Gas purification apparatus, glovebox and regeneration method

Abstract

The application discloses a kind of gas purification device and glove box and regeneration method, comprising: air inlet pipeline;Air outlet pipeline;Adsorption column;Oxygen adsorption material layer is arranged in the adsorption column;Circulating fan;Regeneration device.The application completely changes the irreversible chemical adsorption oxygen-removing material and high temperature and hydrogen regeneration process in the prior art, but uses reversible adsorption oxygen-removing material and inert gas purging or vacuum physical method, using the reversibility of the combination of oxygen adsorption material and oxygen molecule and the mechanism affected by oxygen gas pressure, so that the oxygen molecule adsorbed by oxygen adsorption material is separated from the adsorption state, and the oxygen adsorption function of oxygen adsorption material is recovered by using inert gas purging or vacuum device.According to actual needs, (1) vacuum can be used;Or (2) normal pressure or low pressure inert gas purging;Or (3) multiple inert gas filling and vacuum way;Or (4) the above-mentioned 3 kinds of ways auxiliary heating, realize the regeneration of oxygen adsorption material.Overcome the complex and safe hidden trouble of hydrogen reduction regeneration process at about 200 DEG C currently used.

Description

TECHNICAL FIELD

[0001] The present application relates to the field of gas purification system and glove box, and particularly relates to a gas purification device, a glove box and a regeneration method. BACKGROUND

[0002] Glove box is a relatively advanced closed system, which provides a space filled with inert atmosphere isolated from air. The glove box is usually composed of two parts, a box and a gas purification system. The box is the working space, and the gas purification system is used to maintain the atmosphere in the box to meet the working requirements. The atmosphere in the box contains impurities such as oxygen, moisture and organic solvents. Organic solvents can be removed by activated carbon and other adsorbent materials, and molecular sieve and activated alumina can adsorb water. Materials containing active metals such as copper catalyst are used to remove oxygen.

[0003] The traditional glove box gas purification system contains two purification columns, also known as adsorption columns (such as Figure 5 , adsorption column 10 and adsorption column 4). The adsorption column 10 is usually filled with activated carbon, and the adsorption column 4 is usually filled with molecular sieve and copper catalyst. The gas in the box enters the adsorption column 10 of the gas circulation system under the action of the circulating fan, and the organic solvent is adsorbed by the activated carbon in the column. The gas then enters the adsorption column 4, and the moisture and oxygen in the gas are removed by the molecular sieve and copper catalyst, respectively. The gas returns to the box through the circulating fan. After the gas passes through the purification system, part of the oxygen, moisture and organic solvent impurities are removed, improving the purity of the inert gas. This purification process is continuously carried out, and the gas in the box is continuously purified, so that the gas purity is always maintained within the required range.

[0004] The principle of removing oxygen by copper catalyst is that the copper (or other active metals, but copper is commonly used) on the material reacts with oxygen to form oxides such as copper oxide (2Cu + O2 = 2CuO). The purification performance of the glove box is an important indicator of the glove box, which requires the atmosphere in the glove box to be maintained within the required range at all times.

[0005] When the impurity removal capacity of the material in the purification column is exhausted, the material needs to be replaced or regenerated after saturation. Molecular sieve and activated carbon can be replaced or regenerated. The regeneration of molecular sieve and activated carbon is relatively simple. The adsorbent is heated, and air is passed or vacuum is applied to remove the physically adsorbed water and organic solvent from the adsorbent, so that the adsorbent restores the ability to remove water and organic solvent. The copper on the copper catalyst is oxidized to copper oxide, and the regeneration is relatively complex. A reducing gas such as hydrogen is used to reduce the copper oxide to metallic copper (CuO + H2→ Cu + H2O) at about 200°C, which takes about 20 hours. During regeneration, the adsorption column cannot be used. Since hydrogen is used in the process, there is a certain risk, a high temperature is required, and the adsorption efficiency of the traditional oxygen adsorption material will decrease significantly with the increase of the number of regeneration; the traditional purification column needs to prepare two sets of adsorption columns at the same time in order to meet the uninterrupted requirements of customer experiments during regeneration, which requires more space planning and cost. SUMMARY

[0006] In view of the above-mentioned defects of the prior art, the present application provides a gas purification device and a glove box.

