CN112473316A - Temperature swing adsorption gas purification system and purification process - Google Patents
Temperature swing adsorption gas purification system and purification process Download PDFInfo
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- CN112473316A CN112473316A CN202011347487.2A CN202011347487A CN112473316A CN 112473316 A CN112473316 A CN 112473316A CN 202011347487 A CN202011347487 A CN 202011347487A CN 112473316 A CN112473316 A CN 112473316A
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- 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
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Abstract
The invention discloses a temperature swing adsorption gas purification system and a purification process, which comprises a raw material gas inlet main pipe, an adsorption purification device, a product gas discharge main pipe, a regeneration heater, a regeneration vacuum pump and a regeneration liquid separation tank, wherein the device adopts an adsorbent regeneration mode as vacuum negative pressure regeneration when a control system operates, the temperature swing flushing regeneration is switched once when the control index of the device rises after the vacuum negative pressure regeneration operates for several months, the temperature swing flushing regeneration is performed for several months, the vacuum negative pressure regeneration is performed to the next flushing regeneration, and the cycle regeneration is performed. By adopting the circulating regeneration mode, the consumption of the regenerated gas and steam and the consumption of circulating cooling water which are required by adopting the temperature-variable flushing regeneration all the time can be saved; the overall investment of the device is greatly reduced.
Description
Technical Field
The invention relates to the technical field of temperature swing adsorption towers and adsorbent regeneration, in particular to a temperature swing adsorption gas purification system and a purification process.
Background
The temperature swing adsorption is mainly used for removing trace impurity components which are difficult to desorb at normal temperature and normal pressure after adsorption, the regeneration of the adsorbent is carried out at normal pressure and high temperature, and the regeneration comprises two steps of high-temperature flushing regeneration and low-temperature flushing regeneration. The regenerated gas source is generally the product gas after temperature swing adsorption purification or other gas which is not free of impurity removal and has no influence on the performance of the adsorbent from the outside of the boundary zone. When the regeneration is carried out by high-temperature flushing, the regeneration air source is heated by steam through the heater, and then the bed layer is heated to the required temperature from top to bottom through the adsorption tower, so that the adsorbed impurities are desorbed at high temperature. When the regeneration is carried out by low-temperature flushing, the bed layer is flushed to the normal temperature from top to bottom through the adsorption tower by the regeneration gas at the normal temperature. Because the water adsorbed during the high-temperature washing regeneration needs a large amount of heat for vaporization and the temperature rise of the adsorption bed layer, and the flow rate of the regeneration gas is constant, the temperature swing adsorption regeneration time is generally longer (about more than 10 hours), the adsorption time is also longer, the loading amount of the adsorbent is larger, the weight of equipment is increased, and the overall investment of the device is larger.
The adsorbent has an effect on the performance of the adsorbent functional groups during high temperature rinse regeneration (maximum regeneration temperature about 220 ℃). The performance of the adsorbent is attenuated to a certain extent along with the increase of the high-temperature flushing regeneration times, so that the service life of the adsorbent and the performance index of purified gas are influenced.
The temperature of the regenerated tail gas after regeneration is 40-220 ℃, the tail gas needs to be cooled to 50 ℃ by a cooler before going out of the border area, and a large amount of circulating cooling water is consumed.
The existing regeneration process has the following problems:
the regeneration of temperature swing adsorption requires large amount of regenerated gas, large consumption of steam and cooling water, and high operation cost.
Secondly, the long regeneration time (the total time of high-temperature washing regeneration and low-temperature washing regeneration is about 10 hours) causes large adsorbent filling amount, increases the equipment weight of the adsorption tower and increases the total investment of the device.
And thirdly, the performance of the adsorbent is obviously attenuated due to frequent high-temperature washing regeneration, and the service life of the adsorbent and the performance index of the device are influenced. Or in order to solve the problem caused by the performance degradation of the adsorbent, the amount of the adsorbent needs to be increased, thereby increasing the investment of the device.
And fourthly, when the product gas purified by the device is used as a regeneration gas source, the processing load of the device needs to be additionally increased, and further the investment and the consumption are increased.
Disclosure of Invention
The invention aims to provide a temperature swing adsorption gas purification system and a purification process.
