CN112206756A - Desorption method of adsorbent - Google Patents
Desorption method of adsorbent Download PDFInfo
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- CN112206756A CN112206756A CN202011139964.6A CN202011139964A CN112206756A CN 112206756 A CN112206756 A CN 112206756A CN 202011139964 A CN202011139964 A CN 202011139964A CN 112206756 A CN112206756 A CN 112206756A
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/30—Processes for preparing, regenerating, or reactivating
- B01J20/34—Regenerating or reactivating
- B01J20/345—Regenerating or reactivating using a particular desorbing compound or mixture
- B01J20/3458—Regenerating or reactivating using a particular desorbing compound or mixture in the gas phase
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- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D53/00—Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols
- B01D53/02—Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols by adsorption, e.g. preparative gas chromatography
Abstract
The invention discloses a desorption method of an adsorbent, which comprises the following steps: s1, placing the adsorbent to be desorbed in a container; s2, introducing helium into the container, and maintaining the pressure in the container at 0.2-0.4 Mpa; s3, vacuumizing the container, and keeping the vacuum degree at 5-10 pa; s4, repeating the steps S2-S3; s5, repeating the step S2, cooling the adsorbent in the container to room temperature, and repeating the step S3; s6, introducing passivation gas into the container to passivate the adsorbent; s7, repeating the steps S2-S3 to obtain the desorbed adsorbent. By using the desorption method, the adsorbate on the adsorbent can be completely desorbed, high activity of the adsorbent caused by high-temperature activation is avoided, the activity of the desorbed adsorbent is reduced, the conditions that the adsorbent generates heat at high temperature and is subjected to chemical reaction in the subsequent cyclic adsorption process to introduce new impurities are avoided, and meanwhile, the desorption cost is low, so that the method is beneficial to industrial application.
Description
Technical Field
The invention relates to the technical field of adsorbent desorption, in particular to a desorption method of an adsorbent.
Background
The adsorption separation, namely the desorption process is one of the important means for purifying and separating industrial gas, and the adsorption separation technology can reduce the adsorbate adsorbed by the adsorbent saturated in adsorption to a lower range, even below the detection limit, and can be suitable for the production of large-scale ultrapure gas.
The existing desorption process can reduce the adsorption capacity of the adsorbent by adopting a method of raising the temperature, thereby achieving the desorption effect; or the adsorbent is desorbed by reducing the pressure of the system or vacuumizing; or the desorption of the adsorbent is carried out by flushing with an inert solvent or extracting with an extracting agent; other adsorbates may also be used to displace the original adsorbate from the adsorbent to complete desorption. The method usually causes incomplete desorption of the adsorbent in single implementation, and is easy to saturate in subsequent adsorbate adsorption, so that the combination of a plurality of desorption modes is mostly adopted to ensure the best desorption effect of the adsorbent. After the combined desorption step is completed, the active adsorbent subjected to high-temperature replacement can obtain a good desorption effect, but because the activity of the desorbed adsorbent is very high, the desorbed adsorbent is contacted with gas with the same activity when being used for adsorption again, so that violent chemical reaction is easy to occur, a large amount of heat is released, a large amount of impurities are generated, and the adsorption effect of the desorbed adsorbent is reduced.
Disclosure of Invention
The invention mainly aims to provide a desorption method of an adsorbent, and aims to solve the technical problems that the adsorbent after desorption is over-active, and if the adsorption activity is high or gas which is easy to react with the adsorbent is easy to generate a large amount of impurities, the adsorption effect is poor in the existing desorption method.
In order to achieve the above object, the present invention provides a desorption method of an adsorbent, comprising the steps of:
s1, placing the adsorbent to be desorbed in a container;
s2, introducing helium into the container, and maintaining the pressure in the container at 0.2-0.4 Mpa;
s3, vacuumizing the container, and keeping the vacuum degree at 5-10 pa;
s4, repeating the steps S2-S3;
s5, repeating the step S2, cooling the adsorbent in the container to room temperature, and repeating the step S3;
s6, introducing passivation gas into the container to passivate the adsorbent;
s7, repeating the steps S2-S3 to obtain the desorbed adsorbent.
