CN211384418U - Device for recovering special gas adsorbed by molecular sieve - Google Patents
Device for recovering special gas adsorbed by molecular sieve Download PDFInfo
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- CN211384418U CN211384418U CN201921748658.5U CN201921748658U CN211384418U CN 211384418 U CN211384418 U CN 211384418U CN 201921748658 U CN201921748658 U CN 201921748658U CN 211384418 U CN211384418 U CN 211384418U
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Abstract
The utility model discloses a device for recovering special gas absorbed by a molecular sieve, which comprises a first gas conveying pipeline, a second gas conveying pipeline and a condenser; the first gas conveying pipeline is used for blowing non-impurity gas into the molecular sieve adsorption column adsorbed with the special gas so as to desorb the special gas on the molecular sieve; the second gas conveying pipeline is used for conveying the mixed gas desorbed from the molecular sieve adsorption column to the condenser; the condenser is used for condensing the special gas in the mixed gas to separate the special gas from the non-impurity gas; the special gas is arsine, phosphine or germane. The utility model discloses a hydrogen or helium are non-impurity gas, make the desorption of the special gas on the molecular sieve under the normal atmospheric temperature, and then the condensation is retrieved, makes its and non-impurity gas separation, and the recovery cost is low, easy to operate, the environmental protection, and the rate of recovery is high, has compensatied the technical defect of trade, has reduced the purification cost of special gas.
Description
Technical Field
The utility model relates to a special gas retrieves technical field, especially relates to a retrieve adsorbed special gas's of molecular sieve device.
Background
In the field of high-purity special gases, such as arsine, phosphine, germane and the like, molecular sieves, such as 3A, 4A, 5A, 13X and the like, are generally used for removing impurities, such as moisture and the like, in the special gases. The purification by using the molecular sieve has the advantages of high efficiency, capability of deeply removing water and other small molecular impurities, capability of being heated and recycled and the like, thereby being widely applied to the purification of various gases.
However, molecular sieves adsorb impurities and also adsorb a large amount of specialty gases. For example, arsine passes through an adsorption column with the volume of 100L filled with 4A molecular sieve, and the 4A molecular sieve can adsorb 20-30 kg of arsine while adsorbing water. Arsine can be decomposed at 230 ℃, and if the molecular sieve is directly activated, arsine can be directly lost and the molecular sieve is easily deactivated. If the molecular sieve is directly pumped out for replacing and then activated, the molecular sieve adsorbing the arsine enters a tail gas absorption spray tower, so that a large amount of oxidant is consumed, and the arsine in the molecular sieve cannot be recovered. It can be seen that activation of a 100L molecular sieve column results in loss of tens of thousands of yuan. Especially for germane, which is a special gas with high price, the market price per kg is as high as tens of thousands yuan, and more than ten thousands yuan can be lost when the molecular sieve is activated once. In actual industrial production, the molecular sieve needs to be activated once for treating 100-200 kg of special gas, and the special gas adsorbed in the molecular sieve cannot be recovered, so that the cost of an enterprise is increased by more than 10%.
Therefore, the development of equipment for efficiently recovering the special gas adsorbed in the molecular sieve has very important significance.
SUMMERY OF THE UTILITY MODEL
In order to solve the disadvantages and deficiencies existing in the prior art, a first object of the present invention is to provide a method for recovering a special gas adsorbed by a molecular sieve, and a second object of the present invention is to provide a device for recovering a special gas adsorbed by a molecular sieve. The utility model discloses a method and device are supporting to be used, can high-efficiently retrieve the adsorbed special gas in the molecular sieve, and the rate of recovery is up to more than 90%, is showing the loss that has reduced the purification of special gas, has reduced the purification cost of special gas.
For realizing the purpose, the utility model adopts the following technical scheme:
the utility model provides a pair of retrieve method of adsorbed special gas of molecular sieve, it includes following step:
(1) blowing non-impurity gas to the molecular sieve adsorbed with the special gas to desorb the special gas on the molecular sieve to obtain mixed gas containing the non-impurity gas and the special gas;
(2) condensing the special gas in the mixed gas to separate the special gas from the non-impurity gas;
(3) and (3) recovering the special gas condensed in the step (2).