[0007] To achieve the above-mentioned purposes, the present application is realized by the following technical solutions:

[0008] A gas purification device comprises:

[0009] An air inlet pipeline;

[0010] An air outlet pipeline;

[0011] At least one adsorption column, the inlet of the adsorption column is connected with the outlet of the air inlet pipeline, and the outlet of the adsorption column is connected with the air outlet pipeline; a plurality of adsorption columns can be connected in series, in parallel or in series-parallel. The parallel branch is usually used as a backup, so the filling materials in the parallel adsorption columns are generally the same.

[0012] At least one of the adsorption columns is filled with oxygen adsorption material or comprehensive adsorption material;

[0013] A circulating fan, which is arranged on the air inlet pipeline or the air outlet pipeline, is used to drive the gas to enter from the air inlet pipeline, flow through the adsorption column, and then be discharged from the outlet of the air outlet pipeline;

[0014] A regeneration device, which comprises a vacuum pumping device and / or an inert gas filling device, is in communication with the adsorption column filled with oxygen adsorption material or comprehensive adsorption material.

[0015] The present application completely changes the prior art process of regeneration by using high temperature and hydrogen, and instead uses a vacuum pumping method to utilize the mechanism that the combination of oxygen adsorption material and oxygen molecules is affected by air pressure, so that the oxygen molecules adsorbed by the oxygen adsorption material are separated from the adsorption state and are pumped away by the vacuum pumping device, thereby realizing the recovery of the oxygen adsorption function of the oxygen adsorption material. According to actual needs, multiple vacuum pumping methods, or multiple inert gas filling and vacuum pumping methods, or auxiliary inert gas or heating vacuum pumping methods can be used to realize the regeneration of the oxygen adsorption material or the comprehensive adsorption material. The current complex and potentially dangerous hydrogen reduction regeneration process at about 200 DEG C is overcome.

[0016] Further, the regeneration device further comprises an adsorption column heating device for heating the oxygen adsorption material layer or the comprehensive adsorption material layer in the adsorption column.

[0017] Further, the heating device comprises a heating element arranged inside or outside the adsorption column.

[0018] Further, the heating element comprises one or a combination of an electric heating element, a liquid medium or a gaseous medium heating pipeline.

[0019] Further, the heating device further comprises a temperature control device, and the temperature T1 is controlled at 30-150 DEG C, preferably 50-100 DEG C.

[0020] Further, the adsorption column is one, a third valve is arranged on the inlet side of the adsorption column, the gas purification device is further provided with a bypass pipeline, the inlet of the bypass pipeline is connected to the air inlet pipeline before the third valve, and the outlet is connected to the inlet end of a circulating fan, the circulating fan is arranged on the pipeline between the second valve and the outlet of the air outlet pipeline, and a fourth valve is arranged on the bypass pipeline.

[0021] Further, the pipeline of the vacuum pumping device is connected to the pipeline between the third valve or the second valve and the adsorption column.

[0022] Further, the adsorption column is two or more in parallel, and the inlet side and the outlet side of each adsorption column are provided with valves, and the upper end and the lower end of each adsorption column filled with oxygen adsorption material or the upper end and the lower end of each adsorption column filled with comprehensive adsorption material are respectively connected to the inert gas filling device and the pipeline of the vacuum pumping device.

[0023] Further, the oxygen adsorption material in the oxygen adsorption material layer or the comprehensive adsorption material layer is in the form of cylindrical, spherical particles, or honeycomb columnar structure.

[0024] The present application also discloses a glove box comprising a glove box body, and further comprising the above-mentioned gas purification device for purifying the gas atmosphere in the glove box body.

