CN105664669B - The processing method of unreacted ammonia in acrylonitrile reactor device - Google Patents
The processing method of unreacted ammonia in acrylonitrile reactor device Download PDFInfo
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Abstract
The present invention relates to the processing method of unreacted ammonia in acrylonitrile reactor device, mainly solves unreacted ammonia in the prior art and absorbs incomplete problem.By using including：High ammonolysis product air-flow unreacted ammonia in chilling tower contacts the high ammonolysis product air-flow of absorption with poor ammonium absorbing liquid, obtains rich ammonium absorbing liquid and low ammonolysis product air-flow；By rich ammonium absorbing liquid in stripper through stripper stripping gas stripping volatile organic component, supernatant light component is separated off in separator again and is sunken to the heavy constituent of lower floor, then heated in Analytic Tower and Analytic Tower stripping gas strips to obtain thick ammonia flow and poor ammonium absorbing liquid, and poor ammonium absorbing liquid returns to the absorption that chilling tower is used for unreacted ammonia；Thick ammonia, which flows through, to be obtained no ammonia logistics after CWO and is used for device cycling use of water；Wherein, the technical scheme selected from least one of phosphoric acid, ammonium dihydrogen phosphate or sulfuric acid absorbent is contained in poor ammonium absorbing liquid and preferably solves the problem, available in acrylonitrile process.
Description
Technical field
The present invention relates to the processing method of unreacted ammonia in acrylonitrile reactor device.
Background technology
10% or so unreacted ammonia is had in Acrylonitrile Production to be needed to be absorbed to isolate from reaction stream
Come.Although there is the content that technology can reduce reactor outlet ammonia, but still there is the presence of a large amount of unreacted ammonia.Production technology at present
Mainly by sulfuric acid scrubbing so as to absorb unreacted ammonia, amine wastewater of sulphuric acid is directly injected into deep-well processing, or through thiamine recovery workshop section
Recovery crystallization sulphur ammonium, or sulphur ammonium are burned and SO are made3, then sulfuric acid is made through absorption and returns system circulation use.Also partial monopoly leads to
In peroxophosphoric acid, ammonium dihydrogen phosphate or the two mixture and recovery unreacted ammonia.
Patent CN1204620A discloses a kind of reaction for being used to from generation alkene nitrile or methacrylonitrile reaction zone obtain
The method of middle recovery unreacted ammonia, above-mentioned reactor effluent is quenched with ammonium phosphate solution after device outflow, wherein, described molten
The ratio between ammonium ion and phosphate anion in liquid are about 0.7-1.3, preferably 1.0-1.2.It is useless remaining in absorbing liquid in order to remove
Organic matter, wet oxidation unit, temperature and 600-3000 of the wet oxidation reaction at about 200 DEG C -650 DEG C are added in method
Pound/square inch pressure under carry out.
Patent CN101027252A discloses a kind of modification method that ammonia is reclaimed and circulated from steam stream, and this method includes
The aqueous solution quenching reaction device effluent of ammonium phosphate is used at least two stages, so as to capture the ammonia components in effluent.It is logical
The ammonia of year capture can be reclaimed by crossing heated phosphoric aqueous ammonium, then circulate the ammonium phosphate solution.Before circulation, by wet
Formula oxidation can remove pollutant contained in ammonium phosphate solution.
But in the prior art, low ammonia production of the high ammonolysis product air-flow from ammonia oxidation reactor after the absorption of poor ammonium absorbing liquid
The ammonia of significant quantity is still remained in product air-flow, so as to influence the raising of product quality.Ammonia is realized by rectifier unit in the prior art
Recycling, rectification cell and want big energy to maintain, so high energy consumption.
The content of the invention
The problem of technical problems to be solved by the invention are incomplete unreacted ammonia absorption in the prior art, high energy consumption,
A kind of processing method of unreacted ammonia in new acrylonitrile reactor device is provided.There is this method ammonia to absorb, and complete, energy consumption is low
Advantage.
In order to solve the above technical problems, the technical solution adopted by the present invention is as follows：
The absorption process of unreacted ammonia, comprises the following steps in acrylonitrile reactor device：
High ammonolysis product air-flow 6 from ammonia oxidation reactor out contacts absorption height with poor ammonium absorbing liquid 14 in chilling tower 1
Unreacted ammonia in ammonolysis product air-flow, obtain rich ammonium absorbing liquid 8 and low ammonolysis product air-flow 7；By rich ammonium absorbing liquid 8 in stripper 2
It is interior through the stripping volatile organic component 10 of stripper stripping gas 9, then be separated off in separator 3 supernatant light
Component 11 and the heavy constituent 12 for being sunken to lower floor, it is then heated in Analytic Tower 4 to obtain thick ammonia with the stripping of Analytic Tower stripping gas 13
Air-flow 15 and poor ammonium absorbing liquid 14, poor ammonium absorbing liquid 14 return to the absorption that chilling tower 1 is used for unreacted ammonia；Thick ammonia flow 15 is with containing
Carrier of oxygen 16 obtains pure ammonia logistics 17 after the reaction of CWO reactor 5；Wherein, contain in poor ammonium absorbing liquid and be selected from phosphorus
At least one of acid, ammonium dihydrogen phosphate or sulfuric acid absorbent.Volatile organic constituents (10) are preferably returned to chilling tower 1.Poor ammonium
Absorbent in absorbing liquid preferably includes：(a) at least one of phosphoric acid and ammonium dihydrogen phosphate；Sulfuric acid (b)；More preferably poor ammonium
S/P mol ratios are 0.01-0.5 in absorbing liquid, and wherein S represents element sulphur, and P represents P elements；Poor ammonium is inhaled in above-mentioned technical proposal
It is preferably 2-6.5 to receive liquid pH value.In above-mentioned technical proposal in preferred poor ammonium absorbing liquid 14 mass content of P element for 3%~
8%.