In order to achieve the purpose, the invention is implemented according to the following technical scheme:
the temperature swing adsorption gas purification system comprises a raw material gas inlet main pipe, adsorption purification devices, a product gas discharge main pipe, a regeneration heater, a regeneration vacuum pump and a regeneration liquid separation tank, wherein the adsorption purification devices are in multiple groups, an inlet pipeline of each group of adsorption purification device is connected with the raw material gas inlet main pipe in parallel, an outlet pipeline of each group of adsorption purification device is connected with the product gas discharge main pipe in parallel, an inlet pipeline of the adsorption purification device is connected with an inlet of the regeneration vacuum pump through a group of branch pipelines connected in parallel, an inlet pipeline of the adsorption purification device is connected with an inlet of a pressure reduction regulating valve through another group of branch pipelines, an outlet of the pressure reduction regulating valve and an outlet of the regeneration vacuum pump are both connected with an inlet of the regeneration liquid separation tank, and an outlet of the regeneration liquid separation tank is a vacuum desorption gas outlet main pipe, the outlet pipeline of the adsorption and purification device is simultaneously connected with the outlet of the regenerative heater and the outlet of the eighth program control valve through a group of branch pipelines, the inlet of the regenerative heater is connected with the outlet of the ninth program control valve, and the inlets of the eighth program control valve and the ninth program control valve are connected with the high-temperature flushing regeneration air inlet main pipe.
The product gas discharge main pipe is connected with one end of a pressure boosting pipe, the middle section of the pressure boosting pipe is provided with a pressure boosting regulating valve, and the other end of the pressure boosting pipe is connected with another group of branch pipelines arranged on an outlet pipeline of the adsorption purification device in parallel.
The inlet pipeline of the adsorption purification device is connected with a high-temperature flushing regeneration air outlet main pipe through another group of branch pipelines connected in parallel.
The adsorption purification device comprises a raw material gas inlet branch pipe, an adsorption tower, a product gas discharge branch pipe, a third branch pipe, a fourth branch pipe, a first gas outlet branch pipe, a second gas outlet branch pipe, a third gas outlet branch pipe, a first program control valve, a second program control valve, a third program control valve, a fourth program control valve, a fifth program control valve, a sixth program control valve and a seventh program control valve, wherein one end of the raw material gas inlet branch pipe is connected with the raw material gas inlet main pipe in parallel through the first program control valve, the other end of the raw material gas inlet branch pipe is connected with an inlet of the adsorption tower, the pipe walls of the raw material gas inlet branch pipe are respectively communicated and connected with one ends of the first gas outlet branch pipe, the second gas outlet branch pipe and the third gas outlet branch pipe, the other ends of the first gas outlet branch pipe, the second gas outlet branch pipe and the third gas outlet branch pipe are communicated and connected with another group of the first gas outlet branch pipe, the second gas outlet branch pipe and the, the terminals of the first gas outlet branch pipe, the second gas outlet branch pipe and the third gas outlet branch pipe are respectively connected with the fifth program control valve, the sixth program control valve and the seventh program control valve in series, one end of the product gas discharge branch pipe is connected with the outlet of the adsorption tower, the other end of the product gas discharge branch pipe is connected with one end of the second program control valve, the other end of the second program control valve is connected with the product gas discharge main pipe, the pipe wall of the product gas discharge branch pipe is respectively communicated and connected with one end of the third branch pipe and one end of the fourth branch pipe, the other ends of the third branch pipe and the fourth branch pipe are connected with the third branch pipe and the fourth branch pipe of the adsorption purification device in parallel and communicated, the third branch pipe and the fourth branch pipe are connected with the third program control valve and the fourth program control valve in series, the third gas outlet branch pipe is connected with the high-temperature washing regeneration main pipe, and the second gas outlet branch pipe is connected with the inlet of the regeneration, the first air outlet branch pipe is connected with an inlet of the pressure reduction regulating valve, the fourth branch pipe is connected with the eighth program control valve and the regeneration heater, and the third branch pipe is connected with the pressure increase regulating valve.
The invention relates to a temperature swing adsorption gas purification process, which comprises a vacuum negative pressure regeneration process and a temperature swing flushing regeneration process, wherein the vacuum negative pressure regeneration process comprises the following steps:
adsorption: the raw material gas enters the adsorption tower through the first program control valve, impurity components in the raw material gas are sequentially adsorbed by a plurality of adsorbents filled in the adsorption tower, the obtained purified product gas is discharged through the second program control valve, and along with the adsorption, when the front edge of impurities rises to be close to the height of the adsorption bed, the first program control valve and the second program control valve are closed, and the adsorption is stopped;
reverse playing: after the adsorption process is finished, the adsorption front of the adsorption tower basically reaches the outlet of the bed layer, at the moment, a fifth program control valve is opened, the pressure of the adsorption tower is reduced to normal pressure against the adsorption direction, at the moment, a small part of adsorbed impurity components begin to be desorbed from the adsorbent, the reverse desorption gas enters a regeneration liquid separation tank after being regulated by a pressure reduction regulating valve, and then enters a gas pipe network along with the vacuum desorption gas;
when the adsorption pressure is lower or the regeneration pressure is close to the adsorption pressure, the process step II is not needed;