[0025] The present application also provides a regeneration method of an oxygen adsorption material. When the oxygen adsorption material is over-adsorbed with oxygen molecules and needs to be regenerated, the reversible oxygen adsorption material is regenerated by vacuumizing, or by blowing inert gas at normal pressure or low pressure, or by repeatedly filling inert gas and vacuumizing. BRIEF DESCRIPTION OF DRAWINGS

[0026] In order to more clearly illustrate the technical solutions in the embodiments of the present application or the prior art, the following will briefly introduce the drawings needed to be used in the embodiments or the prior art description. Obviously, the drawings in the following description are only some embodiments of the present application, and other drawings can be obtained by those skilled in the art without any creative effort on the basis of these drawings.

[0027] Figures 1-4 The figures are schematic diagrams of four different embodiments of the gas purification device and glove box of the present application.

[0028] Figure 5 The figure is a schematic diagram of the prior art.

[0029] The numbers in the figures represent respectively:

[0030] Glove box body 1; air inlet pipeline 2; air outlet pipeline 3; second valve 31; adsorption column 4 and 8; circulating fan 5; third valve 22; bypass pipeline 7; fourth valve 71; vacuum pipeline valves 61 and 62

[0031] Vacuumizing device 6; valves 81 and 82 on both sides of adsorption column 8; nitrogen valve 91; second nitrogen valve 92; nitrogen cylinder 9; adsorption column 10; adsorption column inlet and outlet valves 11 and 12. DETAILED DESCRIPTION

[0032] In order to make the objectives, technical solutions and advantages of the embodiments of the present application clearer, the following will clearly and completely describe the technical solutions in the embodiments of the present application with reference to the drawings in the embodiments of the present application. Obviously, the described embodiments are only some of the embodiments of the present application, but not all the embodiments. Based on the embodiments in the present application, all other embodiments obtained by those skilled in the art without any creative effort fall within the protection scope of the present application.

[0033] The present application will be further described below with reference to the embodiments.

[0034] A gas purification device, comprising:

[0035] Air inlet pipeline 2;

[0036] an air outlet pipeline 3 provided with a second valve 31;

[0037] an adsorption column 4, an inlet of which is connected with an outlet of the air inlet pipeline 2, and an outlet of which is connected with the air outlet pipeline 3; the adsorption column 4 is provided with an oxygen adsorption material layer; or simultaneously provided with an active carbon layer, a molecular sieve layer and an oxygen adsorption material layer, or provided with a comprehensive adsorption layer made of active carbon material, molecular sieve material and oxygen adsorption material mixed and granulated; a plurality of adsorption columns can form a series connection, parallel connection or series-parallel connection structure, and the parallel connection branch is usually used as a backup, so that the internal filling materials of the adsorption columns in parallel connection are generally the same.

[0038] a circulating fan 5 provided on the air inlet pipeline 2 or the air outlet pipeline 3, for driving the gas to enter from the air inlet pipeline 2, flow through the adsorption column 4, and then be discharged from the outlet of the air outlet pipeline 3; generally, as shown in the examples of Figure 1 and Figure 2 , the circulating fan 5 is provided on the air outlet pipeline 3.

[0039] a regeneration device including a vacuumizing device 6 in communication with the adsorption column 4.

[0040] In the prior art, a process of regeneration by using high temperature of about 200 DEG C and hydrogen gas is used, and the equipment is complex and the use of hydrogen gas has a high risk. The present application completely changes the process of regeneration by using irreversible chemical adsorption oxygen-removing material and high temperature and hydrogen gas in the prior art, and instead uses reversible adsorption oxygen-removing material and inert gas purging or vacuumizing physical method, utilizes the reversibility of the combination of oxygen adsorption material and oxygen molecules and the mechanism affected by oxygen gas pressure, so that the oxygen molecules adsorbed by the oxygen adsorption material are separated from the adsorption state, and the oxygen adsorption function of the oxygen adsorption material or the comprehensive adsorption material is recovered by using the inert gas purging or vacuumizing device. According to actual needs, (1) the vacuumizing method can be used; or (2) the normal pressure or low pressure inert gas purging method; or (3) the method of multiple inert gas filling and vacuumizing; or (4) the above-mentioned three methods assisted by heating, so as to realize the regeneration of the oxygen adsorption material. The process of reduction regeneration by using the complex and safe hydrogen gas at about 200 DEG C at present is overcome.