Preferably, the non-impurity gas includes at least one of hydrogen and helium. Most preferably, the non-contaminant gas is hydrogen. The hydrogen has small molecular radius, high molecular motion speed and excellent diffusivity, can continuously invade gaps of the molecular sieve and continuously impact special gas molecules adsorbed on the molecular sieve to break loose the adsorption effect of the molecular sieve, and further desorb. In addition, hydrogen is inexpensive.
Preferably, the specialty gas comprises at least one of arsine, phosphine, and germane.
Preferably, the blowing manner of the non-impurity gas is continuous blowing, and the blowing direction is blowing from bottom to top. The continuous blowing can make the non-impurity gas continuously impact the special gas molecules in the molecular sieve to make the special gas molecules quickly desorbed. Blowing from bottom to top can make the non-impurity gas flow along the natural flow direction of the gas, fully invade into the molecular sieve and make the special gas in the molecular sieve desorb.
Preferably, the flow rate of the non-impurity gas is 60-100L/min, and the blowing time is 8-12 h. Preferably, the flow rate of the non-impurity gas is 60L/min. Because the recovery rate of the special gas is obviously improved along with the increase of the flow rate of the non-impurity gas, but the recovery rate of the special gas is not obviously improved when the flow rate reaches above 60L/min, the invention takes 60L/min as the optimal flow rate of the non-impurity gas, the recovery cost of the flow rate is lower, and the purity of the recovered special gas is higher.
Preferably, the temperature of the special gas condensed and recovered in the step (2) is below-170 ℃, and the adopted condensing medium is liquid nitrogen, liquid argon, liquid helium or other refrigerants capable of providing a cooling environment below-170 ℃ and the like. Because the melting point of the special gas is about-100 to-170 ℃, the gaseous special gas is condensed and converted into liquid or solid at the temperature below-170 ℃, and the hydrogen is still gaseous at the temperature, so that the special gas and the hydrogen can be easily separated. Most preferably, said step (2) condenses the specialty gas at the temperature of liquid nitrogen. The temperature of the liquid nitrogen is-196 ℃, the condensing efficiency to the special gas is higher, and the price of the liquid nitrogen is cheaper.
Preferably, in the step (3), when the condensed special gas is recovered, the special gas is firstly converted into a gaseous state and then directly filled into a gas cylinder so as to directly recover the special gas. Compared with the method for directly recovering the special gas by only recovering the key elements such as germanium, arsenic and phosphorus in the special gas, the method for directly recovering the special gas is more efficient and has higher recovery rate.
The above recovery method of the utility model adopts hydrogen or helium as carrier gas, brings out the special gas from the molecular sieve built-in without heating. Under the continuous flushing of the carrier gas flow, the desorbed special gas is mixed in the carrier gas flow to form mixed gas. Under the condensation condition of the invention, the special gas in the mixed gas is converted into liquid or solid state, but the non-impurity gas is still gaseous, so that the special gas is separated from the non-impurity gas. Finally, the discharged non-impurity gas can be returned to the initial process by a gas circulator, and the non-impurity gas can be used as carrier gas to flow into the molecular sieve adsorbed with special gas, or can be recycled for standby by a gas cylinder or other equipment. After the blowing is finished, the condensed special gas is converted into a gas state again and then directly recovered into the gas cylinder.
