CN107344058B - Energy-saving hydrogen chloride gas deep purification process - Google Patents
Energy-saving hydrogen chloride gas deep purification process Download PDFInfo
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- CN107344058B CN107344058B CN201710804294.7A CN201710804294A CN107344058B CN 107344058 B CN107344058 B CN 107344058B CN 201710804294 A CN201710804294 A CN 201710804294A CN 107344058 B CN107344058 B CN 107344058B
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Abstract
The invention discloses an energy-saving hydrogen chloride gas deep purification process which comprises the processes of adsorption, sequential discharge, reverse discharge, heating regeneration, cold blowing, pressurizing and the like. Three purifying towers are adopted in the process, and the three purifying towers are in different processes of adsorption, heating regeneration, cold blowing and the like. In order to improve the purification effect, the raw material gas, cold blowing gas and a regenerator are all condensed by adopting frozen brine, so that the impurity content in the raw material gas and the circulating gas returned to the inlet of a compressor is reduced as far as possible, the requirement of deep purification is met, the impurity content in the product gas is reduced to 50PPm from the original 250PPm, meanwhile, in order to improve the single-pass yield of the product gas, the energy consumption generated by the gas returned to a system is reduced, a forward pressure reducing step is arranged before the heating and regeneration of a purification tower, and meanwhile, the cold blowing gas is directly used for heating and is used as the regenerated gas, so that the gas circulation quantity is reduced, the single-pass yield is improved, and the energy consumption is greatly reduced.
Description
Technical Field
The invention belongs to the field of gas purification, and particularly relates to an energy-saving hydrogen chloride gas deep purification process.
Background
The prior art discloses a gas impurity removal process, which comprises adsorption, thermal regeneration and cold blowing processes, wherein a plurality of adsorption towers are used in the process, and the adsorption, regeneration and cold blowing processes are alternately performed, so that the continuity of gas purification is realized, and the impurity removal is thorough. In the process, however, after the adsorption is completed, the reverse discharge is directly carried out, part of qualified gas is pressurized and then recycled to the purification system, so that the single-pass yield of the product is reduced, the energy consumption is increased, the adsorption is carried out by temperature swing adsorption alone, the impurity removal depth is insufficient, and the product purity is not high enough.
Disclosure of Invention
Aiming at the defects in the prior art, the invention aims to solve the technical problems of insufficient impurity removal depth in gas, insufficient product purity, overlarge recycle quantity of regenerated gas and low single-pass yield of the product.
In order to achieve the above purpose, the technical scheme adopted by the invention is as follows: the energy-saving hydrogen chloride gas deep purification process comprises the following specific steps (S103A adsorption is adopted as an example):
(1) Adsorption: after the raw material gas is pressurized to 0.5-0.6 Mpa, cooling by a condenser S108, and then entering a gas-liquid separator S102 for gas-liquid separation; the gas part enters a purification tower S103A at the temperature of-10 to 0 ℃, and impurities in the raw material gas are adsorbed by an adsorbent filled in the tower; pure hydrogen chloride gas flows out from the top of the tower and is sent out of the boundary region through a PV valve;
(2) Forward and reverse releasing and depressurization: after the adsorption of the purifying tower S103A is finished, automatically switching a valve to the purifying tower S103B for adsorption, and enabling the tower S103A to enter a desorption process; firstly, putting gas with pressure higher than pressure at the downstream of a PV valve in a tower into a product gas pipeline along an adsorption direction, and then reversely putting the rest gas into a condenser S106 against the adsorption direction, and reducing the pressure in a purifying tower S103A to normal pressure; at this time, the purification column S103C is in a cold blowing stage;
(3) And (3) heating and regenerating: the cold blowing gas from the top of the purification tower S103C is heated into regenerated gas by a heater S105, and then enters a purification tower S103A which needs to be regenerated in the opposite direction of adsorption, and adsorbed components are desorbed; the desorption gas enters a condenser S106 from the bottom of a purification tower S103A to be cooled, then enters a regeneration separator S107 to carry out gas-liquid separation, and the separated gas returns to the inlet of a raw gas compressor S101; after heating and regenerating, the purification tower S103A enters a cold blowing stage;
(4) And (3) cold blowing: introducing a part of product gas from a product gas pipeline, cooling the product gas into cold blowing gas through a condenser S104, and then entering a purification tower S103A needing cold blowing along the adsorption direction until the adsorbent in the purification tower is cooled to normal temperature; the cold blown gas is used as the gas source of the next purifying tower needing to be heated and regenerated;
(5) Pressurizing: after the cold blowing is finished, introducing product gas into the purification tower S103A, and enabling the pressure in the tower to reach the adsorption pressure of 0.5-0.6 Mpa; at this time, the purification tower S103A completes the whole desorption process and enters a standby stage;
(6) And (5) repeating the steps (1) - (5), and continuously purifying the raw material gas into qualified product gas.