[0041] In some embodiments, in order to shorten the time consumed by the regeneration of the oxygen adsorption material, the regeneration device further includes an adsorption column heating device for heating the oxygen adsorption material layer or the comprehensive adsorption material layer in the adsorption column 4. The adsorption force of the oxygen adsorption material to oxygen is mainly affected by the gas pressure, and the lower the oxygen gas pressure, the weaker the oxygen adsorption force, and the oxygen gas is separated from the adsorption state and is sucked away by the vacuumizing device. Meanwhile, the adsorption force is also affected by the temperature, and the higher the temperature, the weaker the adsorption force, so that the separation of the oxygen gas can be accelerated by adjusting the temperature, and the heating temperature is generally set between 50 DEG C and 100 DEG C.

[0042] In practical applications, the heating device comprises a heating element arranged inside or outside the adsorption column.

[0043] The heating element can be one or a combination of electric heating element, liquid medium or gaseous medium heating pipeline.

[0044] In practical applications, the heating device further comprises a temperature control device, and the temperature T1 is controlled at 30-150°C, preferably in the temperature range of 50-100°C. The temperature can be conveniently controlled as required.

[0045] In the example shown in Figure 1 , the adsorption column 4 is one, the third valve 22 is arranged on the inlet side of the adsorption column 4, the gas purification device further comprises a bypass pipeline 7, the inlet of the bypass pipeline 7 is connected to the air inlet pipeline 2 before the third valve 22, and the outlet is connected to the inlet end of the circulating fan 5. The circulating fan 5 is arranged on the pipeline between the second valve 31 and the outlet of the air outlet pipeline 3. The fourth valve 71 is arranged on the bypass pipeline 7. The bypass pipeline 7 is arranged because some glove boxes or other devices using other purification devices cannot allow the circulating fan 5 to stop during operation. Therefore, when the adsorption column 4 is saturated, only the operation can be stopped, and the regeneration device is used to complete the regeneration of the oxygen adsorption material in the adsorption column 4, and then the device is restarted for operation. In order to not stop the circulating fan and the device during the regeneration of the adsorption column 4, the bypass pipeline 7 and the fourth valve 71 are arranged. During normal operation, the fourth valve 71 is closed, and the bypass pipeline 7 does not work. When the oxygen adsorption material needs to be regenerated, the fourth valve 71 is opened, and then the second valve 31 and the third valve 22 are closed. At this time, the circulating fan 5 can continue to circulate the gas in the device through the bypass pipeline 7 without stopping. Then the vacuum pipeline valve 61 on the vacuum pipeline is opened, and the vacuum device 6 is opened to perform vacuumization on the adsorption column 4, so as to regenerate the oxygen adsorption capacity of the oxygen adsorption material.

[0046] In some embodiments, the bypass pipeline 7 and the fourth valve 71 are not necessary devices. In the gas purification device provided with the bypass pipeline 7, one or more adsorption columns are generally arranged on the air inlet pipeline 2 before the third valve 22. In this way, when the regeneration operation of the adsorption column 4 is performed, the adsorption column 4 is cut off by the bypass pipeline 7, and the remaining adsorption columns can continue to work.

[0047] The pipeline of the vacuum device 6 is connected to the pipeline between the third valve 22 or the second valve 31 and the adsorption column 4. In the example shown in Figure 1 , the pipeline of the vacuum device 6 is connected to the pipeline between the second valve 31 and the adsorption column 4. The pipeline of the vacuum device 6 can be generally connected to the tank on the outlet side of the adsorption column or the outlet pipeline.