Preferably, between the step S1 and the step S2, the method further comprises the following steps:
s01, introducing nitrogen into the container for purging;
s02, vacuumizing the container until the vacuum degree is 5-10 pa;
s03, heating the adsorbent in the container to a desorption temperature at which the adsorbent achieves a desorption effect;
s04, introducing nitrogen into the container, and maintaining the pressure in the container at 0.2-0.4 Mpa;
s05, repeating the step S02;
s06, repeating the steps S04-S05.
Preferably, the passivation gas is air or water vapor.
Preferably, between the step S6 and the step S7, the method further comprises the following steps: s61, repeating the step S3, and raising the temperature of the adsorbent in the container to 100-200 ℃.
Preferably, the adsorbent comprises a zeolite molecular sieve or activated alumina;
in the step S03, the desorption temperature of the zeolite molecular sieve is 320-370 ℃, and the desorption temperature of the activated alumina is 220-270 ℃.
Preferably, the temperature increase rate in the step S03 is 3-8 deg.C/min.
Preferably, in the step S01, the purge flow rate of the nitrogen gas is 3-8Nm3And h, the purging time is 1-2 h.
Preferably, the number of times of repetition in the step S7 and the number of times of repetition in the step S05 are both ≧ 4.
Preferably, the helium gas introduction time in the step S2 and the helium gas and nitrogen gas introduction time in the step S04 are both 40-80 min.
Preferably, the vacuumizing time in the step S3 and the vacuumizing time in the step S02 are both 40-80 min.
The desorption method of the adsorbent has the following beneficial effects: after the nitrogen and helium are used for desorbing the adsorbent, the adsorbent obtains a good desorption effect, passivation gas is introduced into the container, so that the adsorbent can adsorb the passivation gas to reduce the activity of the adsorbent, the passivation gas has low activity and small reaction degree with the adsorbent, desorption can be carried out in the subsequent nitrogen re-introduction process, and the adsorbent can reach a good desorption effect while having low activity through the vacuumizing step. When gas which possibly reacts with the adsorbent is introduced later, the adsorbent desorbed by the scheme still has a good adsorption effect.
Drawings
In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings used in the description of the embodiments or the prior art will be briefly described below, it is obvious that the drawings in the following description are only some embodiments of the present invention, and for those skilled in the art, other drawings can be obtained according to the structures shown in the drawings without creative efforts.
FIG. 1 is a process flow diagram of a method of desorption of an adsorbent according to the present invention.
The implementation, functional features and advantages of the objects of the present invention will be further explained with reference to the accompanying drawings.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the drawings in the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
In addition, technical solutions between various embodiments may be combined with each other, but must be realized by a person skilled in the art, and when the technical solutions are contradictory or cannot be realized, such a combination should not be considered to exist, and is not within the protection scope of the present invention.
The invention provides a desorption method of an adsorbent. The desorption method of the adsorbent is used for desorbing the adsorbent saturated in adsorption, so that the adsorbent can be recycled and reused in the adsorption of the adsorbent, the adsorbent on the adsorbent can be completely desorbed, high activity of the adsorbent caused by high-temperature activation is avoided, the activity of the desorbed adsorbent is reduced, and the conditions that the adsorbent generates heat at high temperature and is chemically reacted in the subsequent cyclic adsorption process to introduce new impurities are avoided.
In an embodiment of the present invention, a method for desorbing an adsorbent includes the following steps:
s1, placing the adsorbent to be desorbed in a container;
s2, introducing helium into the container, and maintaining the pressure in the container at 0.2-0.4 Mpa;
s3, vacuumizing the container, and keeping the vacuum degree at 5-10 pa;
s4, repeating the steps S2-S3;
s5, repeating the step S2, cooling the adsorbent in the container to room temperature, and repeating the step S3;
s6, introducing passivation gas into the container to passivate the adsorbent;
s7, repeating the steps S2-S3 to obtain the desorbed adsorbent.