The beneficial effects of the invention are as follows: the raw material gas is pressurized to 0.5-0.6 Mpa and then enters the adsorption tower, so that the adsorption capacity of the adsorbent is increased under the condition of pressurization, and the adsorption effect is better. Before entering an adsorption tower, the raw material gas firstly passes through a condenser, part of impurities in the raw material gas are condensed and liquefied, and then are separated by a gas-liquid separator, so that the impurities in the raw material gas are reduced; and after condensation, the temperature of the raw material gas is reduced to-10 to 0 ℃, impurities are more easily adsorbed by the adsorbent, the product gas is deeply purified, and the purity of the product gas is higher.
The technical scheme is provided with forward and reverse playing steps, and the beneficial effects of adopting the technical scheme are as follows: the gas with the pressure higher than the downstream of the PV valve in the purification tower enters a product gas pipeline along the adsorption direction, the single-pass yield of the product gas is improved, the amount of the gas returned to the inlet of the compressor is reduced, and the energy consumption of the compressor can be reduced while the load of the compressor is reduced; during reverse discharge, the residual gas in the purifying tower returns to the inlet of the compressor, and is sent to the purifying tower for purification after being boosted by the compressor, so that no gas is discharged, the useful gas is saved, the gas yield is greatly improved, and the environmental pollution is avoided. In addition, after the forward and reverse discharge steps, the pressure in the purifying tower is reduced to normal pressure, and after the heated regenerated gas is introduced, the impurity components can be quickly and completely desorbed, the regeneration degree is high, and the purity of the obtained product gas is improved when the product gas is put into the adsorption process again.
The adsorption capacity of the adsorbent decreases with increasing temperature. During regeneration, the heated regenerated gas is introduced into the purification tower against the adsorption direction, the adsorbed components are fully desorbed, and the adsorbent is fully regenerated; the regenerated gas is condensed and separated from gas and liquid, and then returned to the inlet of the compressor, and the gas circulates in the whole device and is not discharged, so that the gas yield of the product is improved, and the environmental pollution is avoided. And the desorbed gas passes through a regenerated gas condenser and a gas-liquid separator taking frozen brine as a refrigerant in the process of returning to the inlet of the compressor, so that impurity components in the gas are completely separated, and the gas purification depth is deep.
After regeneration is completed, part of product gas is introduced into the purifying tower, the pressure in the tower is raised to the adsorption pressure, and the adsorbent is ensured to have stronger adsorption capacity.
The adsorption, heating regeneration and cold blowing processes are carried out among the three purification towers at the same time, and the adsorption, regeneration and cold blowing processes are alternately carried out in the three purification towers according to the time sequence, so that the gas quantity for regeneration is reduced, the compression quantity of a compressor is reduced, and the energy consumption is greatly reduced.
Further, the specific flow direction of the gas is as follows: the raw material gas enters from the bottom of a purification tower for adsorption process, and adsorption purification is carried out in the tower; a part of purified product gas from the top of the adsorption purification tower enters a condenser S104 from a product pipeline 6 through a program-controlled valve V10, is cooled by the condenser S104 and becomes cold blowing, and enters a purification tower needing cold blowing along the adsorption direction through a program-controlled valve V6 until the temperature in the tower is reduced to normal temperature; cold blowing air flows into a pipeline 8 through a program-controlled valve V3 arranged at the top of the tower, enters a heater S105 after passing through a program-controlled valve V9, is heated by the heater S105 to become regenerated gas, the regenerated gas enters a purifying tower to be regenerated in the opposite direction to the adsorption direction after passing through the pipeline 9 and the program-controlled valve V4, and the adsorbed components in the tower enter a condenser S106 through a program-controlled valve V5 after being desorbed, and then enter a regenerating separator S107 for gas-liquid separation; the separated gas is returned to the inlet of the compressor S101 through the pipe 12.