[0048] In some embodiments, an inert gas filling device, such as a high purity nitrogen filling device, can be connected between the third valve 22 and the adsorption column 4, including a pipe and a nitrogen valve 91. When performing vacuum regeneration, the second valve 31 and the third valve 22 are closed, the vacuum pipe valve 61 is opened for vacuuming, and the nitrogen valve 91 is opened, so that the adsorption column 4 is filled with high purity nitrogen from the nitrogen tank or cylinder 9, and the process is repeated several times until the oxygen adsorption capacity of the oxygen adsorption material is regenerated. Generally, the vacuum device 6 is connected below the oxygen adsorption material layer, and the inert gas filling device is connected above the oxygen adsorption material layer. For example, the vacuum device 6 is connected below the adsorption column 4, and the inert gas filling device is connected to the upper end cover of the adsorption column. In this way, the inert gas injected by the inert gas filling device passes through the oxygen adsorption material from top to bottom, and the oxygen is blown off from the adsorption state. The vacuum device below the oxygen adsorption material can enhance the blowing effect, and at the same time, due to the decrease of oxygen gas pressure, the oxygen in the adsorption state is removed. The oxygen gas pressure refers to, for example, when the gas pressure in the adsorption column is 1 atmosphere, and the oxygen concentration is 1%, the corresponding oxygen gas pressure is 1% of the atmospheric pressure, so the oxygen gas pressure represents both the oxygen concentration and the gas pressure. The inert gas filling device is generally connected to the tank on the inlet side of the adsorption column, or connected to the pipe on the inlet side of the adsorption column.

[0049] In other embodiments, the adsorption column is two or more in parallel, such as Figure 2 As shown in the figure, two adsorption columns (4 and 8 respectively) are provided, and each adsorption column is provided with a valve on the inlet side and the outlet side, Figure 2 In the example shown in the figure, the valves on the two sides of the adsorption column 4 are 22 and 31 respectively, and the valves on the two sides of the adsorption column 8 are 81 and 82 respectively. A vacuum pipe is provided between the outlet of each adsorption column and the outlet side valve, and the vacuum pipe is connected to the vacuum device through a valve. Figure 2 In the example shown in the figure, the adsorption column 4 and the adsorption column 8 are connected to the vacuum device through the vacuum pipes and the valves 61 and 62 on the corresponding pipes. Figure 2 In the example shown in the figure, two adsorption columns can be used, one for work and one for standby. When regeneration is needed, the standby adsorption column is activated. Two or more adsorption columns can also be used simultaneously, but when regeneration is needed, only one or part of the adsorption columns are used for regeneration, and the remaining adsorption columns continue to work until all the adsorption columns have completed the regeneration.

[0050] In some embodiments, the inert gas filling device adopts a high-purity nitrogen filling device, including a pipeline and nitrogen valves 91 and 92, the nitrogen valve 91 and the corresponding pipeline are connected between the third valve 22 and the adsorption column 4, and the second nitrogen valve 92 and the pipeline are connected between the valve 81 and the adsorption column 8. When the adsorption column 4 is regenerated by vacuumizing, the second valve 31 and the third valve 22 are closed, the vacuum pipeline valve 61 is opened for vacuumizing, and the nitrogen valve 91 is opened at the same time, so that the adsorption column 4 is filled with high-purity nitrogen from the nitrogen tank or cylinder 9, and the process is repeated several times until the regeneration of the oxygen adsorption capacity of the oxygen adsorption material is achieved. When the adsorption column 8 is regenerated by vacuumizing, the valve 81 and the valve 82 are closed, the vacuum pipeline valve 62 is opened for vacuumizing, and the second nitrogen valve 92 is opened at the same time, so that the adsorption column 8 is filled with high-purity nitrogen from the nitrogen tank or cylinder 9, and the process is repeated several times until the regeneration of the oxygen adsorption capacity of the oxygen adsorption material is achieved.

[0051] In some embodiments, as shown in Figure 3 , an adsorption column 10 and inlet valves 11 and 12 of the adsorption column 10 are additionally arranged before the adsorption column 4, and the bypass valve 72 of the adsorption column 10 is connected outside the inlet valves 11 and 12. The additional adsorption column 10 can be filled with a moisture adsorption material such as a molecular sieve material alone, or can be additionally filled with one or more layers of activated carbon to adsorb organic components. Then, the adsorption column 4 can be filled with a single oxygen adsorption material for adsorbing oxygen. Of course, the adsorption column 4 can also be filled with a multifunctional adsorption material mixed with a molecular sieve and activated carbon. The regeneration of the activated carbon and the molecular sieve in the adsorption column 10 requires the use of a high-temperature regeneration device, and the heating device in the adsorption column 10 can be used. Figure 3 The bypass pipeline 7 and the bypass valves 71 and 72 arranged in the bypass pipeline 7 can cut off the adsorption column 10 or the adsorption column 4 by opening and closing the two bypass valves, so that the cut-off adsorption column can be regenerated. Therefore, the adsorption columns 10 and 4 can be alternately regenerated through the bypass pipeline.

