CN219839665U - Resource utilization system for ammonia in low-temperature methanol washing acid process gas - Google Patents
Resource utilization system for ammonia in low-temperature methanol washing acid process gas Download PDFInfo
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- CN219839665U CN219839665U CN202320954559.2U CN202320954559U CN219839665U CN 219839665 U CN219839665 U CN 219839665U CN 202320954559 U CN202320954559 U CN 202320954559U CN 219839665 U CN219839665 U CN 219839665U
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- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 title claims abstract description 120
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 title claims abstract description 81
- 239000002253 acid Substances 0.000 title claims abstract description 64
- 229910021529 ammonia Inorganic materials 0.000 title claims abstract description 40
- 238000000034 method Methods 0.000 title claims abstract description 36
- 238000005406 washing Methods 0.000 title claims abstract description 25
- 238000010521 absorption reaction Methods 0.000 claims abstract description 43
- 238000002425 crystallisation Methods 0.000 claims abstract description 25
- 230000008025 crystallization Effects 0.000 claims abstract description 25
- 238000004064 recycling Methods 0.000 claims abstract description 21
- 238000000926 separation method Methods 0.000 claims abstract description 19
- 238000005496 tempering Methods 0.000 claims abstract description 10
- 238000011084 recovery Methods 0.000 claims abstract description 8
- 230000001105 regulatory effect Effects 0.000 claims abstract description 5
- 239000007789 gas Substances 0.000 claims description 116
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 58
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 43
- 229910052757 nitrogen Inorganic materials 0.000 claims description 31
- 238000004140 cleaning Methods 0.000 claims description 13
- 230000002378 acidificating effect Effects 0.000 claims description 5
- 238000005201 scrubbing Methods 0.000 claims 2
- -1 amino compound Chemical class 0.000 abstract description 20
- 239000012535 impurity Substances 0.000 abstract description 5
- 239000006096 absorbing agent Substances 0.000 abstract description 2
- 230000008929 regeneration Effects 0.000 description 11
- 238000011069 regeneration method Methods 0.000 description 11
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 description 8
- 239000013078 crystal Substances 0.000 description 8
- 230000000694 effects Effects 0.000 description 8
- 239000012071 phase Substances 0.000 description 8
- 235000011114 ammonium hydroxide Nutrition 0.000 description 7
- 239000002994 raw material Substances 0.000 description 7
- 229920006395 saturated elastomer Polymers 0.000 description 7
- 239000007788 liquid Substances 0.000 description 6
- 230000001276 controlling effect Effects 0.000 description 4
- 125000002924 primary amino group Chemical group [H]N([H])* 0.000 description 4
- 239000007787 solid Substances 0.000 description 4
- LRDIEHDJWYRVPT-UHFFFAOYSA-N 4-amino-5-hydroxynaphthalene-1-sulfonic acid Chemical compound C1=CC(O)=C2C(N)=CC=C(S(O)(=O)=O)C2=C1 LRDIEHDJWYRVPT-UHFFFAOYSA-N 0.000 description 3
- ATRRKUHOCOJYRX-UHFFFAOYSA-N Ammonium bicarbonate Chemical compound [NH4+].OC([O-])=O ATRRKUHOCOJYRX-UHFFFAOYSA-N 0.000 description 3
- 229910000013 Ammonium bicarbonate Inorganic materials 0.000 description 3
- MKKVKFWHNPAATH-UHFFFAOYSA-N [C].N Chemical compound [C].N MKKVKFWHNPAATH-UHFFFAOYSA-N 0.000 description 3
- 235000012538 ammonium bicarbonate Nutrition 0.000 description 3
- 239000001099 ammonium carbonate Substances 0.000 description 3
- 238000001704 evaporation Methods 0.000 description 3
- 230000008020 evaporation Effects 0.000 description 3
- 238000011010 flushing procedure Methods 0.000 description 3
- 125000001741 organic sulfur group Chemical group 0.000 description 3
- 230000001737 promoting effect Effects 0.000 description 3
- 238000010926 purge Methods 0.000 description 3
- 238000003756 stirring Methods 0.000 description 3
- RWSOTUBLDIXVET-UHFFFAOYSA-N Dihydrogen sulfide Chemical compound S RWSOTUBLDIXVET-UHFFFAOYSA-N 0.000 description 2