The utility model discloses a method that this kind of adoption non-impurity gas flows and makes special gas and molecular sieve desorption is different with the principle of heating molecular sieve desorption. The recovery method of the invention does not need heating, can desorb the special gas from the molecular sieve at normal temperature, and the water has great polarity and can not be desorbed from the molecular sieve. However, in the method for heating the molecular sieve to realize desorption, the special gas is decomposed or converted during heating, a large amount of moisture adsorbed in the molecular sieve is brought out in the heating process, and the molecular sieve plays a role in removing water in the field of the special gas. Therefore, if the special gas adsorbed by the molecular sieve is recovered by a method of heating the molecular sieve, the moisture desorbed by heating needs to be removed by the molecular sieve, and the special gas can be trapped in a dead cycle. Therefore, in the actual production process of the industry at present, the special gas adsorbed by the molecular sieve cannot be directly recovered, the molecular sieve adsorbed with the special gas can only be heated and activated to desorb the special gas, the special gas is mostly toxic, and finally KMnO needs to be sprayed by a tail gas purification system4And the key elements (such as germanium, arsenic and phosphorus) in the special gas are recovered by heating and oxidizing the absorbent or the incinerator. The existing recovery method has low economic benefit and higher recovery cost. Therefore, the recovery method has the advantages of low cost, easy operation, environmental protection, high efficiency, direct recovery of special gas, considerable economic benefit and the like, and makes up for the technical defects of the prior industry.
The utility model provides a device for recovering special gas adsorbed by a molecular sieve, which comprises a first gas conveying pipeline, a second gas conveying pipeline and a condenser; the first gas conveying pipeline is used for blowing non-impurity gas into the molecular sieve adsorption column which adsorbs the special gas so as to desorb the special gas in the molecular sieve adsorption column; the second gas conveying pipeline is used for conveying the mixed gas desorbed from the molecular sieve adsorption column to the condenser; the condenser is used for condensing the special gas in the mixed gas to separate the special gas from the non-impurity gas. Here, the definition and preference of the special gas, non-impurity gas and molecular sieve are the same as those of the above recovery method of the present invention, and will not be described in detail.
Preferably, the first gas conveying pipeline is connected with an interface at the bottom of the molecular sieve adsorption column, one end of the second gas conveying pipeline is connected with an interface at the top of the molecular sieve adsorption column, and the other end of the second gas conveying pipeline is connected with the condenser. Therefore, the hydrogen flow or the helium flow can flow from bottom to top in the molecular sieve adsorption column, has the same direction as the natural flow, and can reach higher flow rate under lower blowing pressure, thereby being better immersed in the gaps of the molecular sieve to impact the special gas, and leading the special gas to be easier to desorb.
Preferably, the condenser is a shell-side condenser, the mixed gas flows through a shell side of the condenser, a condensing medium is filled in the condenser, and the second gas conveying pipeline is connected with a shell side gas inlet of the condenser. The mixed gas in the shell-side condenser is the shell-side, and the condensing medium in the shell-side condenser is the shell-side.
Preferably, the device further comprises a condensing medium conveying pipeline, a third gas conveying pipeline, a gas circulator and a gas cylinder; the condensing medium conveying pipeline is used for conveying condensing medium into the tubes of the condenser; the third gas conveying pipeline and the gas cylinder are respectively connected with a shell pass gas outlet of the condenser, the third gas conveying pipeline is used for discharging non-impurity gas separated by the condenser, the third gas conveying pipeline is further connected with the gas circulator, and the gas circulator is further connected with the first gas conveying pipeline, so that the non-impurity gas separated by the condenser can be reused as carrier gas, and is re-conveyed back to the first gas conveying pipeline through the gas circulator to be blown into the molecular sieve adsorption column. The gas cylinder is used for recovering the special gas condensed by the condenser. And after the blowing is finished, closing the first gas conveying pipeline, the second conveying pipeline, the condensing medium conveying pipeline and the third gas conveying pipeline, and performing auxiliary heating on the condenser to ensure that the condensed special gas is directly recovered by the gas cylinder after being converted into a gas state again. Preferably, the condensation temperature of the condenser is below-170 ℃, the adopted condensation medium is liquid nitrogen, liquid argon, liquid helium or other refrigerants capable of reaching the condensation temperature, and liquid nitrogen is most preferably adopted.
Preferably, all be equipped with the governing valve of regulation flow on all pipelines of device.