[0052] Similarly, as shown in Figure 4 , in the system with the backup adsorption column 10, the adsorption column 4 and the adsorption column 8 can also be additionally provided with the adsorption column 10, and the internal material and principle of the adsorption column 10 are the same as those of the example in Figure 3 , and will not be described again.

[0053] Further, the adsorption material in the oxygen adsorption material layer or the comprehensive adsorption material layer is a plurality of cylindrical particle structures. Of course, it is not limited to the cylindrical particle structure, and can also be spherical, hollow beads with holes, cylindrical with honeycomb holes or other cubic structures. These particles are stacked in the adsorption column to form the oxygen adsorption material layer or the comprehensive adsorption material layer, and the gaps between the particles form the passage for the gas to flow through.

[0054] The oxygen adsorption material or comprehensive adsorption material used in the present application is prepared by the present application applicant, and the preparation method of the oxygen adsorption material or comprehensive adsorption material is original to the present application applicant, and the preparation method is as follows:

[0055] Step one, first, the ligand material is prepared:

[0056] A 3L reaction container is connected with a reflux condensing device, a constant pressure dropping device, a temperature control device and a heating stirring device, after vacuum replacement, inert gas is filled, 2 mol of 2.4-pentanedione, 3 mol of acetic anhydride and 2.4 mol of ethyl acetoacetate are added into the reaction container, the adding ratio of the three is 1:1.5:1.2, the reaction is carried out under the protection of inert gas, the stirring speed is 300 rpm, the temperature of the mixed solution is controlled at 90 DEG C, after the mixed reaction solution is refluxed at the temperature control point for 2 h, the heating is turned off, and the temperature is lowered to room temperature under the protection of inert gas;

[0057] The reaction container is connected with a reduced pressure distillation device, the airtightness of the device system is checked, and the airtightness is ensured to be good, then the condensing stirring device is started, the stirring speed is 300 rpm, the vacuum inlet device system is slowly connected at room temperature, the vacuum degree is adjusted to 30 KPa, the boiling degree of the mixed solution is controlled by adjusting the vacuum degree, after the liquid drops no longer drop, the vacuum degree is increased to 15 KPa, then the temperature of the solution is slowly increased to 60 DEG C, the by-product in the mixture is gradually extracted, and the by-product receiving container is collected, until no liquid drops are dropped, the device system is restored to normal pressure;

[0058] The above by-product receiving container is replaced with a target intermediate product receiving container, the vacuum degree is adjusted to 10 KPa, the reaction mixture is gradually heated to 100 DEG C, the solution starts to boil, liquid drops are dropped in the target intermediate product receiving container, the temperature of the solution is finally increased to 115 DEG C, the collection of the target intermediate product is carried out, the target intermediate product is weighed, and the yield is 73%.

[0059] The above target intermediate product is reacted with ethylenediamine and methanol under stirring, the proportion of the reactants is 2:1:6, after the reaction, the target product, i.e. the oxygen adsorption material ligand, is obtained by filtering and drying, and the yield is 90%.

[0060] Step two, preparation of the oxygen adsorption material:

[0061] Preparation of raw materials: cobalt acetate, ligand prepared in step one, isopropyl alcohol, potassium hydroxide and methylpyridine;

[0062] Step 1: Into a 250ml beaker, add 0.1mol cobalt acetate, 0.1mol ligand, add isopropyl alcohol reagent, control the reagent concentration at 4mol.L-1, under heating condition (control the temperature at 50-60℃), start stirring, set the stirring rate at 400R / min, to obtain mixed solution 1. Into another 250ml conical flask, add 0.1mol potassium hydroxide, add isopropyl alcohol reagent, control the concentration at 4mol.L-1, heat and stir at 60℃ until the solid is completely dissolved to obtain mixed solution 2. Under the heating and stirring condition of mixed solution 1, add mixed solution 2 into mixed solution 1, control the adding time at 30min. Stop the reaction after holding the temperature for 4h. Filter the reaction solution to obtain red-brown solid product COL, with a yield of 95%.

