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Full-temperature-range simulated rotating moving bed pressure swing adsorption process for extracting H2 and NH3 from synthetic ammonia purge gas

A technology of synthetic ammonia degassing and pressure swing adsorption, which is applied in the direction of ammonia preparation/separation, separation methods, bulk chemical production, etc., and can solve the problems of discounted mass transfer efficiency, non-standard deamination and impurity removal, and fluctuations in ammonia content and other issues to achieve the effect of reducing manufacturing complexity and cost

Pending Publication Date: 2022-06-07
ZHEJIANG TIANCAIYUNJI TECH CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, the traditional PSA separation method still has some significant defects: first, the size and fluctuation of the ammonia content in the purge gas seriously restricts the separation and extraction of H by PSA. 2 s efficiency
However, the RWPSA process also has obvious limitations and disadvantages: First, the diameter and height (thickness) of the adsorption wheel are relatively limited, resulting in an insufficient scale of adsorption treatment. This is because the RWPSA is essentially a moving bed, and similar cycle In the "steady state" mass transfer of these typical moving bed adsorption processes such as bed or fluidized bed, the axial mass transfer diffusion or radial mass transfer diffusion capacity must be limited, and thus cannot meet the requirements for the removal of ammonia or water to balance adsorption. Purification Requirements for Mechanism-Based Adsorbate Components
This feature is an advantage for the axial flow or radial flow fixed bed process; second, the manufacturing of the rotary PSA equipment is complicated, especially the equipment with equalization is more complicated, and the number of equalization is not more than 2 times. Therefore, it is not suitable for high-pressure purge gas PSA purification of H 2 Working conditions, because for the high-pressure purge gas, the pressure equalization two times makes the pressure change too large, which will cause the air flow in the adsorption tower to be too fast and bring out the solid adsorbent particles, which will cause the process control valve and regulating valve or Rotary valves bring erosion and wear, coupled with the influence of the rotational shear force of the adsorbent itself, the pulverization of the adsorbent particles will be quite serious, which will cause leakage and safety hazards in the corresponding rotary valves or control valves
At present, the rotary PSA equipment is mostly manufactured or monopolized by foreign companies, and the cost is relatively high; third, it is more suitable for the rapid adsorption and rapid desorption of a single adsorbate component, and the adsorption mechanism of the adsorbate component is mainly kinetic adsorption. working conditions, such as the purification of exhaust gas containing VOCs, etc.
For the deamination process based on equilibrium adsorption, the RWPSA process is not suitable, especially when the synthetic ammonia release gas contains more NH with strong polarity. 3 , CO 2 Impurity components such as water, hydrocarbons, etc. require a long enough mass transfer path for adsorption. The too short adsorbent bed height in the RWPSA process cannot fully absorb these impurity components, resulting in deamination and impurity removal not up to standard. At the same time, the adsorbent cannot form a composite bed filled with various adsorbents in a fixed bed for treatment, and is especially vulnerable to water droplets in the vent gas, high hydrocarbons and other easily polluted droplets such as compressors; Fourth, the adsorbent in the RWPSA is prone to throwing due to the existence of shear force when rotating, resulting in partial flow or short flow of the process gas in the adsorption bed, which greatly reduces the mass transfer efficiency and makes the adsorbent easier to absorb. Pulverization leads to shortened adsorbent life
In the rotary pressure swing adsorption method, regular adsorbents are also commonly used instead of granular granular adsorbents, which can reduce the alternating stress and loss of adsorbent particles, but for the deamination purification and purification of synthetic ammonia purge gas 2 For this type of regular adsorbent, especially composite structured adsorbent, there are few reports at home and abroad.

Method used

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  • Full-temperature-range simulated rotating moving bed pressure swing adsorption process for extracting H2 and NH3 from synthetic ammonia purge gas
  • Full-temperature-range simulated rotating moving bed pressure swing adsorption process for extracting H2 and NH3 from synthetic ammonia purge gas
  • Full-temperature-range simulated rotating moving bed pressure swing adsorption process for extracting H2 and NH3 from synthetic ammonia purge gas

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0032] like figure 1 As shown, the described one extracts H from the synthetic ammonia purge gas 2 with NH 3The full temperature range simulated rotary moving bed pressure swing adsorption process, in which the full temperature range simulated rotary moving bed pressure swing adsorption (FTrSRMPSA) system is composed of 5 (n'=5') axial flow and A fixed composite bed adsorption tower with a height-to-diameter ratio of 3 and a fixed composite of 5 (n=5) axial flows loaded with aluminum oxide, silica gel, activated carbon, molecular sieve / carbon molecular sieve and a height-to-diameter ratio of 4.5 to 5.0 The bed adsorption tower is installed in a rotating speed of ω 2 The adsorption tower (n'+n=10) and the corresponding drive mechanism on the annular rotating tray with =0, the number of channels are m'=9 and m=9 respectively, and they are placed in the center of the annular tray, and respectively Take the rotation speed as ω 1 ’=500~700s and ω 1 = 400~600s upper and lower t...