The utility model has the advantages that: the utility model discloses a hydrogen or helium blow in to the molecular sieve adsorption column as the carrier gas under normal atmospheric temperature to striking the special gas in the molecular sieve, thereby realize the special gas in the direct recovery molecular sieve under the normal atmospheric temperature, the recovery cost is low, easy to operate, environmental protection safety, the rate of recovery is up to more than 90%, economic benefits is considerable. Because the utility model discloses a recovery method need not the heating, so other impurity such as the moisture of adsorbing in the molecular sieve are difficult for the desorption for the special gas impurity content of retrieving is low, and the value degree is high. Additionally, the utility model discloses a carrier gas can not introduce impurity, and follow-up direct cryocondensation special gas can be with special gas and carrier gas separation, and the carrier of separation can directly recycle. Therefore, the utility model makes up the technical defect that the special gas adsorbed in the molecular sieve can not be directly recovered in the current industry, and greatly reduces the purification cost of the special gas.
Drawings
Fig. 1 is a schematic structural diagram of the device for recovering the special gas adsorbed by the molecular sieve.
In the figure, a first gas conveying pipeline 1, a second gas conveying pipeline 2, a third gas conveying pipeline 3, a condensing medium conveying pipeline 4, a tube array condenser 5, a gas circulator 6, a gas cylinder 7, a molecular sieve adsorption column 8, a cooling medium inlet 9, a regulating valve 10, a cooling medium outlet 11, a shell-side gas inlet 12 and a shell-side gas outlet 13.
Detailed Description
For better illustration of the objects, technical solutions and advantages of the present invention, the present invention will be further described with reference to the accompanying drawings and examples. It should be understood that the embodiments of the present invention are only used for illustrating the technical effects of the present invention, and are not used for limiting the protection scope of the present invention.
Example 1
As shown in fig. 1, this embodiment 1 provides an apparatus for recovering a special gas adsorbed by a molecular sieve, which includes a first gas conveying pipeline 1, a second gas conveying pipeline 2, a third gas conveying pipeline 3, a condensing medium conveying pipeline 4, a shell and tube condenser 5, a gas circulator 6, and a gas cylinder 7. Specifically, the first gas delivery pipeline 1 is connected to an interface at the bottom of the molecular sieve adsorption column 8, which adsorbs the special gas, and is used for blowing the non-impurity gas into the molecular sieve adsorption column 8 to desorb the special gas in the molecular sieve. One end of the second gas conveying pipeline 2 is connected with an interface at the top of the molecular sieve adsorption column 8, and the other end of the second gas conveying pipeline 2 is connected with a shell side gas inlet 12 of the tube nest condenser 5, so that the mixed gas desorbed from the molecular sieve adsorption column 8 is conveyed to the tube nest condenser 5. The mixed gas passes through the shell side of the tube in the shell-and-tube condenser 5, the tube is filled with a condensing medium, the special gas in the mixed gas outside the tube is condensed by the condensing medium, but the non-impurity gas keeps a gaseous state, so that the special gas is separated from the non-impurity gas. The condensing medium conveying pipeline 4 is connected with a cooling medium inlet 9 at the bottom of the tube array condenser 5 and is used for conveying condensing medium into the tube array of the tube array condenser 5. The third gas conveying pipeline 3 and the gas cylinder 7 are respectively connected with a shell pass gas outlet 13 of the shell-and-tube condenser 5, the third gas conveying pipeline 3 is further connected with the gas circulator 6, and the gas circulator 6 is further connected with the first gas conveying pipeline 1. The third gas transport line 3 is used to discharge the non-impurity gas separated by the shell and tube condenser 5 and to re-transport the discharged non-impurity gas back into the first gas transport line 1 by the gas circulator 6 for re-use as a carrier gas. The gas cylinder 7 is used for recovering the special gas condensed by the tube still condenser 5. After the blowing is finished, evacuating the gas in the shell pass of the tube condenser 5, closing the first gas conveying pipeline 1, the second conveying pipeline 2, the third gas conveying pipeline 3 and the condensing medium conveying pipeline 4, performing auxiliary heating on the tube condenser 5 to convert the special gas condensed into solid or liquid state into gas state again, and then directly recovering the gas from the gas cylinder 7. In addition, the pipelines of the device are all provided with a regulating valve 10 for regulating the flow.
The special gas is arsine, phosphine or germane, the non-impurity gas is hydrogen or helium, and the condensing medium is liquid nitrogen, liquid argon or liquid helium. The top of the tube array condenser 5 is provided with a cooling medium outlet 11, and the gasified nitrogen or argon in the tube array can be discharged from the cooling medium outlet 11.