[0063] Step 2: Into a 250ml beaker, add 0.15mol product COL, 0.12mol potassium hydroxide, 0.14mol methylpyridine, solvent methyl isopropyl alcohol, control the reagent concentration at 4mol.L-1, start the experiment under heating and stirring condition, set the stirring rate at 300R / min, slowly heat to 75-85℃. Stop the reaction after holding the temperature for 6h.

[0064] Reaction solution treatment: filter the above reaction solution by vacuum pump, dry the obtained product, with a yield of 97%. The product is used as oxygen absorbing material, with an oxygen absorption rate of 6.02%. The oxygen absorption rate refers to the percentage of oxygen adsorption mass to the mass of oxygen absorbing material.

[0065] The target product is subjected to cyclic oxygen absorption test, in the way of oxygen purging→nitrogen purging→oxygen purging again→nitrogen purging again, continuously absorbing and desorbing oxygen for 6 times. After purging with nitrogen, the oxygen absorbing material of the application can be desorbed to the original state and cyclically absorb oxygen. By means of gas purging, the oxygen absorbing material can continuously cyclically absorb oxygen, and the oxygen absorption rate remains 6% after several cycles, which remains unchanged. It is proved that the oxygen absorbing material of the application has high oxygen absorption rate, can be continuously used, and is easy and fast to operate, energy-saving and environment-friendly.

[0066] The application further discloses a glove box, as shown in Figure 1 and Figure 2 which comprises a glove box body 1 and the above-mentioned gas purifying device for purifying the gas atmosphere in the glove box body.

[0067] For example, as shown in Figure 1 the glove box body 1 is a single-station glove box body, with a length of 1200mm, a depth of 750mm and a height of 900mm.

[0068] The adsorption column 4 is one or two, the size is ID 200mm, the height is 200mm, the adsorption column 4 has a heating pipe, the column has two KF40 flanges on the top, connects two KF40 angle valves, one is the third valve 22 for circulating the inlet air, and the other is the second valve 31 for circulating the outlet air. In addition, the adsorption column 4 is also provided with a gas supplement pipeline and a gas supplement valve. The column is filled with 6kg of molecular sieve and 800g of new adsorption material.

[0069] In the initial operation, air is injected into the glove box, the fourth valve 71 and the circulating fan are opened, and the oxygen concentration is stable.

[0070] Then the second valve 31 and the third valve 22 are opened, the fourth valve 71 is closed, and the oxygen concentration is reduced from 1030PPM to 218PPM after circulating for 20 minutes.

[0071] The fourth valve 71 is opened again, the second valve 31 and the third valve 22 are closed, the adsorption column 4 is heated to about 70 degrees, and the adsorption column 4 is filled with pure nitrogen after being vacuumized for 60 minutes.

[0072] The second valve 31 and the third valve 22 are opened, the fourth valve 71 is closed, and the oxygen concentration is reduced from 218PPM to 8PPM after circulating for 300 minutes.

[0073] The fourth valve 71 is opened again, the second valve 31 and the third valve 22 are closed, the adsorption column 4 is heated to about 70 degrees, and the adsorption column 4 is filled with pure nitrogen after being vacuumized for 60 minutes.

[0074] The second valve 31 and the third valve 22 are opened, the fourth valve 71 is closed, and the oxygen concentration is reduced from 8PPM to less than 1PPM after circulating for 200 minutes. After the atmosphere in the glove box meets the requirements, the glove box can start to work. When the oxygen in the adsorption column 4 is saturated, the oxygen adsorption capacity of the oxygen adsorption material needs to be regenerated as described above.