The beneficial effects of adopting the further technical scheme are as follows: the invention carries out cold blowing and regeneration simultaneously. The gas from the condenser S104 enters one of the purifying towers needing cold blowing and then enters the heater for heating, and then enters the purifying tower needing heating and desorption, so that the gas used for cold blowing and heating is the same gas, and the energy consumption generated by gas recovery is reduced. The regenerated gas needing to be returned to the inlet of the compressor passes through the regenerated gas condenser and the regenerated gas separator in sequence, so that the impurity content of the gas returned to the inlet of the raw material gas is greatly reduced, and the purity of the product gas is greatly improved.
Further, the condensing medium in the condenser S104, the condenser S106 and the condenser S108 is chilled brine.
The beneficial effects of adopting above-mentioned technical scheme are: the condensing medium in the condenser S104, the condenser S106 and the condenser S108 is chilled brine, so that the gas in the pipeline can be cooled to a required temperature, and meanwhile, impurities easy to liquefy in the gas can be condensed into liquid, so that the circulation of the impurities in the purifying device is reduced, the purity of the product gas can be improved, and the energy consumption can be reduced.
Further, the temperature of cold blowing is-5 to 0 ℃.
The beneficial effects of adopting the further technical scheme are as follows: the cold blowing at the temperature of 5 ℃ to 0 ℃ reduces the purification tower to be cold blown to a lower temperature, and after the raw material gas in a low-temperature state enters the purification tower, the adsorption rate of the adsorbent to impurities under the low-temperature condition is ensured, and the purity of the product gas is improved.
Further, the temperature of the regenerated gas is 180-230 ℃.
The beneficial effects of adopting the further technical scheme are as follows: the regenerated gas with the temperature of 180-230 ℃ can fully desorb the impurity components adsorbed in the adsorbent, so that the adsorbent in the purifying tower can fully regenerate, and impurities in the raw material gas can be fully adsorbed when entering the subsequent adsorption step, and the purity of the product gas is improved.
Further, the purification column is packed with at least one molecular sieve adsorbent.
The beneficial effects of adopting the further technical scheme are as follows: different molecular sieve adsorbents have different adsorption effects on different impurities, and the scheme can set different adsorbents according to the characteristics of the impurities in the raw material gas, so that the impurities in the raw material gas can be reduced to the minimum, and the high-purity product gas is obtained.
Drawings
FIG. 1 is a piping diagram of the present invention;
Detailed Description
The following describes the embodiments of the present invention in detail with reference to the drawings.
The invention provides an energy-saving hydrogen chloride gas deep purification process which comprises the steps of adsorption, sequential discharge, reverse discharge, heating regeneration, cold blowing, pressurizing and the like. The process uses a plurality of purifying towers which are arranged in parallel; in the invention, three purifying towers are adopted, and adsorption, heating regeneration and cold blowing processes are alternately carried out in the three purifying towers.
The specific process of gas purification comprises the following steps: the raw material gas enters a compressor S101 through a pipeline 1, is pressurized to 0.5-0.6 Mpa, then enters a frozen brine condenser S108 through a pipeline 2 for cooling, and impurity components easy to condense in the raw material gas are liquid and are subjected to gas-liquid separation in a gas-liquid separator S102. The temperature of the raw material gas coming out of the top of the gas-liquid separator S102 is-10-0 ℃, and the raw material gas enters the purification tower S103A for adsorption through the pipelines 3 and 4 from the program-controlled valve V1a arranged at the bottom of the purification tower. Under the action of the adsorbent in the tower, the impurity components are adsorbed, and pure hydrogen chloride product gas flows into the product gas pipeline 6 through the programmable valve V2a at the top of the tower and is sent out from the boundary region under stable pressure after being regulated by the PV valve. After the adsorption saturation of the adsorbent in the column, the adsorption process is carried out by transferring the adsorbent to the purification column S103B by an automatic control program. The purification tower S103A enters a regeneration process, firstly, gas with pressure higher than that of the downstream of the PV valve in the purification tower S103A is placed into a product gas pipeline 7 through a program-controlled valve V8 along the adsorption direction, so that the single-pass yield of the product gas is improved, the gas quantity returned to a compressor is reduced, the energy consumption is reduced, then, the residual gas in the tower is cooled through a condenser S106 through a program-controlled valve V5a against the adsorption direction, and liquefied impurity components are separated through a regeneration separator S107, and the gas returns to the inlet of the compressor S101 through a pipeline 12 so as to recover regenerated gas, improve the total yield and avoid environmental pollution; liquefied impurities at the bottom of the gas-liquid separator are collected and recycled. After the sequential releasing and reversing steps, the pressure in the purifying tower S103A is reduced to normal pressure, and then the heating regeneration gas is introduced to heat and regenerate the adsorbent in the purifying tower S103A.