Example 2: method for recovering germane adsorbed by molecular sieve
200kg of 13X molecular sieve is filled in a molecular sieve adsorption column to be recovered, and the molecular sieve is used for purifying 100kg of germane, and 10kg of germane is absorbed in the molecular sieve.
In this embodiment 2, the device of embodiment 1 is matched to recover germane in the molecular sieve adsorption column, which is specifically as follows:
(1) adopting non-impurity gas as hydrogen, blowing hydrogen flow into the molecular sieve adsorption column at the flow rate of 60L/min, and continuously blowing for 8 h;
(2) condensing the mixed gas discharged from the molecular sieve adsorption column at the temperature of liquid nitrogen, discharging the residual uncondensed hydrogen from a third gas conveying pipeline, and returning the residual uncondensed hydrogen to the first gas conveying pipeline through a gas circulator;
(3) after the hydrogen is blown, evacuating the gas in the shell pass of the tube still condenser, converting the condensed solid germane into gas state again by auxiliary heat, and then directly recovering by using a gas cylinder.
Through detection and statistics, the recovered germane is 9.5kg, and the recovery rate is as high as 95%.
The impurity content of germane recovered in this example is shown in table 1. Therefore, the recovered germane has low impurity content, high purity and high utilization value.
TABLE 1 impurity content of recovered germane
| Gas phase impurity project | H2 | O2 | N2 | CH4 | CO | CO2 | Moisture content |
| Content (ppm) | 230 | 0.23 | 0.47 | ND | ND | ND | 1.9 |
Example 3: method for recovering arsine adsorbed by molecular sieve
The molecular sieve adsorption column to be recovered is filled with 200kg of 4A molecular sieve, which was used for purifying 200kg of arsine, and 30kg of arsine is absorbed in the molecular sieve.
In this embodiment 3, the apparatus of embodiment 1 is used to recover arsine in the molecular sieve adsorption column, which is specifically as follows:
(1) adopting non-impurity gas as hydrogen, blowing hydrogen flow into the molecular sieve adsorption column at the flow rate of 60L/min, and continuously blowing for 8 h;
(2) condensing the mixed gas discharged from the molecular sieve adsorption column at the temperature of liquid nitrogen, discharging the residual uncondensed hydrogen from a third gas conveying pipeline, and returning the residual uncondensed hydrogen to the first gas conveying pipeline through a gas circulator;
(3) after the hydrogen blowing is finished, the gas in the shell pass of the condenser is pumped out, the condensed solid arsine is converted into a gaseous state again through auxiliary heat, and then the gaseous arsine is directly recovered by using a gas cylinder.
Through detection and statistics, the recovered arsine in the embodiment is 28kg, and the recovery rate is up to 93.3%.
Example 4: the influence of the flow rate and the blowing time of the non-impurity gas on the recovery effect of the special gas is explored
The experimental method comprises the following steps: referring to the recovery method of example 2, 13X molecular sieves adsorbed with 10kg of germane were blown with hydrogen gas at flow rates of 10L/min, 20L/min, 40L/min, 60L/min, 80L/min and 100L/min, respectively, for 8 hours, and the recovered germane weights are as shown in Table 2 below.
TABLE 2 germane recovery effect at different hydrogen flow rates
As can be seen from Table 2, the higher the recovery rate of germane with the increase of the hydrogen flow rate, the less significant the increase of the recovery rate of germane when the hydrogen flow rate reaches 60L/min or more, and other impurities are carried over with the flow rate being too high. Therefore, the invention takes 60L/min as the preferable flow rate of the non-impurity gas, the recovery rate of germane reaches 95 percent, and the recovered germane has higher purity.
The experimental method comprises the following steps: referring to the recovery method of example 2, 13X molecular sieves, which absorbed 10kg of germane, were blown with hydrogen gas at a flow rate of 60L/min for 2 hours, 4 hours, 6 hours, 8 hours, 10 hours and 12 hours, respectively, and the weights of the recovered germane were as shown in Table 3 below.