Specifically, the adsorbent to be desorbed is placed in a vessel. And introducing helium into the container, wherein the pressure of the introduced helium is kept at 0.2-0.4Mpa, the introduced helium can adsorb adsorbate in the adsorbent to be desorbed to achieve the replacement effect, and the adsorbent to be desorbed after helium replacement can be desorbed. The pressure is kept in the pressure range, the pressure is relatively small and stable, and the helium has better desorption effect on the adsorbent to be desorbed; after the first desorption is finished, the container is vacuumized, so that helium gas adsorbed with adsorbate is completely removed, the helium gas is easier to remove due to the fact that the molecular weight of the helium gas is small, the vacuum degree is kept in a low range at the moment, the desorption effect of the helium gas is further promoted, and the two steps are used for finishing the first desorption process of the helium gas on the adsorbent. The introduced helium is in a normal temperature state, and is introduced again without temperature rise, so that over-severe replacement caused by over-high temperature is avoided. When the helium gas is used for desorbing the adsorbent, the desorption effect of the adsorbent is not very good when only one desorption process is performed, and the desorption process is usually repeated.
After the desorption step is repeated, the container and the adsorbent inside the container are cooled to room temperature, the desorbed adsorbent is lower than the activation temperature, so that the adsorbent does not have a particularly severe reaction with the passivation gas in the air in the subsequent air introducing step, then the passivation gas is introduced into the container, so that the adsorbent can adsorb the passivation gas to reduce the activity of the adsorbent, the passivation gas has lower activity and lower reaction degree with the adsorbent, so that the adsorbent can be desorbed in the subsequent nitrogen introducing process, and the adsorbent can achieve better desorption effect while having lower activity through the vacuumizing step. When gas which possibly reacts with the adsorbent is introduced later, the adsorbent desorbed by the scheme still has a good adsorption effect.
Further, between step S1 and step S2, the following steps are also included:
s01, introducing nitrogen into the container for purging;
s02, vacuumizing the container until the vacuum degree is 5-10 pa;
s03, heating the adsorbent in the container to a desorption temperature at which the adsorbent achieves a desorption effect;
s04, introducing nitrogen into the container, and maintaining the pressure in the container at 0.2-0.4 Mpa;
s05, repeating the step S02;
s06, repeating the steps S04-S05.
Because the price of helium is high, and large cost is consumed when the helium is used for desorption, the nitrogen is used for carrying out early-stage adsorption on the adsorbent to be desorbed, and can be used for replacing part of helium to desorb the adsorbent, so that the production cost is reduced.
Likewise, the desorption process of nitrogen for the adsorbent to be desorbed is more similar to that of helium. Firstly, purging an adsorbent in a container by using nitrogen to finish primary desorption of the adsorbent; and then vacuumizing the container, removing the nitrogen adsorbed with the adsorbate in the container, wherein the pressure in the container is 0.2-0.4Mpa, completing the desorption process of the adsorbent, heating the container to the desorption temperature after vacuumizing to promote the desorption effect of the nitrogen on the adsorbent, and then circularly introducing the nitrogen and vacuumizing for a plurality of times to ensure that the desorption effect of the adsorbent is better.
Further, the passivation gas is air or water vapor. The passivation gas in the scheme is air or water vapor. After steps S1 and S4 are completed, the adsorbent has been well desorbed, the adsorbent is cooled, and passivation gas, i.e., air or water vapor, is introduced into the container, so that the adsorbent is exposed to the air or water vapor and contacts with gases such as moisture in the air, and the adsorbent can adsorb various gases or water vapor contained in the air, thereby reducing the activation effect. The reduced activation of the adsorbent is achieved more quickly by the introduction of water vapor than by the introduction of air.
Further, between the step S6 and the step S7, the following steps are further included: s61, repeating the step S3, and raising the temperature of the adsorbent in the container to 100-200 ℃.
After introducing steam or air, raising the temperature of the container and the adsorbent to 100-200 ℃ to evaporate the steam adsorbed in the adsorbent and finish primary desorption, wherein the temperature rise at the moment should not exceed 200 ℃, otherwise, the adsorbent is in a high-activity state again, and more impurities are generated violently due to reaction in the subsequent adsorption; and then, desorbing various gases adsorbed on the adsorbent by using helium, and after the desorption process is completed, removing moisture and other impurities in the air or the water vapor, wherein the adsorbate on the adsorbent can be completely desorbed, meanwhile, the high activity of the adsorbent caused by high-temperature activation is avoided, the activity of the adsorbent after desorption is reduced, and the situations that the adsorbent generates heat at high temperature and is subjected to chemical reaction in the subsequent cyclic adsorption process to introduce new impurities are avoided. 100-150 ℃ is the preferable temperature rise range, and in the temperature range, not only can the water vapor be completely removed from the adsorbent be ensured, but also the adsorbent can be ensured to be in a lower activation range, the subsequent adsorption process can not generate violent reaction with the adsorbent, and the impurities can be relatively reduced; meanwhile, large energy does not need to be consumed, and the production cost is further reduced.