thirdly, vacuum negative pressure regeneration: after the reverse release is finished, opening a sixth program control valve, performing vacuum-pumping desorption on the adsorption bed layer by using a regeneration vacuum pump, desorbing impurities adsorbed by the adsorbent under negative pressure to finish the regeneration of the adsorbent, and allowing the vacuum regenerated gas to enter a gas pipe network together with the reverse release desorbed gas after passing through a regeneration liquid separation tank;
fourthly, boosting pressure: after the vacuum negative pressure desorption is finished, opening a third program control valve, slowly boosting the purified product gas to the adsorption pressure by a boosting regulating valve against the adsorption direction, and then switching the adsorption tower to the next adsorption process;
when the step II does not exist, the process step IV is not needed;
the adsorption and regeneration processes are alternately carried out by a plurality of adsorption towers, so that the continuous purification of the feed gas can be realized;
the temperature-changing flushing regeneration process comprises the following steps:
cutting off the adsorption tower: after the adsorption tower completes negative pressure regeneration, the control system cuts off the adsorption tower, so that the adsorption tower is isolated from other adsorption towers in the system, preparation is made for temperature-changing flushing regeneration, and at the moment, the other adsorption towers except the adsorption tower still run in a vacuum negative pressure regeneration mode;
sixthly, high-temperature washing regeneration: opening a ninth program control valve, a fourth program control valve and a seventh program control valve, heating the regenerated gas from the outside of the battery compartment to about 240 ℃ by a regeneration heater, then passing through the adsorption tower from top to bottom, flushing the bed layer of the adsorption tower at high temperature to the required temperature, and flushing the desorption gas at high temperature to enter a flare gas pipe network;
flushing and regenerating at high temperature, maintaining the temperature of the gas at the regeneration outlet of the adsorption tower at 40 ℃ at the beginning, and ending the step when the temperature is gradually and slowly increased to be more than or equal to 150 ℃;
seventhly, constant-temperature flushing regeneration: when the outlet temperature of the adsorption tower for high-temperature flushing regeneration reaches the required temperature, continuously keeping the higher-temperature flushing process, namely constant-temperature flushing, for fully regenerating the adsorbent, and controlling the constant temperature to be 220 ℃ at 150-;
low-temperature washing and regeneration: after the constant-temperature flushing is finished, starting to perform low-temperature flushing on the adsorption tower, closing the ninth program-controlled valve, opening the eighth program-controlled valve, the fourth program-controlled valve and the seventh program-controlled valve to enable low-temperature flushing gas with the temperature of less than or equal to 40 ℃ to enter the adsorption tower from top to bottom, performing low-temperature flushing on a bed layer of the adsorption tower to the required temperature, and enabling regenerated desorption gas to enter a flare gas pipe network;
low-temperature flushing regeneration, wherein the temperature of the gas at the regeneration outlet of the adsorption tower is basically maintained to be more than or equal to 150 ℃ at the beginning stage, and the step (b) is finished when the temperature is gradually and slowly reduced to be less than or equal to 45 ℃;
ninthly, investment into an adsorption tower: and closing all the program control valves connected with the cut adsorption tower after the low-temperature flushing regeneration is finished, and putting the adsorption tower into operation through a control system, so that the adsorption tower finishes a temperature-changing flushing regeneration process.
The invention has the beneficial effects that:
the invention relates to a temperature swing adsorption gas purification system and a purification process, compared with the prior art, the invention has the following effects:
firstly, the regeneration mode of the adsorbent during the operation of the device is vacuum negative pressure regeneration, after the vacuum negative pressure regeneration is operated for several months, when the control index of the device has a rising trend, the temperature-variable flushing regeneration is switched once, after the temperature-variable flushing regeneration is performed for several months, the vacuum negative pressure regeneration is performed to the next temperature-variable flushing regeneration, and the cycle regeneration is performed. By adopting the circulating regeneration mode, the consumption of the regeneration gas and the steam and the consumption of circulating cooling water which are required by adopting the temperature-changing flushing regeneration all the time can be saved. With a throughput of 60000Nm3The purification of the coke oven gas is carried out by taking an example, 6000Nm can be saved in each hour3Regeneration gas, about 3t medium pressure steam and about 30t circulating cooling water. The operation cost is greatly reduced, and the economic benefit is obvious.
Secondly, because the content of the impurities to be removed in the raw material gas is trace, the total amount of the removed impurities is not much, the air suction amount required by a vacuum pump is small when vacuum negative pressure desorption is adopted, the vacuumizing time of one tower is controlled to be several hours, so that the vacuum negative pressure desorption time is only about 40% of the temperature-variable flushing regeneration desorption time, and the filling amount of the adsorbent in the vacuum negative pressure desorption process can be reduced to about 70% of the adsorbent amount required by the temperature-variable flushing regeneration. The amount of the adsorbent is reduced, the adsorption tower equipment is also reduced, and the overall investment of the device is greatly reduced.
Thirdly, because the temperature-changing flushing regeneration is carried out for several months, the performance attenuation of the adsorbent caused by the high-temperature flushing regeneration is effectively slowed down, the service life of the adsorbent and the performance index of the device are effectively ensured, and meanwhile, the using amount of the adsorbent can be properly reduced, thereby reducing the investment of the device.