- 238000009825 accumulation Methods 0.000 description 2
- CBHOOMGKXCMKIR-UHFFFAOYSA-N azane;methanol Chemical compound N.OC CBHOOMGKXCMKIR-UHFFFAOYSA-N 0.000 description 2
- 238000000354 decomposition reaction Methods 0.000 description 2
- 238000004090 dissolution Methods 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 229910052739 hydrogen Inorganic materials 0.000 description 2
- 229910000037 hydrogen sulfide Inorganic materials 0.000 description 2
- 239000002184 metal Substances 0.000 description 2
- 229910052751 metal Inorganic materials 0.000 description 2
- 230000000630 rising effect Effects 0.000 description 2
- 230000015572 biosynthetic process Effects 0.000 description 1
- 238000003889 chemical engineering Methods 0.000 description 1
- 238000012824 chemical production Methods 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 239000003034 coal gas Substances 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000011033 desalting Methods 0.000 description 1
- 230000018109 developmental process Effects 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 238000010790 dilution Methods 0.000 description 1
- 239000012895 dilution Substances 0.000 description 1
- 238000007599 discharging Methods 0.000 description 1
- 239000003344 environmental pollutant Substances 0.000 description 1
- 238000003912 environmental pollution Methods 0.000 description 1
- 238000001914 filtration Methods 0.000 description 1
- 230000001788 irregular Effects 0.000 description 1
- 238000012423 maintenance Methods 0.000 description 1
- 231100000719 pollutant Toxicity 0.000 description 1
- 238000010992 reflux Methods 0.000 description 1
- 239000007790 solid phase Substances 0.000 description 1
- 239000007921 spray Substances 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
- 238000005979 thermal decomposition reaction Methods 0.000 description 1
Abstract
The utility model discloses a recycling system for ammonia in low-temperature methanol washing acid process gas, which comprises a crystallization system, a tempering and absorbing system and a separation system; the crystallization system comprises a crystallizer; the bottom of the crystallizer is connected with an acid gas input pipeline; an inlet valve group comprising a ball valve and a pneumatic regulating valve is arranged at one end of the acid gas input pipeline, which is close to the crystallizer; the heat recovery and absorption system comprises a heat exchanger and an absorption tank; the separation system comprises an outgoing pipeline connected with the absorption tank and a vacuum pump, and an air outlet of the vacuum pump is connected with an acid gas flare gas-phase pipeline; the separation system further includes a heat trace system coupled to the absorber tank. According to the system provided by the utility model, the impurity ammonia in the acid gas is collected and separated, and the impurity ammonia in the acid gas is recycled through process design and combination, so that the ammonia recovery rate is improved; by adopting two crystallizers, continuous operation of amino compound resource utilization in the low-temperature methanol washing process is realized.
Description
Technical Field
The utility model belongs to the technical field of chemical engineering, relates to a low-temperature methanol washing process system, and particularly relates to a recycling system for ammonia in low-temperature methanol washing acidic process gas.
Background
In the chemical production process starting from coal gas, the synthesis gas is passed through a conversion device and H contained therein 2 S、COS、CO 2 The acid gas is removed by low-temperature methanol eluting process. In order to reduce the consumption of methanol, the low-temperature methanol washing process adopts a methanol recycling mode, so that the original trace NH in the system is realized 3 Gradually enriching. NH after enrichment 3 With H in methanol 2 S、COS、CO 2 And acid gases react to form amino compound crystals in the system, so that the safety and stable operation of equipment are seriously affected.