In order to enhance the condensing effect and reduce the impurity content in the return gas, the regenerated gas cooler S106 is filled with a refrigerant with better condensing effect, and the invention adopts frozen brine preferentially. Meanwhile, according to different components of impurities in the raw material gas, at least one molecular sieve adsorbent is filled in the purifying tower, and the molecular sieve adsorbent is selected from the following components: activated carbon, clay, perlite, vermiculite, zeolite, or the like. When the purification column S103A performs adsorption, a cold blowing process is performed in the purification column S103B. The cold blow gas is from the product gas. Part of the product gas flows into a condenser S104 filled with frozen brine from a cold air blowing pipeline 10 connected with a product gas pipeline 6, is cooled to-5-0 ℃ through the condenser S104, enters a purification tower S103B along the adsorption direction through a program-controlled valve V6B, and is subjected to cooling treatment until the temperature of the adsorbent is reduced to the optimal adsorption temperature. Cold blowing gas from the purifying tower S103B enters the pipeline 8 through the program-controlled valve V3B, then enters the heater S105 through the program-controlled valve V9, and is heated to 180-230 ℃ through the heater S105 to become heated regenerated gas. The heated regenerated gas enters the purification tower S103C through the program-controlled valve V4C in the opposite direction to the adsorption direction, the adsorbent in the purification tower S103C is heated and regenerated, and the impurity components adsorbed on the adsorbent are desorbed. The gas flows into the regenerated gas cooler S106 through the program-controlled valve V5c, impurities are condensed, the impurities enter the regenerated gas separator S107 for gas-liquid separation, and the gas returns to the inlet of the compressor S101 through the pipeline 12. So far, the purification tower S103B completes the cold blowing process, the adsorption process is transferred from the purification tower S103A to S103B through an automatic control program, the purification tower S103C enters the cold blowing process, and the purification tower S103A enters the heating regeneration process. And the like, adsorption, heating regeneration and cold blowing processes are alternately carried out in the three purifying towers.
(1) Embodiment one:
taking 10m 3 Wherein the main chlorohydrocarbons content: and (3) pressurizing to 5.0% by a compressor to 0.5Mpa, cooling to-10 ℃ by a condenser taking chilled brine as a refrigerant, separating liquefied chlorinated hydrocarbon liquid by a gas-liquid separator, allowing gas to enter from the bottom of a purification tower S103A (three purification towers are arranged), adsorbing chlorinated hydrocarbon in the gas by an adsorbent, sending the purified chlorinated hydrocarbon product gas out of a boundary region at a stable pressure through a pipeline 7, allowing the rest of the product gas to enter a condenser S104 through a program-controlled valve V10 for cooling, cooling to-5 ℃, and then entering the purification tower S103B along the adsorption direction for cold blowing the purification tower S103B. Cold blowing air flows out from a program-controlled valve V3b arranged at the top of the tower and enters a heater S105, gas is heated to about 200 ℃ and then enters a purification tower S103C against the adsorption direction, and the adsorbent in the purification tower S103C is subjected to heating regeneration treatment. The gas desorbed from the adsorbent after heating and regeneration enters a regenerated gas condenser S106 from the bottom of the tower through a program-controlled valve V5c, impurities in the gas are cooled and condensed through frozen brine and then enter a regeneration separator S107, and the cooled chlorine is separated through a gas-liquid separatorThe hydrocarbon liquid is separated and the gas is returned to the inlet of the compressor via conduit 12. After the adsorbent in the purification tower S103A is adsorbed and saturated, the adsorption process is transferred to the purification tower S103B for carrying out, the purification tower S103A puts the gas with the pressure higher than the pressure at the lower stream of the PV valve into the product gas pipeline 7 along the adsorption direction, then the rest gas is put into the regenerated gas condenser S106 against the adsorption direction, and the cooled liquid is separated by the regenerated gas separator S107 and then returned to the inlet of the compressor; after the pressure of the purification tower S103A is reduced to normal pressure, the purification tower S103A enters a heating regeneration process, and at the moment, cold blowing and pressurizing processes are carried out in the purification tower S103C. The purification tower S103A, the purification tower S103B and the purification tower S103C alternately circulate to perform adsorption, heating regeneration and cold blowing processes, and the working processes are as follows:
(2) Comparative example one:
taking 10m 3 Wherein the main chlorohydrocarbons content: and (3) pressurizing to 0.0% by using a compressor to 0.5Mpa, cooling to-10 ℃ by using a condenser taking chilled brine as a refrigerant, separating the cooled chlorinated hydrocarbon liquid by using a gas-liquid separator, enabling gas to enter a purification tower S103A from the bottom of the purification tower S103A (two purification towers are arranged), sending the pressure of chlorinated hydrocarbon impurities in the gas out of a boundary region, automatically controlling and switching a program after the adsorbent in the purification tower S103A is saturated, transferring the adsorption process from the tower S103A to the tower S103B, and enabling the tower S103A to enter a regeneration process. That is, part of gas is introduced from a product gas pipeline and enters a heater S105, the gas is heated to 200 ℃ and then enters a purification tower S103A against the adsorption direction, impurity gas adsorbed by an adsorbent in the purification tower S103A is desorbed under the condition of high temperature, the gas enters a regenerated gas condenser S106 from a program-controlled valve V5a at the bottom of the tower, the temperature is reduced, and the gas returns to the inlet of a compressor for recycling through a pipeline 12 after passing through a regenerated separator. Until the desorption of the adsorbent in the purification tower S103A is completed, introducing part of gas from the product gas pipeline, and cooling to 35 ℃ by entering a cooler S104 taking circulating cooling water as a refrigerant through a program-controlled valve V10Then, the gas enters the purification column S103A against the adsorption direction, and cold blowing is performed on the purification column S103A. Cold blowing air flows out from the bottom of the tower through a program control valve V3a and then enters a cold blowing air condenser S106 taking circulating cooling water as a refrigerant, after being cooled, enters a regeneration air separator S107, after the cooled liquid substances are removed, the air returns to the inlet of the compressor through a pipeline 12 for recycling; after the temperature of the cooling tower is reduced to normal temperature, the purification tower S103A completes the regeneration process, and the adsorption process is automatically transferred to the purification tower S103A for carrying out through automatic control of a program. The purification tower S103A and the purification tower S103B alternately circulate to perform adsorption, regeneration and cold blowing processes, and the working processes are as follows:
analysis of results:
as can be seen from the analysis of the results, the invention simultaneously carries out cold blowing and heating regeneration by cooling the raw material gas, cold blowing and regenerated gas by freezing and adding one tower, and after the forward and reverse pressure release steps are added, the impurity content in the product gas is greatly reduced, the impurity content is reduced from the original 250PPm to 50PPm, the energy consumption of the recovered gas is also greatly reduced, and the power is reduced by 55.36 percent. In addition, because the raw material gas is subjected to pressurization and cooling treatment before entering the purification tower, impurity components in the raw material gas can be adsorbed more rapidly, the time spent in the whole process is shorter, and the time for purifying operation is shortened.
Based on the technical scheme, the invention can also be improved as follows: if the gas amount is increased, the number of towers can be increased to reduce the space velocity of purification, such as one tower adsorption is increased to two towers or three towers adsorption; the pressure of pressurization in this example may employ different adsorption pressures depending on the gas; the temperature of the frozen brine can be different according to the dew point temperature of the impurity content in the gas.
Although specific embodiments of the invention have been described in detail with reference to the accompanying drawings, it should not be construed as limiting the scope of protection of the present patent. Various modifications and variations which may be made by those skilled in the art without the creative effort are within the scope of the patent described in the claims.