And fourthly, when the purified product gas is used as a regeneration gas source, the design load of the device can be reduced by 10% in the vacuum negative pressure regeneration process compared with the variable temperature flushing regeneration process, so that the flow rate of the raw material gas can be saved, the yield of the effective gas can be improved, and the overall investment of the device can be reduced.
Drawings
Fig. 1 is a schematic structural view of the present invention.
In the figure: 1-raw material gas inlet main pipe, 2-adsorption purification device, 3-product gas discharge main pipe, 4-regenerative heater, 5-regenerative vacuum pump, 6-regenerative liquid separation tank, 7-pressure rising pipe, 8-raw material gas inlet branch pipe, 9-adsorption tower, 10-product gas discharge branch pipe, 11-third branch pipe, 12-fourth branch pipe, 13-first gas outlet branch pipe, 14-second gas outlet branch pipe, 15-third gas outlet branch pipe, 16-high temperature flushing regenerative gas inlet main pipe, 17-vacuum desorption gas outlet main pipe, and 18-high temperature flushing regenerative gas outlet main pipe.
Detailed Description
The invention will be further described with reference to the drawings and specific embodiments, which are illustrative of the invention and are not to be construed as limiting the invention.
As shown in fig. 1: the invention comprises a raw material gas inlet main pipe 1, adsorption purification devices 2, a product gas discharge main pipe 3, a regeneration heater 4, a regeneration vacuum pump 5 and a regeneration liquid separation tank 6, wherein the adsorption purification devices 2 are in multiple groups, the inlet pipeline of each group of adsorption purification device 2 is connected with the raw material gas inlet main pipe 1 in parallel, the outlet pipeline of each group of adsorption purification device 2 is connected with the product gas discharge main pipe 3 in parallel, the inlet pipeline of the adsorption purification device 2 is connected with the inlet of the regeneration vacuum pump 5 through a group of branch pipelines connected in parallel, the inlet pipeline of the adsorption purification device 2 is connected with the inlet of a pressure reduction regulating valve V11 through another group of branch pipelines, the outlet of the pressure reduction regulating valve V11 and the outlet of the regeneration vacuum pump 5 are connected with the inlet of the regeneration liquid separation tank 6, the outlet of the regeneration liquid separation tank 6 is a vacuum desorption gas outlet main pipe 17, the outlet pipeline of the adsorption and purification device 2 is connected with the outlet of the regenerative heater 4 and the outlet of the eighth program control valve V8 through a group of branch pipelines, the inlet of the regenerative heater 4 is connected with the outlet of the ninth program control valve V9, and the inlets of the eighth program control valve V8 and the ninth program control valve V9 are connected with the high-temperature flushing regeneration air inlet main pipe 16.
One end of a booster pipe 7 is connected to the pipeline of the product gas discharge main pipe 3, a booster regulating valve V10 is arranged in the middle section of the booster pipe 7, and the other end of the booster pipe 7 is connected in parallel with another group of branch pipelines arranged on the outlet pipeline of the adsorption and purification device 2.
The inlet pipeline of the adsorption purification device 2 is connected with a high-temperature flushing regeneration gas outlet main pipe 18 through another group of branch pipelines connected in parallel.
The adsorption purification device 2 is composed of a raw material gas inlet branch pipe 8, an adsorption tower 9, a product gas discharge branch pipe 10, a third branch pipe 11, a fourth branch pipe 12, a first gas outlet branch pipe 13, a second gas outlet branch pipe 14, a third gas outlet branch pipe 15, a first program control valve V1A, a second program control valve V2A, a third program control valve V3A, a fourth program control valve V4A, a fifth program control valve V5A, a sixth program control valve V6A and a seventh program control valve V7A, one end of the raw material gas inlet branch pipe 8 is connected with the raw material gas inlet main pipe 1 in parallel through the first program control valve V1A, the other end of the raw material gas inlet branch pipe 8 is connected with an inlet of the adsorption tower 9, the pipe wall of the raw material gas inlet branch pipe 8 is respectively communicated with one ends of the first gas outlet branch pipe 13, the second gas outlet branch pipe 14 and the third gas outlet branch pipe 15, and the other ends of the first gas outlet branch pipe 13, the second gas outlet branch pipe 14 and the third branch pipe 15 are respectively connected with one end of the first gas outlet branch pipe 13, The second outlet branch pipe 14 and the third outlet branch pipe 15 are connected in parallel and in communication, the terminals of the first outlet branch pipe 13, the second outlet branch pipe 14 and the third outlet branch pipe 15 are respectively connected in series with the fifth program control valve V5A, the sixth program control valve V6A and the seventh program control valve V7A, one end of the product gas discharge branch pipe 10 is connected with the outlet of the adsorption tower 9, the other end of the product gas discharge branch pipe 10 is connected with one end of the second program control valve V2A, the other end of the second program control valve V2A is connected with the main product gas discharge pipe 3, the pipe wall of the product gas discharge branch pipe 10 is respectively connected in communication with one end of the third branch pipe 11 and one end of the fourth branch pipe 12, the other ends of the third branch pipe 11 and the fourth branch pipe 12 are connected in parallel and in communication with another group of the third branch pipe 11 and the fourth branch pipe 12 of the adsorption purification device 2, the middle section of the third branch pipe 11 and the fourth branch pipe 12 are connected in series with the third program control valve V3A and the fourth program control valve V4A, third air outlet branch pipe 15 is connected high temperature and is washed regeneration air outlet main pipe 18, the entry of regeneration vacuum pump 5 is connected to second air outlet branch pipe 14, the entry of decompression governing valve V11 is connected to first air outlet branch pipe 13, eighth programme-controlled valve V8 and regenerative heater 4 are connected to fourth branch pipe 12, third branch pipe 11 is connected pressure boost governing valve V10.