The main technical route of the current method for eliminating amino compounds comprises the following steps: 1. and (3) thermal decomposition: the temperature of the system is raised by heat exchange to decompose amino compounds into acid gas and NH 3 And (5) discharging. The method does not realize acid gas and NH 3 The gas is recrystallized in the acid gas torch, and a great potential safety hazard exists. 2. Replacement methanol process: the low-temperature methanol washing system is supplemented with methanol at irregular intervals to play a role of NH 3 Concentration dilution effect, NH in control system 3 The process is costly to operate.
In recent years, the control technology of amino compound crystallization in the low-temperature methanol washing process has attracted much interest of researchers, and the regulation measures include: reducing stripping/CO 2 H of concentration section of desorber 2 S amount; periodically analyzing the liquid ammonia content of the acid gas separator; ensuring the filtering effect of the lean methanol filter; lean methanol ammonia content is analyzed periodically, etc.
Chinese patent CN114887456A relates to a scheme for preventing carbon ammonia crystallization in a low-temperature methanol washing process, which adopts a two-stage acid gas separating tank, cools the first-stage outlet gas, heats the second-stage outlet gas, and causes the carbon ammonia crystallization to decompose, thereby achieving the purpose of decomposing the carbon ammonia crystallization.
CN205874328U discloses a device for preventing accumulation of ammonia and organic sulfur in a low-temperature methanol washing system and eliminating crystallization of ammonium bicarbonate of equipment, a small amount of reflux liquid of a thermal regeneration tower rich in organic sulfur is used as spray methanol of a hydrogen sulfide rich gas condenser, the accumulation of system ammonia and organic sulfur is solved by using the minimum amount of methanol, excessive burden on a pre-washing methanol regeneration system is avoided, and the crystallization problem of ammonium bicarbonate of equipment is solved.
CN104140852a discloses a device and method for treating low-temperature methanol ammonium washing crystallization and purifying lean methanol. The device and the method adopt a normal-temperature water washing mode to solve the problem that a condenser and a pipeline at the top of a thermal regeneration tower are blocked due to ammonium bicarbonate crystallization in the traditional flow, and solve the problem of intermittent pollution discharge methanol treatment at the same time, thereby purifying lean methanol and reducing methanol consumption.
Along with the development of control technology of amino compound crystallization and the continuous reuse of low-temperature methanol washing methanol, NH in the methanol 3 The content is continuously enriched, and the demand for techniques for controlling the crystallization of amino compounds is gradually increasing.
Disclosure of Invention
Aiming at the defects of the prior art, the utility model provides a recycling system for ammonia in low-temperature methanol washing acid process gas, which can realize the efficient utilization of ammonia resources in amino compounds in the low-temperature methanol washing process, and the recovery rate of enriched ammonia in the system reaches 90-95%.
A recycling system for ammonia in low-temperature methanol washing acid process gas comprises a crystallization system, a tempering and absorbing system and a separation system;
the crystallization system comprises a crystallizer; the bottom of the crystallizer is connected with an acid gas input pipeline; an inlet valve group comprising a ball valve and a pneumatic regulating valve is arranged at one end of the acid gas input pipeline, which is close to the crystallizer;
the heat recovery and absorption system comprises a heat exchanger and an absorption tank, wherein a shell side inlet of the heat exchanger is connected with a low-pressure nitrogen input pipeline, and a shell side outlet of the heat exchanger is connected with a low-pressure nitrogen output pipeline; the other end of the low-pressure nitrogen output pipeline is also connected with the top of the crystallizer and the middle of an inlet valve group on the acid gas input pipeline; a rewarming pipeline is connected between the absorption tank and the top of the crystallizer, and extends into the absorption tank; a cleaning water pipeline is connected between the bottom of the crystallizer and the top of the absorption tank; the tempering and absorbing system further comprises a desalted water pipeline which is connected with the bottom of the crystallizer;
the separation system comprises an outgoing pipeline connected with the absorption tank and a vacuum pump, and an air outlet of the vacuum pump is connected with an acid gas flare gas-phase pipeline; the separation system further includes a heat trace system coupled to the absorber tank.
Preferably, two crystallizers are provided, including a first crystallizer and a second crystallizer connected in parallel.