In above-mentioned technical proposal, separator 3 preferably has the upper outlet of discharge light component 11.
In above-mentioned technical proposal, separator 3 preferably has the lower outlet of discharge heavy constituent 11.
In above-mentioned technical proposal, the temperature of poor ammonium absorbing liquid is preferably 50-85 DEG C.
In above-mentioned technical proposal, stripper stripping gas 9 and/or Analytic Tower stripping gas 13 are preferably inert to stripping thing
Gas.
In above-mentioned technical proposal, the gas inert to stripping thing is preferably at least one in water vapour, air and nitrogen
Kind.
In above-mentioned technical proposal, the heavy constituent 12 is high polymer and/or catalyst fines.
In above-mentioned technical proposal, the poor ammonium absorbing liquid 14 is using water as solvent.
In above-mentioned technical proposal, Analytic Tower temperature is preferably 150-250 DEG C.
In above-mentioned technical proposal, parsing pressure tower is preferably the saturated vapor pressure of solution in Analytic Tower under relevant temperature.
In above-mentioned technical proposal, wet oxidation reactor interior reaction temperature is preferably 150-300 DEG C, and pressure is preferably
5MPa-12MPa。
In above-mentioned technical proposal, oxygen-containing gas is the oxygen rich gas that air, pure oxygen and oxygen content are 35-50v%.Oxygen content
Can be by oxygen mix in inert diluent gas for 35-50v% oxygen rich gas, conventional inert diluent may be incorporated for this
Invention, such as nitrogen, carbon dioxide, helium, neon, argon gas etc..Inert diluent in the embodiment of the present invention in oxygen rich gas
Use nitrogen.
In above-mentioned technical proposal, wet oxidation reaction used catalyst is not particularly limited, and preferred pair ammonia nitrogen, which has, preferably to be gone
Except those catalyst of rate, such as, but not limited to include the loaded catalyst of at least one of Pt, Pd, Ru and Rh active component.
The carrier of loaded catalyst does not limit, those commonly used in the art, such as, but not limited to silica, aluminum oxide, oxygen
Change titanium etc..Silica supports are used in the embodiment of the present invention.
Place a small amount of sulfuric acid in poor ammonium absorbing liquid in the inventive method, can make the absorption efficiency of ammonia than only with phosphoric acid and/
Or ammonium dihydrogen phosphate is high, also than only using, sulfuric acid is high, and absorptivity reaches 100%, improves the quality of product air-flow.
Ammonia being removed with wet oxidation method in the inventive method and substituting ammonia rectifier unit, wet oxidation reaction is that heat release is anti-
Should, generation energy, and ammonia distillation process consumed energy, energy consumption reduces in the process of the present invention for institute.
The present invention is described in detail with reference to the accompanying drawings and detailed description.
Brief description of the drawings
Fig. 1 is the process flow diagram of the present invention.
In Fig. 1,1 is chilling tower, and 2 be stripper, and 3 be separator, and 4 be Analytic Tower, and 5 be that CWO reacts
Device；6 be high ammonolysis product air-flow, and 7 be low ammonolysis product air-flow, and 8 be rich ammonium absorbing liquid, and 9 be stripper stripping gas, and 10 have for volatility
Machine component, 11 be light component, and 12 be heavy constituent, and 13 be Analytic Tower stripping gas, and 14 be poor ammonium absorbing liquid, and 15 be thick ammonia flow, 16
It is without ammonia flow for oxygen-containing gas, 17.
Flow is shown in Fig. 1：High ammonolysis product air-flow 6 from ammonia oxidation reactor is in chilling tower 1 and poor ammonium absorbing liquid 15
Contact absorbs unreacted ammonia, obtains low ammonolysis product air-flow 7 and rich ammonium absorbing liquid 8, rich ammonium absorbing liquid 8 is in stripper 2 through stripping
Gas 9 removes volatile organic constituents 10, then is separated off supernatant light component 11 in separator 3 and is sunken to lower floor
Heavy constituent 12, it is then heated in Analytic Tower 4 to obtain thick ammonia flow 15 and poor ammonium absorbing liquid with the stripping of Analytic Tower stripping gas 13
14, poor ammonium absorbing liquid 14 returns to chilling tower 1 and is used to circulate the absorption for unreacted ammonia；Thick ammonia flow 15 is through CWO
Reactor 5 obtains no ammonia logistics 17 with the reaction of oxygen-containing gas 16, and no ammonia logistics 17 can be used for device cycling use of water (not shown).