Further, the adsorbent comprises a zeolite molecular sieve or activated alumina; in step S03, the desorption temperature of the zeolite molecular sieve is 320-370 ℃, and the desorption temperature of the activated alumina is 220-270 ℃.
Specifically, the temperature raising process in step S20 is to promote the desorption effect of the adsorbent, so that the kinetic energy of the adsorbate molecules is increased and the adsorbate molecules are more easily desorbed from the adsorbent, and different temperature raising ranges are provided for different adsorbents, such as when the adsorbent is a zeolite molecular sieve, the desorption temperature is in the range of 220-. Likewise, the desorption temperature of activated alumina was 220-270 ℃.
Further, the temperature increase rate in step S03 is 3 to 8 deg.C/min. Therefore, the heating period is shorter, the desorption effect of nitrogen on the adsorbent in the desorption process is more stable, and the adjustment can be carried out adaptively.
Further, in step S01, the purge flow rate of nitrogen gas is 3 to 8Nm3And h, the purging time is 1-2 h. It can be understood that when the purge flow of nitrogen is increased, the desorption effect on the adsorbent can be improved, the impact force on the adsorbate molecules is increased synchronously due to the increase of the flow velocity of nitrogen in the container, the adsorbate is easily carried out of the adsorbent, and the purge flow of nitrogen is set to 3-8Nm m in consideration of energy saving and production cost3H; the purge time is specifically set to 1 to 2 hours, and the desorption promoting effect on the adsorbent does not increase significantly after the nitrogen purge exceeds 2 hours, and therefore, the purge time is set to 1 to 2 hours.
Further, the number of repetitions in step S7 and the number of repetitions in step S05 are ≧ 4. Therefore, the continuous effect of the helium and the nitrogen on the adsorbent can be realized only by repeating for many times, and the preferable repetition time in the scheme is 4 times, so that the better desorption effect of the adsorbent can be ensured, and the production cost range can be controlled to be proper.
Furthermore, the helium gas introduction time in the step S2 and the nitrogen gas introduction time in the step S04 are both 40-80 min. It can be understood that the helium and nitrogen are introduced for 40-80min, preferably 1h, to ensure the adsorbent has better desorption effect and relatively shorter desorption period.
Further, the vacuuming time in the step S3 and the vacuuming time in the step S02 are both 40-80 min. Thus, the helium and nitrogen purge time (i.e., the evacuation time) is 40-80min, preferably 1h, and the relative desorption period is short while ensuring complete helium and nitrogen purge.
The technical solutions of the present invention are further described in detail with reference to the following specific examples, which should be understood as merely illustrative and not limitative.
Example 1
A method of desorbing an adsorbent comprising the steps of:
s1, putting the zeolite molecular sieve to be desorbed into a container;
s01, introducing nitrogen into the container for purging, wherein the purging flow rate of the nitrogen is 4Nm3H, the purging time is 1.5 h;
s02, vacuumizing the container for 1h until the vacuum degree is 10 pa;
s03, heating the zeolite molecular sieve in the container to 350 ℃, wherein the heating rate is 4 ℃/min;
s04, introducing nitrogen into the container for 1h, and maintaining the pressure in the container at 0.4 Mpa;
s05, repeating the step S02;
s06, repeating the steps S04-S05;
s2, introducing helium into the container for 1h, and maintaining the pressure in the container at 0.4 Mpa;
s3, vacuumizing the container for 1h, and keeping the vacuum degree at 10 pa;
s4, repeating the steps S2-S3 for 4 times;
s5, repeating the step S2, cooling the zeolite molecular sieve in the container to room temperature, and repeating the step S3;
s6, introducing air into the container;
s61, repeating the step S3, and heating the zeolite molecular sieve in the container to 100 ℃;
s7, repeating the steps S2-S3 for 4 times, and obtaining the desorbed zeolite molecular sieve.