Preferably, the recycling system further comprises a circulating pipeline, wherein an inlet of the circulating pipeline is connected with the delivery pipeline, and an outlet of the circulating pipeline is connected with one end, close to the crystallizer, of the desalted water pipeline.
The utility model has the advantages that:
(1) The system provided by the utility model collects and separates the impurity ammonia of the acid washing gas, converts the external exhaust dangerous pollutant into usable resources, avoids the environmental pollution and equipment maintenance and safety accidents caused by ammonia crystallization, recycles the impurity ammonia in the acid gas through process design and combination, improves the ammonia recovery rate, and ensures that the ammonia recovery rate in the system reaches 90-95%;
(2) By adopting two crystallizers, continuous operation of amino compound resource utilization in the low-temperature methanol washing process is realized, and the risk that personnel are exposed to high-concentration hydrogen sulfide environment in the intermittent operation process is avoided.
Drawings
FIG. 1 is a schematic diagram of a system for recycling ammonia in a low temperature methanol wash acid process gas;
reference numerals: 1-a first crystallizer, 2-a second crystallizer, 3-an absorption tank, 4-a heat exchanger, 5-a vacuum pump, 10-an acid gas input pipeline, 20-an acid gas flare gas phase pipeline, 30-a low-pressure nitrogen input pipeline, 40-a low-pressure nitrogen output pipeline, 50-a desalting water pipeline, 60-a cleaning water pipeline, 70-a rewarming pipeline, 80-an outgoing pipeline and 90-a circulating pipeline.
Detailed Description
Example 1
A recycling system for ammonia in low-temperature methanol washing acid process gas comprises a crystallization system, a tempering and absorbing system and a separation system;
the crystallization system comprises a crystallizer; the bottom of the crystallizer is connected with an acid gas input pipeline 10; an inlet valve group comprising a ball valve and a pneumatic regulating valve is arranged at one end, close to the crystallizer, of the acid gas input pipeline 10; a wire mesh is arranged in the crystallizer;
the heat recovery and absorption system comprises a heat exchanger 4 and an absorption tank 3, wherein a shell side inlet of the heat exchanger 4 is connected with a low-pressure nitrogen input pipeline 30, and a shell side outlet of the heat exchanger 4 is connected with a low-pressure nitrogen output pipeline 40; the other end of the low-pressure nitrogen output pipeline 40 is also connected with the top of the crystallizer and the middle of an inlet valve group on the acid gas input pipeline 10; a rewarming pipeline 70 is connected between the absorption tank 3 and the top of the crystallizer, and the rewarming pipeline 70 extends into the absorption tank 3; a cleaning water pipeline 60 is connected between the bottom of the crystallizer and the top of the absorption tank 3; the tempering and absorbing system further comprises a desalted water pipeline 50, wherein the desalted water pipeline 50 is connected with the bottom of the crystallizer;
the separation system comprises an outgoing pipeline 80 and a vacuum pump 5 which are connected with the absorption tank 3, and an acid gas flare gas phase pipeline 20 is connected with the gas outlet of the vacuum pump 5; the separation system further comprises a heat tracing system connected to the absorption tank 3.
