | 2022-04-29 | Zeolite adsorption temperature and pressure changing system for recovering dry ammonium fluoride |
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| CN217646123U true CN217646123U (en) | 2022-10-25 |
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| CN202221031814.8U Active CN217646123U (en) | 2022-04-29 | 2022-04-29 | Zeolite adsorption temperature and pressure changing system for recovering dry ammonium fluoride |
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