Example 2
A method of desorbing an adsorbent comprising the steps of:
s1, putting the zeolite molecular sieve to be desorbed into a container;
s01, introducing nitrogen into the container for purging, wherein the purging flow rate of the nitrogen is 7Nm3The purging time is 2 hours;
s02, vacuumizing the container for 1.3h until the vacuum degree is 9 pa;
s03, heating the zeolite molecular sieve in the container to 350 ℃, wherein the heating rate is 6 ℃/min;
s04, introducing nitrogen into the container for 1h, and maintaining the pressure in the container at 0.4 Mpa;
s05, repeating the step S02;
s06, repeating the steps S04-S05;
s2, introducing helium into the container for 1.3h, and maintaining the pressure in the container at 0.4 Mpa;
s3, vacuumizing the container for 1h, and keeping the vacuum degree to 9 pa;
s4, repeating the steps S2-S3 for 4 times;
s5, repeating the step S2, cooling the zeolite molecular sieve in the container to room temperature, and repeating the step S3;
s6, introducing water vapor into the container;
s61, repeating the step S3, and heating the zeolite molecular sieve in the container to 170 ℃;
s7, repeating the steps S2-S3 for 4 times, and obtaining the desorbed zeolite molecular sieve.
Example 3
A method of desorbing an adsorbent comprising the steps of:
s1, putting the zeolite molecular sieve to be desorbed into a container;
s01, introducing nitrogen into the container for purging, wherein the purging flow rate of the nitrogen is 6Nm3The purging time is 1.6 h;
s02, vacuumizing the container for 0.9h until the vacuum degree is 7 pa;
s03, heating the zeolite molecular sieve in the container to 350 ℃, wherein the heating rate is 6 ℃/min;
s04, introducing nitrogen into the container for 1h, and maintaining the pressure in the container at 0.3 Mpa;
s05, repeating the step S02;
s06, repeating the steps S04-S05;
s2, introducing helium into the container for 0.9h, and maintaining the pressure in the container at 0.3 Mpa;
s3, vacuumizing the container for 1h, and keeping the vacuum degree to be 7 pa;
s4, repeating the steps S2-S3 for 4 times;
s5, repeating the step S2, cooling the zeolite molecular sieve in the container to room temperature, and repeating the step S3;
s6, introducing water vapor into the container;
s61, repeating the step S3, and heating the zeolite molecular sieve in the container to 160 ℃;
s7, repeating the steps S2-S3 for 4 times, and obtaining the desorbed zeolite molecular sieve.
Example 4
A method of desorbing an adsorbent comprising the steps of:
s1, putting the zeolite molecular sieve to be desorbed into a container;
s01, introducing nitrogen into the container for purging, wherein the purging flow rate of the nitrogen is 3Nm3The purging time is 1 h;
s02, vacuumizing the container for 0.8h until the vacuum degree is 5 pa;
s03, heating the zeolite molecular sieve in the container to 350 ℃, wherein the heating rate is 4 ℃/min;
s04, introducing nitrogen into the container for 0.8h, and maintaining the pressure in the container at 0.2 Mpa;
s05, repeating the step S02;
s06, repeating the steps S04-S05;
s2, introducing helium into the container for 0.8h, and maintaining the pressure in the container at 0.2 Mpa;
s3, vacuumizing the container for 0.8h, and keeping the vacuum degree at 5 pa;
s4, repeating the steps S2-S3 for 4 times;
s5, repeating the step S2, cooling the zeolite molecular sieve in the container to room temperature, and repeating the step S3;
s6, introducing air into the container;
s61, repeating the step S3, and heating the zeolite molecular sieve in the container to 130 ℃;
s7, repeating the steps S2-S3 for 4 times, and obtaining the desorbed zeolite molecular sieve.