The specific working principle of the cyclic regeneration process is as follows:
the whole process of the main flow will be described by taking the adsorption tower 9 as an example, and the operation processes of the adsorption towers 9 in the plurality of adsorption purification devices 2 are completely the same.
Firstly, a vacuum negative pressure regeneration process:
the vacuum negative pressure regeneration is realized by using the principle that the adsorption capacity of the adsorbent to impurities is obviously weakened under the negative pressure, and the adsorbed impurities are desorbed from the adsorbent, so that the adsorbent is regenerated. For the desorption effect of removing trace impurities with strong adsorption capacity: the vacuum negative pressure regeneration effect is stronger than the normal pressure flushing regeneration effect but weaker than the temperature-changing flushing regeneration effect. Therefore, under the working condition, the adsorbent needs to be regenerated by adopting temperature-changing flushing after vacuum negative pressure regeneration for several months to strengthen the regeneration effect.
When the adsorbent is put into operation for the first time or is regenerated by temperature-changing flushing, the adsorbent can be put into vacuum negative pressure regeneration, and the technical process is as follows:
1, adsorption:
the raw material gas enters the adsorption tower 9 through a first program control valve V1A, impurity components in the raw material gas are sequentially adsorbed by a plurality of adsorbents filled in the adsorption tower 9, and the obtained purified product gas is discharged through a second program control valve V2A. When the front of the impurities (i.e. adsorption front) rises to a certain height close to the adsorption bed as the adsorption proceeds, the first and second programmable valves V1A and V2A are closed to stop the adsorption.
2 is put in the reverse direction
After the adsorption process is finished, the adsorption front of the adsorption tower 9 has substantially reached the bed outlet. At this point, the fifth programmable valve V5A is opened to reduce the pressure in the adsorption column 9 to atmospheric pressure against the adsorption direction, at which point a small portion of the adsorbed impurity components begins to desorb from the adsorbent. The reverse desorption gas enters a regeneration liquid separation tank after being regulated by a pressure reduction regulating valve V11, and then enters a gas pipe network along with the vacuum desorption gas.
This process step is not required when the adsorption pressure is low (e.g., gas purge, which has an adsorption pressure of about 10KPa) or the regeneration pressure is close to the adsorption pressure.
3, vacuum negative pressure regeneration:
and after the reverse release is finished, opening a sixth program control valve V6A, and performing vacuum-pumping desorption on the adsorption bed layer by using a regenerative vacuum pump. At the moment, the impurities adsorbed by the adsorbent are desorbed under negative pressure, and the regeneration of the adsorbent is completed. The vacuum regenerated gas passes through the regeneration liquid separation tank and then enters a gas pipe network together with the reverse desorption gas.
4, boosting pressure:
after the vacuum negative pressure desorption is finished, the third program control valve V3A is opened, the purified product gas is slowly boosted to the adsorption pressure by the pressure boosting regulating valve V10 against the adsorption direction, and then the adsorption tower is shifted to the next adsorption process.
When there is no reverse step, step 2, then this process step is not required.
The 4 adsorption towers alternately carry out the adsorption and regeneration processes, so that the continuous purification of the feed gas can be realized.
Second, temperature-changing flushing regeneration process
The temperature-changing flushing regeneration comprises three main processes: high-temperature washing regeneration, constant-temperature washing regeneration and low-temperature washing regeneration.
The temperature-varying flushing regeneration includes two aspects of bed heating and flushing, and its principle is that the adsorption capacity of adsorbent to adsorbed impurity is weakened at higher temp., at the same time, the adsorption impurity content in regenerated gas is low, and the concentration of adsorbed impurity between adsorbent micropores and gaps is high, and when the regenerated gas is passed through the adsorption bed layer in the course of flushing from top to bottom, the adsorbed impurity can be transferred from high concentration to low concentration so as to make the adsorbent obtain desorption and regeneration.