[0075] The application also provides a regeneration method of oxygen adsorption material. When the oxygen molecules attached to the oxygen adsorption material are too much and cannot meet the requirements, the oxygen adsorption material is regenerated by using the reversibility of the combination of the oxygen adsorption material and the oxygen molecules and the mechanism of being affected by the oxygen gas pressure, using the vacuumization mode, or the normal pressure or low pressure inert gas purging mode, or the combination of multiple inert gas filling and vacuumization modes.

[0076] On the basis of the above three methods, the efficiency of the regeneration can be further improved by heating the oxygen adsorption material, which is described in the foregoing embodiments, and will not be repeated here.

[0077] The above examples are only used to illustrate the technical solutions of the present application, and are not intended to limit the present application; although the present application has been described in detail with reference to the foregoing examples, those skilled in the art should understand that the technical solutions recorded in the foregoing examples can be modified, or some technical features can be replaced by equivalent features; and these modifications or replacements will not cause the essence of the corresponding technical solutions to deviate from the spirit and scope of the technical solutions of the embodiments of the present application.

Claims

1. A gas purification apparatus, characterized by, The gas purification device comprises: an inlet pipe; an outlet pipe; at least one adsorption column, the inlet of which is connected to the outlet of the inlet pipe, and the outlet of which is connected to the outlet pipe; wherein the at least one adsorption column is filled with reversible oxygen adsorption material or comprehensive adsorption material containing reversible oxygen adsorption material; a circulating fan, which is arranged on the inlet pipe or the outlet pipe, and is used to drive the gas to enter from the inlet pipe, flow through the adsorption column, and then be discharged from the outlet of the outlet pipe; a regeneration device, which comprises a vacuum pumping device and / or an inert gas filling device, and is in communication with the adsorption column filled with the oxygen adsorption material or the comprehensive adsorption material; the regeneration device is used to restore the oxygen adsorption function of the reversible oxygen adsorption material by physical regeneration, and comprises any one of the following operations: (a) vacuum pumping to separate the adsorbed oxygen molecules; (b) inert gas purging at normal pressure or low pressure; (c) multiple inert gas filling combined with vacuum pumping.

2. The gas purification device according to claim 1, characterized in that, The regeneration device further comprises an adsorption column heating device used to heat the oxygen adsorption material layer or the comprehensive adsorption material layer in the adsorption column.

3. The gas purification device of claim 2, wherein, The heating device comprises a heating element arranged inside or outside the adsorption column.

4. The gas purification device of claim 3, wherein The heating element comprises one or more combinations of an electric heating element, a liquid medium, or a gaseous medium heating pipeline.

5. The gas purification device of claim 2, wherein, The heating device further comprises a temperature control device, and the temperature T1 is controlled at 30-150°C.

6. The gas purification device of claim 5, wherein, The adsorption column is one, the inlet side of the adsorption column is provided with a third valve, the gas purification device is further provided with a bypass pipeline, the inlet of the bypass pipeline is connected to the inlet pipe before the third valve, and the outlet is connected to the inlet end of the circulating fan, the circulating fan is arranged on the pipeline between the second valve and the outlet of the outlet pipe, and the bypass pipeline is provided with a fourth valve.

7. The gas purification device of claim 6, wherein, The pipeline of the vacuum pumping device is connected to the pipeline between the third valve or the second valve and the adsorption column.

8. The gas purification device of claim 5, wherein, The adsorption columns are two or more in parallel, the inlet side and the outlet side of each adsorption column are provided with valves, and the upper end and the lower end of each adsorption column filled with the oxygen adsorption material or the comprehensive adsorption material are respectively connected to the pipeline of the inert gas filling device and the vacuum pumping device.

9. A gas purification device according to any one of claims 1-8, characterized in that The oxygen adsorption material in the oxygen adsorption material layer or the comprehensive adsorption layer is in the form of a cylindrical particle structure, a spherical particle structure, or a honeycomb columnar structure.

10. The gas purification device of claim 5, wherein, The heating device further comprises a temperature control device, and the temperature T1 is preferably 50-100°C.

11. A glove box comprising a glove box housing, characterized in that The gas purification device of any one of claims 1-10 is further included.

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