TABLE 3 recovery of germane at different blowing times
As can be seen from table 3, the higher the recovery rate of germane as the blowing time increased, and when the blowing time reached 8 hours or more, the increase in the recovery rate of germane was insignificant. Therefore, the invention takes 8h as the preferable blowing time of the non-impurity gas, the recovery rate of the germane is as high as 95%, and the recovered germane has higher purity.
It should be finally noted that the above embodiments are only intended to illustrate the technical solutions of the present invention and not to limit the scope of the present invention, and although the present invention has been described in detail with reference to the preferred embodiments, those skilled in the art should understand that the technical solutions of the present invention can be modified or replaced with equivalents without departing from the spirit and scope of the technical solutions of the present invention.
Claims (9)
1. The device for recovering the special gas adsorbed by the molecular sieve is characterized by comprising a first gas conveying pipeline, a second gas conveying pipeline and a condenser; the first gas conveying pipeline is used for blowing non-impurity gas into the molecular sieve adsorption column which adsorbs the special gas so as to desorb the special gas in the molecular sieve adsorption column; the second gas conveying pipeline is used for conveying the mixed gas desorbed from the molecular sieve adsorption column to the condenser; the condenser is used for condensing the special gas in the mixed gas to separate the special gas from the non-impurity gas; the non-impurity gas is hydrogen or helium; the special gas is arsine, phosphine or germane.
2. The apparatus for recovering a specialty gas from molecular sieve adsorption of claim 1, wherein said first gas delivery line is connected to an interface at the bottom of a molecular sieve adsorption column.
3. The apparatus for recovering a specialty gas from molecular sieve adsorption of claim 1, wherein one end of said second gas feed line is connected to a port at the top of said molecular sieve adsorption column and the other end of said second gas feed line is connected to said condenser.
4. The apparatus for recovering a specialty gas from molecular sieve adsorption of claim 1, wherein said condenser is a shell-side condenser, the mixed gas is fed out of the shell side of the tube, the tube is filled with a condensing medium, and said second gas feed line is connected to the shell side gas inlet of said condenser.
5. The apparatus for recovering a specialty gas from molecular sieve adsorption of claim 1, further comprising a condensing medium delivery line; and the condensing medium conveying pipeline is used for conveying condensing medium into the condenser.
6. The apparatus for recovering a specialty gas from molecular sieve adsorption of claim 4, further comprising a third gas delivery line and a gas circulator; one end of the third gas conveying pipeline is connected with a shell pass gas outlet of the condenser, the other end of the third gas conveying pipeline is connected with the gas circulator, and the gas circulator is further connected with the first gas conveying pipeline.
7. The apparatus for recovering a specialty gas from molecular sieve adsorption of claim 4, wherein said apparatus further comprises a gas cylinder; the gas cylinder is connected with a shell pass gas outlet of the condenser and is used for recovering the special gas collected by the condenser.
8. The apparatus for recovering a specialty gas from molecular sieve adsorption of claim 4 or 5 wherein said condensing medium is liquid nitrogen, liquid argon or liquid helium.
9. The apparatus for recovering a specialty gas from molecular sieve adsorption of claim 4, wherein all lines of said apparatus are provided with flow regulating valves.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110548364A (en) * | 2019-10-17 | 2019-12-10 | 清远先导材料有限公司 | method and device for recovering special gas adsorbed by molecular sieve |
| CN115155249A (en) * | 2022-09-05 | 2022-10-11 | 济南德洋低温科技有限公司 | Method and device for recovering special gas adsorbed by molecular sieve |
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2019
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110548364A (en) * | 2019-10-17 | 2019-12-10 | 清远先导材料有限公司 | method and device for recovering special gas adsorbed by molecular sieve |
| CN115155249A (en) * | 2022-09-05 | 2022-10-11 | 济南德洋低温科技有限公司 | Method and device for recovering special gas adsorbed by molecular sieve |
| CN115155249B (en) * | 2022-09-05 | 2022-12-02 | 济南德洋低温科技有限公司 | Method and device for recovering special gas adsorbed by molecular sieve |
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