When the control index of the device has an ascending trend after the adsorption tower 9 is operated for several months in a vacuum negative pressure regeneration mode, temperature-changing flushing regeneration needs to be carried out, and the process is as follows:
1 cut adsorption column
After the adsorption tower 9 finishes negative pressure regeneration, the adsorption tower 9 is cut off in the control system, so that the adsorption tower 9 is isolated from other adsorption towers in the system, and preparation is made for temperature-changing flushing regeneration. At this time, the adsorption columns other than the adsorption column 9 are still operated in the vacuum negative pressure regeneration mode.
2 high temperature washing regeneration
And opening a ninth program control valve V9, a fourth program control valve V4A and a seventh program control valve V7A, heating the regeneration gas (or using the purified product gas in the device system as a regeneration gas source) from outside the battery limits to about 240 ℃ by a regeneration heater, then passing through the adsorption tower from top to bottom, flushing the bed layer of the adsorption tower to the required temperature at high temperature, and flushing the desorption gas at high temperature to enter a flare gas pipe network. Since the process is to regenerate the adsorption column after the removal of the column, the amount of regeneration gas and steam used can be reduced by extending the high temperature purge time, which usually takes several days.
And (3) high-temperature flushing regeneration, wherein the temperature of the regeneration outlet gas of the adsorption tower is basically maintained at 40 ℃ in the initial stage, and the step is finished when the temperature is gradually and slowly increased to be more than or equal to 150 ℃.
3 constant temperature flushing regeneration
When the outlet temperature of the adsorption tower for high-temperature washing regeneration reaches the required temperature, the process of washing at a higher temperature is continuously kept for fully regenerating the adsorbent, namely constant-temperature washing. The constant temperature flushing time is about several hours according to the different constant temperature of the desorption substance and is controlled at 150 ℃ and 220 ℃.
4 low temperature flushing regeneration
And after the constant-temperature flushing is finished, starting to perform low-temperature flushing on the adsorption tower, closing the ninth program-controlled valve V9, opening the eighth program-controlled valve V8, the fourth program-controlled valve V4A and the seventh program-controlled valve V7A, enabling low-temperature flushing gas with the temperature of less than or equal to 40 ℃ to enter the adsorption tower from top to bottom, performing low-temperature flushing on the bed layer of the adsorption tower to the required temperature, and enabling regenerated desorption gas to enter a flare gas pipe network. In this process, since the adsorption tower is removed and then regenerated, the amount of regeneration gas and cooling water used can be reduced by prolonging the time of low-temperature flushing, and it usually takes several days.
And (3) low-temperature flushing regeneration, wherein the temperature of the gas at the regeneration outlet of the adsorption tower is basically maintained to be more than or equal to 150 ℃ at the beginning stage, and the step is finished when the temperature is gradually and slowly reduced to be less than or equal to 45 ℃.
5 feeding adsorption tower
And closing all program control valves of the adsorption tower 9 after the low-temperature flushing regeneration is finished, and putting the adsorption tower 9 into operation in a control system, so that the adsorption tower 9 finishes a temperature-changing flushing regeneration process.
The adsorption tower 9 is then regenerated by vacuum negative pressure operation, and after several months, the next regeneration by temperature-changing flushing is carried out when the control index of the device is on the rising trend again. The vacuum negative pressure regeneration and the temperature-changing flushing regeneration are continuously circulated to complete the whole regeneration process of the adsorption bed layer, so the process is called a cyclic regeneration process.
In the device for removing trace impurities in the raw material gas by adopting temperature swing adsorption, an independent negative pressure regeneration mode, a regeneration mode of serial connection or parallel connection or cyclic switching of negative pressure regeneration and temperature swing flushing regeneration belong to the cyclic regeneration process.
The above-mentioned example is only one of the preferred embodiments of the cyclic regeneration process, and should not be used to limit the scope of the cyclic regeneration process, but any insubstantial modifications or modifications made in the main design concept and spirit of the cyclic regeneration process, which still solve the technical problems consistent with the cyclic regeneration process, should be included in the scope of the cyclic regeneration process.
The technical solution of the present invention is not limited to the limitations of the above specific embodiments, and all technical modifications made according to the technical solution of the present invention fall within the protection scope of the present invention.