Example 5
A method of desorbing an adsorbent comprising the steps of:
s1, putting the zeolite molecular sieve to be desorbed into a container;
s01, introducing nitrogen into the container for purging, wherein the purging flow rate of the nitrogen is 8Nm3H, the purging time is 1.3 h;
s02, vacuumizing the container for 1h until the vacuum degree is 5.5 pa;
s03, heating the zeolite molecular sieve in the container to 350 ℃, wherein the heating rate is 5 ℃/min;
s04, introducing nitrogen into the container for 0.8h, and maintaining the pressure in the container at 0.25 Mpa;
s05, repeating the step S02;
s06, repeating the steps S04-S05;
s2, introducing helium into the container for 1h, and maintaining the pressure in the container at 0.25 Mpa;
s3, vacuumizing the container for 0.8h, and keeping the vacuum degree at 5.5 pa;
s4, repeating the steps S2-S3 for 4 times;
s5, repeating the step S2, cooling the zeolite molecular sieve in the container to room temperature, and repeating the step S3;
s6, introducing water vapor into the container;
s61, repeating the step S3, and heating the zeolite molecular sieve in the container to 148 ℃;
s7, repeating the steps S2-S3 for 4 times, and obtaining the desorbed zeolite molecular sieve.
The examples 1-5 were tested for performance and the specific test results are shown in table 1 below:
TABLE 1
Evaluation items of adsorbent: the adsorbent desorbed in examples 1 to 5 was again adsorbed, and specifically, CO in an active gas such as difluoromethane2And H2O, and detecting the adsorption rate of the adsorbent.
In order to ensure that the desorption effect is not influenced by the type of the adsorbent, the same adsorbent, namely the zeolite molecular sieve, is adopted as the adsorbent for desorption in the desorption method, and the desorption process and the desorption effect can be realized by using other types of adsorbents in the scheme.
The above test data of examples 1-5 show that the adsorbents obtained by the desorption method of the present embodiment have good adsorption effects on impurities, and have good adsorption effects when adsorbing gases that may react with the adsorbents.
Comparative example 1
The steps of this comparative example are the same as those of step S1 to step S4 of example 5, except that: the desorption process in this comparative example did not go through steps S5 to S7 (including step S61).
Comparative example 2
The steps of this comparative example are the same as those of step S1 to step S5 of example 5, except that: the desorption process in this comparative example was not provided with steps S6 to S7 (including step S61).
The comparative examples 1-2 were subjected to performance tests, and the specific test results are shown in the following table 2:
TABLE 2
Compared with the results of the tests in example 5 and comparative examples 1 to 2, it was shown that, when the desorption step did not pass through the steps S4 to S7, the adsorption effect on the adsorbent that may react with the adsorbent was poor, and the temperature difference before and after desorption was large, since the adsorbent having a large activity during adsorption was brought into contact with the gas that may react with the adsorbent, more impurities were generated, and the adsorption effect of the adsorbent was reduced; similarly, when the desorption of the adsorbent is completed, the temperature of the adsorbent is merely reduced, which does not solve the above problems, and the adsorbent still has a poor adsorption effect when adsorbing gas that may react with the adsorbent.
In addition, the adsorbents in comparative examples 1 and 2 are for CO2And H2The impurity removal efficiency of O is low, and the adsorber is used for adsorbing CO2And H2The temperature rise speed is high when O is generated, and through detection, other fluorocarbon impurities are generated in the adsorber, the adsorbent is blackened, and the adsorption effect is poor.
Comparative example 3
The steps in this comparative example are the same as those in example 5, except that: step S61 in this comparative example allowed the zeolite molecular sieve in the vessel to warm to 228 ℃.
Comparative example 4
The steps in this comparative example are the same as those in example 5, except that: step S61 in this comparative example allowed the zeolite molecular sieve in the vessel to warm to 85 ℃.
Comparative examples 3-4 were tested for performance and the specific test results are shown in table 3 below:
TABLE 3
From the above detection results, when different temperatures are adopted in step S61, the adsorption effect of the subsequent adsorbent is greatly affected, and in the range of 100-200 ℃ in the present embodiment, the adsorption effect of the adsorbent on the gas that may react with the adsorbent is better, but when the temperature exceeds 200 ℃ or is lower than 100 ℃, the adsorption effect is reduced during the subsequent adsorption because the desorption of the adsorbent is not complete or the adsorbent is again brought to the temperature with higher activation degree.
The above description is only a preferred embodiment of the present invention, and not intended to limit the scope of the present invention, and all modifications and equivalents of the present invention, which are made by the present specification and directly/indirectly applied to other related technical fields within the spirit of the present invention are included in the scope of the present invention.