The method for recycling ammonia in the low-temperature methanol washing acid process gas by adopting the recycling system comprises the following steps of:
(1) The raw material gas enters a crystallizer through an acid gas input pipeline 10, the dynamic balance is broken through the expansion of the crystallizer, and H contained in the raw material gas 2 S、COS、CO 2 、NH 3 Is mutually reacted to generate solid phase amino compound crystals at low temperature and is arranged in the wire meshApplying; the crystallizer is provided with an automatic control system, a pressure sensor and a differential pressure meter are arranged at the inlet and the outlet of the crystallizer, the automatic control system takes 5kPa as a signal point, the opening of a pneumatic regulating valve in an inlet valve group on an acid gas input pipeline 10 is controlled in an interlocking manner, and the pressure difference of inlet and outlet gas of the crystallizer is kept at 100-160kPa, so that the acid gas is in the state of optimal flow rate and expansion ratio; when the crystallizer is saturated, and air inlet is stopped;
(2) After the crystallizer is saturated, nitrogen enters a heat exchanger 4 through a low-pressure nitrogen input pipeline 30 to exchange heat, the temperature of the nitrogen after heat exchange is more than or equal to 10 ℃, then the nitrogen is discharged from a low-pressure nitrogen output pipeline 40 and enters the crystallizer, a return temperature and purging are carried out on an inlet valve group and the crystallizer, desalted water is prevented from entering low-temperature equipment to freeze, equipment damage is caused, part of amino compound solids are heated and decomposed in the return temperature process, and the amino compound solids enter an absorption tank 3 through a return temperature pipeline 70; when the temperature of the crystallizer is more than or equal to 10 ℃, desalted water enters the crystallizer from a desalted water pipeline 50, nitrogen is kept to be continuously introduced, the effects of stirring liquid and flushing crystallization are achieved, the amino compound crystals are fully dissolved, after 30-60min, a cleaning water pipeline 60 is opened, and the crystals in the crystallizer and the dissolved desalted water are discharged into an absorption tank 3 from the cleaning water pipeline 60; desalted water with one third of the tank volume is stored in the absorption tank 3 in advance to prevent NH in the re-heat gas 3 Escape of (2);
(3) After the cleaning water is discharged into the absorption tank 3, the heat tracing system is started due to heat absorption in the dissolving process, and the temperature in the absorption tank 3 is controlled to be 10-30 ℃ so as to crystallize and decompose the amino compound into NH 4 + 、NH 2 COO - 、HCO 3 - 、CO 3 2- 、S 2- 、HS - Plasma, then starting a vacuum pump 5, controlling the vacuum degree to be 0.03-0.07MPa, changing the balance state of the system, and promoting acid gas CO 2 、H 2 S overflows to realize NH 3 Separation process from acid gas, separated CO 2 、H 2 S acid gas is discharged to acid gas torch gas from an air outlet of a vacuum pump 5 through an acid gas torch gas phase pipeline 20, generated ammonia is dissolved in water to form ammonia water, and the ammonia water is discharged to an ammonia evaporation system through an output pipeline 80, so that ammonia resource utilization is realized。
Example 2
On the basis of example 1, the crystallizer is provided with two, including a first crystallizer 1 and a second crystallizer 2 connected in parallel.
The raw material gas enters the first crystallizer 1 through an acid gas input pipeline 10, and when the first crystallizer 1 is saturated, the air inlet is stopped; opening an inlet valve group connected with the second crystallizer 2 in the acid gas input pipeline 10, and enabling the raw gas to enter the second crystallizer 2 to finish the switching of the first crystallizer 1 and the second crystallizer 2. By arranging two crystallizers, the continuous feeding of the raw material gas can be ensured, so that when the first crystallizer 1 stops feeding, the raw material continuously enters the second crystallizer 2 for continuous crystallization treatment, and the treatment efficiency is improved.
Example 3
On the basis of embodiment 2, the recycling system further comprises a circulation pipeline 90, wherein an inlet of the circulation pipeline 90 is connected with the delivery pipeline 80, and an outlet of the circulation pipeline 90 is connected with one end, close to the crystallizer, of the desalted water pipeline 50.
The circulating pipeline 90 is arranged, so that the consumption of the whole process water can be saved, the unsaturated ammonia water in the early stage of the absorption tank 3 enters the circulating pipeline 90 through the delivery pipeline 80 and then enters the crystallizer, and the consumption of desalted water is saved.
Example 4
In the gas guide process of the low-temperature methanol washing system, the outlet pressure of the thermal regeneration tower has a slow rising trend, the outlet pressure of the thermal regeneration tower reaches 0.37 MPa from 0.227, meanwhile, the acid gas flow is gradually reduced, and H is the gas flow rate 2 S, the temperature of the outlet of the gas-liquid separation tank slowly rises, a vent valve and a bypass are opened on site, the pressure release effect of the thermal regeneration tower is poor, and the system is judged to be blocked by ammonia compounds.