Claims (6)
1. An energy-saving hydrogen chloride gas deep purification process is characterized in that: the method comprises the following specific steps:
(1) Adsorption: after the raw material gas is pressurized to 0.5-0.6 Mpa, cooling by a condenser S108, and then entering a gas-liquid separator S102 for gas-liquid separation; the gas part enters a purification tower S103A at the temperature of-10 to 0 ℃, and impurities in the raw material gas are adsorbed by an adsorbent filled in the tower; pure hydrogen chloride gas flows out from the top of the tower and is sent out of the boundary region through a PV valve;
(2) Forward and reverse releasing and depressurization: after the adsorption of the purification tower S103A is finished, automatically switching a valve to the purification tower S103B for adsorption, and allowing the purification tower S103A to enter a desorption process; firstly, putting gas with pressure higher than pressure at the downstream of a PV valve in a tower into a product gas pipeline along an adsorption direction, and then reversely putting the rest gas into a condenser S106 against the adsorption direction, and reducing the pressure in a purifying tower S103A to normal pressure; at this time, the purification column S103C is in a cold blowing stage;
(3) And (3) heating and regenerating: the cold blowing gas from the top of the purification tower S103C is heated into regenerated gas by a heater S105, and then enters a purification tower S103A which needs to be regenerated in the opposite direction of adsorption, and adsorbed components are desorbed; the desorption gas enters a condenser S106 from the bottom of a purification tower S103A to be cooled, then enters a regeneration separator S107 to carry out gas-liquid separation, and the separated gas returns to the inlet of a raw gas compressor S101; after heating and regenerating, the purification tower S103A enters a cold blowing stage;
(4) And (3) cold blowing: introducing a part of product gas from a product gas pipeline, cooling the product gas into cold blowing gas through a condenser S104, and then entering a purification tower S103A needing cold blowing along the adsorption direction until the adsorbent in the purification tower is cooled to normal temperature; the cold blown gas is used as the gas source of the next purifying tower needing to be heated and regenerated;
(5) Pressurizing: after the cold blowing is finished, introducing product gas into the purification tower S103A, and enabling the pressure in the tower to reach the adsorption pressure of 0.5-0.6 Mpa; at this time, the purification tower S103A completes the whole desorption process and enters a standby stage;
(6) And (5) repeating the steps (1) - (5), and continuously purifying the raw material gas into qualified product gas.
2. The energy-saving hydrogen chloride gas deep purification process according to claim 1, characterized in that: the specific flow direction of the gas is as follows: the raw material gas enters from the bottom of a purification tower for adsorption process, and adsorption purification is carried out in the tower; a part of purified product gas from the top of the adsorption purification tower enters a condenser S104 from a product pipeline 6 through a program-controlled valve V10, is cooled by the condenser S104 and becomes cold blowing, and enters a purification tower needing cold blowing along the adsorption direction through a program-controlled valve V6 until the temperature in the tower is reduced to normal temperature; cold blowing air flows into a pipeline 8 through a program-controlled valve V3 arranged at the top of the tower, enters a heater S105 after passing through a program-controlled valve V9, is heated by the heater S105 to become regenerated gas, the regenerated gas enters a purifying tower to be regenerated in the opposite direction to the adsorption direction after passing through the pipeline 9 and the program-controlled valve V4, and the adsorbed components in the tower enter a condenser S106 through a program-controlled valve V5 after being desorbed, and then enter a regenerating separator S107 for gas-liquid separation; the separated gas is returned to the inlet of the compressor S101 through the pipe 12.
3. An energy-saving hydrogen chloride gas deep purification process according to claim 1 or 2, characterized in that: the condensing medium in the condenser S104, the condenser S106 and the condenser S108 is chilled brine.
4. An energy-saving hydrogen chloride gas deep purification process according to claim 1 or 2, characterized in that: the temperature of cold blowing is-5-0 ℃.
5. An energy-saving hydrogen chloride gas deep purification process according to claim 1 or 2, characterized in that: the temperature of the regenerated gas is 180-230 ℃.
6. The energy-saving hydrogen chloride gas deep purification process according to claim 1, characterized in that: the purification column is packed with at least one molecular sieve adsorbent.
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