Claims (10)
1. A method of desorbing an adsorbent, comprising the steps of:
s1, placing the adsorbent to be desorbed in a container;
s2, introducing helium into the container, and maintaining the pressure in the container at 0.2-0.4 Mpa;
s3, vacuumizing the container, and keeping the vacuum degree at 5-10 pa;
s4, repeating the steps S2-S3;
s5, repeating the step S2, cooling the adsorbent in the container to room temperature, and repeating the step S3;
s6, introducing passivation gas into the container to passivate the adsorbent;
s7, repeating the steps S2-S3 to obtain the desorbed adsorbent.
2. The method of desorbing an adsorbent according to claim 1, further comprising the steps of, between said step S1 and said step S2:
s01, introducing nitrogen into the container for purging;
s02, vacuumizing the container until the vacuum degree is 5-10 pa;
s03, heating the adsorbent in the container to a desorption temperature at which the adsorbent achieves a desorption effect;
s04, introducing nitrogen into the container, and maintaining the pressure in the container at 0.2-0.4 Mpa;
s05, repeating the step S02;
s06, repeating the steps S04-S05.
3. A method of desorbing an adsorbent as claimed in claim 1, wherein said passivation gas is air or water vapour.
4. The method of desorbing adsorbent according to claim 3, further comprising the step of, between said step S6 and said step S7: s61, repeating the step S3, and raising the temperature of the adsorbent in the container to 100-200 ℃.
5. A method of desorbing an adsorbent as claimed in claim 2, wherein said adsorbent comprises a zeolite molecular sieve or activated alumina;
in the step S03, the desorption temperature of the zeolite molecular sieve is 320-370 ℃, and the desorption temperature of the activated alumina is 220-270 ℃.
6. The method of claim 2, wherein the temperature increase rate in step S03 is 3-8 ℃/min.
7. The method for desorbing an adsorbent according to claim 2, wherein in said step S01, the purge flow rate of nitrogen is 3 to 8Nm3And h, the purging time is 1-2 h.
8. The method of claim 2, wherein the repetition of step S7 and the repetition of step S05 are ≧ 4.
9. The method of claim 2, wherein the helium gas is introduced in step S2 for 40-80min and the nitrogen gas is introduced in step S04 for 40-80 min.
10. The method of claim 2, wherein the evacuation time in step S3 and the evacuation time in step S02 are 40-80 min.
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| CN115779878A (en) * | 2022-12-09 | 2023-03-14 | 吉林大学 | Method for restoring adsorption activity of non-porous self-adaptive crystal material by pressure |
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| US20050255987A1 (en) * | 2004-05-12 | 2005-11-17 | Chevron Phillips Chemical Company Lp | Methods of activating chromium catalysts |
| CN101745288A (en) * | 2010-01-20 | 2010-06-23 | 华东理工大学 | Method for vacuum pressure and temperature varying coupling adsorbing and trapping carbon dioxide in flue gas |
| CN110420538A (en) * | 2019-08-08 | 2019-11-08 | 广东华特气体股份有限公司 | A kind of activation system and method for ultra-pure gases adsorbent |
| CN111013558A (en) * | 2019-12-31 | 2020-04-17 | 北京科技大学 | Adsorbent regeneration method based on cyclic heating mode |
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| US20050255987A1 (en) * | 2004-05-12 | 2005-11-17 | Chevron Phillips Chemical Company Lp | Methods of activating chromium catalysts |
| CN101745288A (en) * | 2010-01-20 | 2010-06-23 | 华东理工大学 | Method for vacuum pressure and temperature varying coupling adsorbing and trapping carbon dioxide in flue gas |
| CN110420538A (en) * | 2019-08-08 | 2019-11-08 | 广东华特气体股份有限公司 | A kind of activation system and method for ultra-pure gases adsorbent |
| CN111013558A (en) * | 2019-12-31 | 2020-04-17 | 北京科技大学 | Adsorbent regeneration method based on cyclic heating mode |
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| CN115779878A (en) * | 2022-12-09 | 2023-03-14 | 吉林大学 | Method for restoring adsorption activity of non-porous self-adaptive crystal material by pressure |
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