In order to solve the above problems, the recycling system for ammonia in the low-temperature methanol-wash acidic process gas according to embodiment 3 of the present utility model is specifically as follows:
(1) The temperature of the raw material gas is minus 32 ℃, the pressure of the gas is 0.28Mpa, and CO in the gas 2 74.08 content of NH 3 1.73%、CO 0.19%、N 2 1.5%、H 2 S 22.24%；The two crystallizers are arranged and comprise a first crystallizer 1 and a second crystallizer 2 which are connected in parallel; volume flow 976.86m 3 The feed gas of/H enters the first crystallizer 1 through an acid gas input pipeline 10, and H contained in the feed gas at low temperature 2 S、COS、CO 2 、NH 3 The two react with each other to generate amino compound crystals on the built-in metal wire mesh; the crystallizer is provided with an automatic control system, a pressure sensor and a differential pressure meter are arranged at the inlet and the outlet of the crystallizer, the automatic control system takes 5kPa as a signal point, the opening of an inlet valve group on an acid gas input pipeline 10 is controlled in an interlocking manner, the gas pressure difference at the inlet and the outlet of the crystallizer is controlled to be 100-150KPa, and when the first crystallizer 1 is saturated, the air inlet is stopped; the inlet valve group connected with the second crystallizer 2 in the acid gas input pipeline 10 is opened in an interlocking way, and the raw gas enters the second crystallizer 2 to finish the switching of the first crystallizer 1 and the second crystallizer 2;
(2) After any crystallizer is saturated, nitrogen enters a heat exchanger 4 through a low-pressure nitrogen input pipeline 30 to exchange heat, the temperature of the nitrogen after heat exchange is more than or equal to 10 ℃, then the nitrogen is discharged from a low-pressure nitrogen output pipeline 40 and enters the crystallizer, a return temperature and purging are carried out on an inlet valve group and the crystallizer, desalted water is prevented from entering low-temperature equipment to freeze, equipment damage is caused, part of amino compound solids are heated and decomposed in the return temperature process, and gas generated by decomposition enters an absorption tank 3 through a return temperature pipeline 70; when the temperature of the crystallizer is more than or equal to 10 ℃, desalted water enters the crystallizer from a desalted water pipeline 50, nitrogen is kept to be continuously introduced, the effects of stirring liquid and flushing crystallization are achieved, the amino compound crystals are fully dissolved, after 30min, a cleaning water pipeline 60 is opened, and the crystallized and dissolved desalted water in the crystallizer is discharged into an absorption tank 3 from the cleaning water pipeline 60; desalted water with one third of the tank volume is stored in the absorption tank 3 in advance to prevent NH in the re-heat gas 3 Escape of (2);
(3) After the cleaning water is discharged into the absorption tank 3, the heat tracing system is started due to heat absorption in the dissolution process, and the temperature in the absorption tank 3 is controlled to be 25 ℃ so as to crystallize and decompose the dissolved amino compound into NH 4 + 、NH 2 COO - 、HCO 3 - 、CO 3 2- 、S 2- 、HS - Plasma (PDP)Then starting a vacuum pump 5, controlling the vacuum degree to be 0.05MPa, changing the balance state of the system, and promoting the acid gas CO 2 、H 2 S overflows to realize NH 3 Separation process from acid gas, separated CO 2 、H 2 S acid gas is discharged to the acid gas torch gas from the gas outlet of the vacuum pump 5 through the acid gas torch gas phase pipeline 20, the generated ammonia is dissolved in water to form ammonia water, and the ammonia water is discharged to an ammonia evaporation system through the delivery pipeline 80, so that ammonia resource utilization is realized.