Claims (10)
1. A temperature swing adsorption gas purification system characterized by: comprises a raw material gas inlet main pipe (1), an adsorption purification device (2), a product gas discharge main pipe (3), a regeneration heater (4), a regeneration vacuum pump (5) and a regeneration liquid separation tank (6), wherein the adsorption purification device (2) is a plurality of groups, each group comprises inlet pipelines of the adsorption purification device (2) which are connected with the raw material gas inlet main pipe (1) in parallel, each group comprises outlet pipelines of the adsorption purification device (2) which are connected with the product gas discharge main pipe (3) in parallel, the inlet pipelines of the adsorption purification device (2) are connected with an inlet of the regeneration vacuum pump (5) through a group of branch pipelines which are connected in parallel, the inlet pipelines of the adsorption purification device (2) are connected with an inlet of a pressure reduction regulating valve (V11) through another group of branch pipelines, an outlet of the pressure reduction regulating valve (V11) and an outlet of the regeneration vacuum pump (5) are connected with an inlet of the regeneration liquid separation tank (6), the outlet of the regeneration liquid separation tank (6) is a vacuum desorption gas outlet main pipe (17), an outlet pipeline of the adsorption and purification device (2) is simultaneously connected with the outlet of the regeneration heater (4) and the outlet of the eighth program control valve (V8) through a group of branch pipelines, the inlet of the regeneration heater (4) is connected with the outlet of the ninth program control valve (V9), and the inlets of the eighth program control valve (V8) and the ninth program control valve (V9) are connected with a high-temperature flushing regeneration gas inlet main pipe (16).
2. The temperature swing adsorption gas purification system according to claim 1, wherein: the product gas discharge main pipe (3) is connected with one end of a pressure boosting pipe (7), the middle section of the pressure boosting pipe (7) is provided with a pressure boosting regulating valve (V10), and the other end of the pressure boosting pipe (7) is connected with another component branch pipe arranged on an outlet pipe of the adsorption and purification device (2) in parallel.
3. The temperature swing adsorption gas purification system according to claim 1, wherein: the inlet pipeline of the adsorption purification device (2) is connected with a high-temperature flushing regeneration gas outlet main pipe (18) through another group of branch pipelines connected in parallel.
4. The temperature swing adsorption gas purification system according to any one of claims 1-3, wherein: the adsorption purification device (2) comprises a raw material gas inlet branch pipe (8), an adsorption tower (9), a product gas discharge branch pipe (10), a third branch pipe (11), a fourth branch pipe (12), a first gas outlet branch pipe (13), a second gas outlet branch pipe (14), a third gas outlet branch pipe (15), a first program control valve (V1A), a second program control valve (V2A), a third program control valve (V3A), a fourth program control valve (V4A), a fifth program control valve (V5A), a sixth program control valve (V6A) and a seventh program control valve (V7A), one end of the raw material gas inlet branch pipe (8) is connected with the raw material gas inlet main pipe (1) in parallel through the first program control valve (V1A), the other end of the raw material gas inlet branch pipe (8) is connected with an inlet of the gas outlet tower (9), and the pipe wall of the raw material gas inlet branch pipe (8) is respectively communicated with one end of the first branch pipe (13), the second gas outlet branch pipe (14) and one end of the third gas outlet branch pipe (15), the other ends of the first gas outlet branch pipe (13), the second gas outlet branch pipe (14) and the third gas outlet branch pipe (15) are communicated with the first gas outlet branch pipe (13), the second gas outlet branch pipe (14) and the third gas outlet branch pipe (15) of another group of the adsorption purification device (2) in parallel, the terminals of the first gas outlet branch pipe (13), the second gas outlet branch pipe (14) and the third gas outlet branch pipe (15) are respectively connected with the fifth program control valve (V5A), the sixth program control valve (V6A) and the seventh program control valve (V7A) in series, one end of the product gas exhaust branch pipe (10) is connected with the outlet of the adsorption tower (9), the other end of the product gas exhaust branch pipe (10) is connected with one end of the second program control valve (V2A), the other end of the second program control valve (V2A) is connected with the product gas exhaust main pipe (3), and the pipe wall of the product gas exhaust branch pipe (10) is respectively communicated with one end of the third branch pipe (11) and the fourth branch pipe (12), third branch pipe (11) with the other end and another group of fourth branch pipe (12) adsorb third branch pipe (11) and fourth branch pipe (12) of purifier (2) and parallelly connected the connection that communicates with each other, third branch pipe (11) with establish ties on the middle section of fourth branch pipe (12) third program control valve (V3A) with fourth program control valve (V4A), third branch pipe (15) of giving vent to anger is connected high temperature and is washed regeneration and give vent to anger person in charge (18), the entry of regeneration vacuum pump (5) is connected in second branch pipe (14), the entry of decompression governing valve (V11) is connected in first branch pipe (13), eighth program control valve (V8) and regenerative heater (4) are connected in fourth branch pipe (12), third branch pipe (11) are connected boost governing valve (V10).