Embodiment 2

[0034] like figure 2 As shown, on the basis of Example 1, the cyclic operation steps of PSA adsorption and desorption in the medium and high temperature pressure swing adsorption ammonia concentration system are followed by replacement (DP') after the adsorption (A') step is completed. step, using a concentrated ammonia gas (NH 3 CG) as a replacement gas (DP') to replace (DP'), and after the replacement (DP') step is completed, a first pressure drop (E1D') and a second pressure drop (E2D') are carried out. The sloping (PP') step is cancelled, and the corresponding m' channel of the rotary valve (such as m'=5') is used as the replacement gas (DP') channel, and the replacement gas (DPW) generated by the replacement (DP') step is used. '), which flows through the original ammonia-rich flushing exhaust gas (NH 3 PW') channel (such as m'=7') and as intermediate gas (IG) into the intermediate gas (IG) buffer tank for recycling, after the secondary pressure equalization (E2D') ste...

Embodiment 3

[0036] like image 3 As shown, on the basis of Examples 1 and 2, in the intermediate gas pressure swing adsorption hydrogen extraction system, the vacuum (V) desorption step is used to replace the reverse discharge (D) step of the ammonia concentrated adsorption phase, and the vacuum (V) is formed. Nitrogen-rich stripping gas (N 2 D) From the outlet of n (such as n=3) adsorption tower, it flows through the external pipeline connected to the outlet of the adsorption tower on the annular rotating tray, and the external pipeline is equipped with a vacuum pump and a control valve to control the flow and enter the rich Nitrogen stripping gas (N 2 D) Buffer tank, the maximum vacuum degree is -0.08MPa, the original reverse degassing (D) channel (such as m=6) in the corresponding m-channel rotary valve becomes an empty channel, and the adsorbent in the n adsorption tower is completely desorbed, get H 2 Product gas (H 2 PG) purity is greater than or equal to 99.99%, the yield is gr...

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Abstract

The invention discloses a full-temperature-range simulated rotating moving bed pressure swing adsorption (FTrSRMPSA) process for extracting H2 and NH3 from synthetic ammonia purge gas. The middle-high temperature pressure swing adsorption ammonia concentration system and the middle gas pressure swing adsorption hydrogen extraction system are formed by a plurality of axial flow fixed bed adsorption towers and a rotating speed mechanism, wherein the axial flow fixed bed adsorption towers are arranged in the center of an upper multi-channel rotating valve and a lower multi-channel rotating valve, and are arranged on a circular ring-shaped rotating tray around the multi-channel rotating valve; gas flowing through a rotary valve channel, pipelines at the inlet and outlet ends of the adsorption towers and the adsorption bed layers can complete mass transfer of respective adsorption and desorption steps at the inlet and outlet positions of each adsorption tower and at each adsorption bed layer while rotating, so that a pressure swing adsorption process of simulating a rotary moving bed is formed; according to the invention, a simulated rotating moving bed pressure swing adsorption process on the basis of axial flow fixed bed pressure swing adsorption is realized, and H2 and NH3 products are obtained with high purity and high yield and are returned to a synthetic ammonia production process for recycling.

Description

technical field [0001] The invention relates to the field of recovery and reuse of synthetic ammonia purge gas, in particular to a method for extracting H from synthetic ammonia purge gas 2 with NH 3 The full temperature range of a rotary moving bed pressure swing adsorption process is simulated. Background technique [0002] During the production of synthetic ammonia, hydrogen (H 2 ) and nitrogen (N 2 ) under the action of high temperature and high pressure and catalyst to generate synthetic ammonia (NH 3 ), but the conversion rate of synthetic ammonia is only 1 / 3. In order to improve the yield of synthetic ammonia, the unreacted hydrogen-nitrogen mixture is returned to the synthetic ammonia production process as a circulating gas to continue to participate in the reaction. During the circulation process, some inert gas components such as argon (Ar), helium ( He), etc. will continue to accumulate resulting in the reaction gas hydrogen (H 2 ) and nitrogen (N 2 ) decre...

Claims

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Application Information

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IPC IPC(8): B01D53/08C01B3/56C01C1/12
CPCB01D53/08C01B3/56C01C1/12Y02P20/52
Inventor 汪兰海陈运唐金财
Owner ZHEJIANG TIANCAIYUNJI TECH CO LTD
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