After the system runs for 35 hours, NH in methanol at the outlet of the thermal regeneration tower 3 The mass concentration is reduced to 30.19 mg/L, the pH is maintained between 0.015 and 0.030 mol/L and between 8 and 9, and meanwhile, the pressure difference of the whole system is gradually recovered to the normal pressure difference of 0.04 MPa and H 2 The gas phase temperature at the outlet of the S gas separation tank reaches minus 28 ℃, which indicates that the crystallization of the ammonia compound in the system is obviously controlled; CO in the obtained ammonia water 2 、H 2 S and other impurities are greatly reduced, and discharged to acid gas flare gas NH 3 The mole fraction ratio is reduced from 0.016% to 0.001%, and the ammonia recycling utilization rate is 93.75%, so that the effect of ammonia recycling utilization is achieved.
Example 5
In the gas guide process of the low-temperature methanol washing system, the outlet pressure of the thermal regeneration tower has a slow rising trend, the outlet pressure of the thermal regeneration tower reaches 0.313 MPa from 0.215, meanwhile, the acid gas flow is gradually reduced, and H is the gas flow rate 2 S, the temperature of the outlet of the gas-liquid separation tank slowly rises, a vent valve and a bypass are opened on site, the pressure release effect of the thermal regeneration tower is poor, and the system is judged to be blocked by ammonia compounds.
In order to solve the above problems, the recycling system for ammonia in the low-temperature methanol-wash acidic process gas according to embodiment 3 of the present utility model is specifically as follows:
(1) The temperature of the raw material gas is minus 28 ℃, the pressure of the gas is 0.28Mpa, and CO in the gas 2 Content of 70.23%, NH 3 1.68%、CO 0.17%、N 2 1.3%、H 2 S24.21%; the two crystallizers are arranged and comprise a first crystallizer 1 and a second crystallizer 2 which are connected in parallel; volume flow 442.15m 3 The raw gas of/h enters the first crystallizer 1 through an acid gas input pipeline 10, and is raw at low temperatureH contained in the feed gas 2 S、COS、CO 2 、NH 3 The two react with each other to generate amino compound crystals on the built-in metal wire mesh; the crystallizer is provided with an automatic control system, a pressure sensor and a differential pressure meter are arranged at the inlet and the outlet of the crystallizer, the automatic control system takes 5kPa as a signal point, the opening of an inlet valve group on an acid gas input pipeline 10 is controlled in an interlocking manner, the gas pressure difference at the inlet and the outlet of the crystallizer is controlled to be 130-160KPa, and when the first crystallizer 1 is saturated, the air inlet is stopped; the inlet valve group connected with the second crystallizer 2 in the acid gas input pipeline 10 is opened in an interlocking way, and the raw gas enters the second crystallizer 2 to finish the switching of the first crystallizer 1 and the second crystallizer 2;
(2) After the crystallizer is saturated, nitrogen enters a heat exchanger 4 through a low-pressure nitrogen input pipeline 30 to exchange heat, the temperature of the nitrogen after heat exchange is more than or equal to 10 ℃, then the nitrogen is discharged from a low-pressure nitrogen output pipeline 40 and enters the crystallizer, an inlet valve group and the crystallizer are subjected to tempering and purging, desalted water is prevented from entering low-temperature equipment to freeze, equipment damage is caused, part of amino compound solids are heated and decomposed in the tempering process, and gas generated by decomposition enters an absorption tank 3 through a tempering pipeline 70; when the temperature of the crystallizer is more than or equal to 10 ℃, desalted water enters the crystallizer from a desalted water pipeline 50, nitrogen is kept to be continuously introduced, the effects of stirring liquid and flushing crystallization are achieved, the amino compound crystals are fully dissolved, after 45min, a cleaning water pipeline 60 is opened, and the crystallized and dissolved desalted water in the crystallizer is discharged into an absorption tank 3 from the cleaning water pipeline 60; desalted water with one third of the tank volume is stored in the absorption tank 3 in advance to prevent NH in the re-heat gas 3 Escape of (2);
(3) After the cleaning water is discharged into the absorption tank 3, the heat tracing system is started due to heat absorption in the dissolution process, and the temperature in the absorption tank 3 is controlled to be 20 ℃ so as to crystallize and decompose the dissolved amino compound into NH 4 + 、NH 2 COO - 、HCO 3 - 、CO 3 2- 、S 2- 、HS - Plasma, then starting a vacuum pump 5, controlling the vacuum degree to be 0.06MPa, changing the balance state of the system, and promoting acid gas CO 2 、H 2 S overflows to realize NH 3 Separation process from acid gas, separated CO 2 、H 2 S acid gas is discharged to the acid gas torch gas from the gas outlet of the vacuum pump 5 through the acid gas torch gas phase pipeline 20, the generated ammonia is dissolved in water to form ammonia water, and the ammonia water is discharged to an ammonia evaporation system through the delivery pipeline 80, so that ammonia resource utilization is realized.