5. A temperature swing adsorption gas purification process is characterized in that: the method comprises a vacuum negative pressure regeneration process and a variable temperature flushing regeneration process, wherein the vacuum negative pressure regeneration process comprises the following steps:
adsorption: the raw material gas enters an adsorption tower (9) through a first program control valve (V1A), impurity components in the raw material gas are sequentially adsorbed by a plurality of adsorbents filled in the adsorption tower (9), the obtained purified product gas is discharged through a second program control valve (V2A), and along with the adsorption, when the front edge of impurities rises to be close to the height of an adsorption bed, the first program control valve (V1A) and the second program control valve (V2A) are closed to stop the adsorption;
reverse playing: after the adsorption process is finished, the adsorption front of the adsorption tower (9) basically reaches the outlet of the bed layer, at the moment, a fifth program control valve (V5A) is opened, the pressure of the adsorption tower (9) is reduced to normal pressure against the adsorption direction, at the moment, a small part of adsorbed impurity components begin to be desorbed from the adsorbent, the reversely desorbed gas enters a regeneration liquid separation tank after being regulated by a pressure reduction regulating valve (V11), and then enters a gas pipe network along with the vacuum desorbed gas;
thirdly, vacuum negative pressure regeneration: after the reverse release is finished, opening a sixth program control valve (V6A), and performing vacuum-pumping desorption on the adsorption bed layer by using a regenerative vacuum pump, wherein impurities adsorbed by the adsorbent are desorbed under negative pressure to complete the regeneration of the adsorbent, and the vacuum regenerated gas passes through a regeneration liquid separation tank and then enters a gas pipe network together with the reverse release desorbed gas;
fourthly, boosting pressure: after the vacuum negative pressure desorption is finished, opening a third program control valve (V3A), slowly boosting the purified product gas to the adsorption pressure by a boosting regulating valve (V10) against the adsorption direction, and then, switching the adsorption tower to the next adsorption process;
the adsorption and regeneration processes of a plurality of adsorption towers (9) are alternately carried out, so that the continuous purification of the feed gas can be realized;
the temperature-changing flushing regeneration process comprises the following steps:
cutting off the adsorption tower: after the adsorption tower (9) completes negative pressure regeneration, the adsorption tower (9) is cut off through a control system, so that the adsorption tower (9) is isolated from other adsorption towers in the system, preparation is made for temperature-changing flushing regeneration, and at the moment, the other adsorption towers except the adsorption tower (9) still run in a vacuum negative pressure regeneration mode;
sixthly, high-temperature washing regeneration: opening a ninth program control valve (V9), a fourth program control valve (V4A) and a seventh program control valve (V7A), heating the regenerated gas from the outside of the battery compartment to about 240 ℃ by a regeneration heater, then passing through the adsorption tower from top to bottom, flushing the bed layer of the adsorption tower to the required temperature at high temperature, and flushing the desorption gas at high temperature to enter a flare gas pipe network;
seventhly, constant-temperature flushing regeneration: when the outlet temperature of the adsorption tower for high-temperature washing regeneration reaches the required temperature, continuously keeping the higher-temperature washing process for fully regenerating the adsorbent, namely constant-temperature washing;
low-temperature washing and regeneration: after the constant-temperature flushing is finished, starting to perform low-temperature flushing on the adsorption tower, closing the ninth program-controlled valve (V9), opening the eighth program-controlled valve (V8), the fourth program-controlled valve (V4A) and the seventh program-controlled valve (V7A), enabling low-temperature flushing gas with the temperature of less than or equal to 40 ℃ to enter the adsorption tower from top to bottom, performing low-temperature flushing on a bed layer of the adsorption tower to the required temperature, and enabling regenerated desorption gas to enter a flare gas pipe network;
ninthly, investment into an adsorption tower: and after the low-temperature flushing regeneration is finished, all the program control valves connected with the adsorption tower (9) are closed, and the adsorption tower (9) is put into operation by the control system, so that the adsorption tower (9) finishes a temperature-changing flushing regeneration process.
6. The temperature swing adsorption gas purification process according to claim 5, wherein: in the second step, when the adsorption pressure is lower or the regeneration pressure is close to the adsorption pressure, the second step is not needed.
7. The temperature swing adsorption gas purification process according to claim 5 or 6, wherein: and in the step (iv), when the step (iv) is not available, the process step (iv) is not required.
8. The temperature swing adsorption gas purification process according to claim 5, wherein: and sixthly, flushing and regenerating at high temperature, keeping the temperature of gas at the regeneration outlet of the adsorption tower at 40 ℃ at the beginning, and ending the step when the temperature is gradually and slowly increased to be more than or equal to 150 ℃.
9. The temperature swing adsorption gas purification process according to claim 5, wherein: the constant temperature flushing regeneration in the step is controlled at 150 ℃ and 220 ℃ according to different constant temperature temperatures of desorption substances.
10. The temperature swing adsorption gas purification process according to claim 5, wherein: and (6) low-temperature flushing regeneration is carried out in the step (b), the temperature of the gas at the regeneration outlet of the adsorption tower is basically maintained to be more than or equal to 150 ℃ in the initial stage, and the step (b) is finished when the temperature is gradually and slowly reduced to be less than or equal to 45 ℃.
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