After the system is operated for 51h, NH in methanol at the outlet of the thermal regeneration tower 3 The mass concentration is reduced to 18.11 mg/L, the pH is maintained between 0.009-0.023 mol/L and 8-9, and at the same time, the pressure difference of the whole system is gradually recovered to the normal pressure difference of 0.04 MPa, H 2 The gas phase temperature at the outlet of the S gas separation tank reaches-26 ℃, which indicates that the crystallization of the ammonia compound in the system is obviously controlled; NH discharged to acid gas flare gas 3 The molar fraction ratio is reduced from 0.013% to 0.001%, and the ammonia recycling utilization rate is 92.30%.
Claims (3)
1. A resource utilization system for ammonia in low-temperature methanol washing acid process gas is characterized in that: comprises a crystallization system, a tempering and absorbing system and a separation system;
the crystallization system comprises a crystallizer; the bottom of the crystallizer is connected with an acid gas input pipeline (10); an inlet valve group comprising a ball valve and a pneumatic regulating valve is arranged at one end, close to the crystallizer, of the acid gas input pipeline (10);
the heat recovery and absorption system comprises a heat exchanger (4) and an absorption tank (3), wherein a shell side inlet of the heat exchanger (4) is connected with a low-pressure nitrogen input pipeline (30), and a shell side outlet of the heat exchanger (4) is connected with a low-pressure nitrogen output pipeline (40); the other end of the low-pressure nitrogen output pipeline (40) is also connected with the top of the crystallizer and the middle of an inlet valve group on the acid gas input pipeline (10); a rewarming pipeline (70) is connected between the absorption tank (3) and the top of the crystallizer, and the rewarming pipeline (70) stretches into the absorption tank (3); a cleaning water pipeline (60) is connected between the bottom of the crystallizer and the top of the absorption tank (3); the tempering and absorbing system further comprises a desalted water pipeline (50), wherein the desalted water pipeline (50) is connected with the bottom of the crystallizer;
the separation system comprises an outer conveying pipeline (80) and a vacuum pump (5), wherein the outer conveying pipeline (80) is connected with the absorption tank (3), and an air outlet of the vacuum pump (5) is connected with an acid gas flare gas-phase pipeline (20); the separation system also comprises a heat tracing system connected with the absorption tank (3).
2. The recycling system for ammonia in low-temperature methanol-scrubbing acidic process gas according to claim 1, wherein the recycling system is characterized in that: the two crystallizers are arranged and comprise a first crystallizer (1) and a second crystallizer (2) which are connected in parallel.
3. The recycling system for ammonia in low-temperature methanol-scrubbing acidic process gas according to claim 2, wherein the recycling system is characterized in that: the recycling system further comprises a circulating pipeline (90), wherein an inlet of the circulating pipeline (90) is connected with the delivery pipeline (80), and an outlet of the circulating pipeline (90) is connected with one end, close to the crystallizer, of the desalted water pipeline (50).
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202320954559.2U CN219839665U (en) | 2023-04-25 | 2023-04-25 | Resource utilization system for ammonia in low-temperature methanol washing acid process gas |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202320954559.2U CN219839665U (en) | 2023-04-25 | 2023-04-25 | Resource utilization system for ammonia in low-temperature methanol washing acid process gas |
Publications (1)
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