Embodiment
Embodiment 1-6 and comparative example 1 and comparative example 2 flow operations as shown in Figure 1, use in poor ammonium absorbing liquid molten
Agent is water.
【Embodiment 1】
High ammonolysis product air-flow from ammoxidation of propylene reactor contacts in chilling tower with poor ammonium absorbing liquid absorbs unreacted
Ammonia obtain low ammonolysis product air-flow and rich ammonium absorbing liquid, S/P mol ratios are 0.01 in poor ammonium absorbing liquid, and P elements mass content is
6.5%, absorbing liquid pH value is 2, and the temperature of poor ammonium absorbing liquid is 85 DEG C, and ammonia contains in the low ammonolysis product air-flow obtained by absorption
Amount is detected as 0.Rich ammonium absorbing liquid enters separator in stripper after water vapour stripping gas stripping, removes light component and bag
The heavy constituent of catalyst and/or polymer is included, Analytic Tower is then entered back into and parses to obtain thick ammonia flow and poor ammonium absorbing liquid, is parsed
Tower operation temperature is 195 DEG C, and stripping gas is air.Poor ammonium absorbing liquid returns to chilling tower and is used to absorb unreacted ammonia.Thick ammonia
Air-flow enters CWO reactor, obtains no ammonia logistics after removing ammonia nitrogen under Pt catalytic action, reaction temperature is
150 DEG C, reaction pressure 5MPa, oxygen-containing gas is purity oxygen.It can be used for device cycling use of water without ammonia logistics.
For ease of comparing, technological condition and result are listed in table 1, table 2.
【Embodiment 2】
High ammonolysis product air-flow from ammoxidation of propylene reactor contacts in chilling tower with poor ammonium absorbing liquid absorbs unreacted
Ammonia obtain low ammonolysis product air-flow and rich ammonium absorbing liquid, S/P mol ratios are 0.05 in poor ammonium absorbing liquid, and P elements mass content is
8.0%, absorbing liquid pH value is 3.5, and the temperature of poor ammonium absorbing liquid is 75 DEG C, ammonia in the low ammonolysis product air-flow obtained by absorption
Content is detected as 0.Rich ammonium absorbing liquid enters separator in stripper after air strips, and removes light component and including catalysis
Agent and/or the heavy constituent of polymer, then enter back into Analytic Tower and parse to obtain thick ammonia flow and poor ammonium absorbing liquid, Analytic Tower operation
Temperature is 250 DEG C, and stripping gas is nitrogen.Poor ammonium absorbing liquid returns to chilling tower and is used to absorb unreacted ammonia.Thick ammonia flows into
Entering CWO reactor, no ammonia logistics is obtained after ammonia nitrogen is removed under Rh catalytic action, reaction temperature is 260 DEG C,
Reaction pressure is 10MPa, and oxygen-containing gas is air.It can be used for device cycling use of water without ammonia logistics.
For ease of comparing, technological condition and result are listed in table 1, table 2.
【Embodiment 3】
High ammonolysis product air-flow from ammoxidation of propylene reactor contacts in chilling tower with poor ammonium absorbing liquid absorbs unreacted
Ammonia obtain low ammonolysis product air-flow and rich ammonium absorbing liquid, S/P mol ratios are 0.1 in poor ammonium absorbing liquid, and P elements mass content is
5.0%, absorbing liquid pH value is 2.5, and the temperature of poor ammonium absorbing liquid is 50 DEG C, ammonia in the low ammonolysis product air-flow obtained by absorption
Content is detected as 0.Rich ammonium absorbing liquid enters separator in stripper after nitrogen stripping, removes light component and including catalysis
Agent and/or the heavy constituent of polymer, then enter back into Analytic Tower and parse to obtain thick ammonia flow and poor ammonium absorbing liquid, Analytic Tower operation
Temperature is 150 DEG C, and stripping gas is water vapour.Poor ammonium absorbing liquid returns to chilling tower and is used to absorb unreacted ammonia.Thick ammonia flow
Into CWO reactor, no ammonia logistics, reaction temperature 300 are obtained after removing ammonia nitrogen under Pd catalytic action
DEG C, reaction pressure 12MPa, oxygen-containing gas is purity oxygen.It can be used for device cycling use of water without ammonia logistics.
For ease of comparing, technological condition and result are listed in table 1, table 2.
【Embodiment 4】
High ammonolysis product air-flow from ammoxidation of propylene reactor contacts in chilling tower with poor ammonium absorbing liquid absorbs unreacted
Ammonia obtain low ammonolysis product air-flow and rich ammonium absorbing liquid, S/P mol ratios are 0.1 in poor ammonium absorbing liquid, and P elements mass content is
6.5%, absorbing liquid pH value is 5.0, and the temperature of poor ammonium absorbing liquid is 80 DEG C, ammonia in the low ammonolysis product air-flow obtained by absorption
Content is detected as 0.Rich ammonium absorbing liquid enters separator in stripper after air strips, and removes light component and including catalysis
Agent and/or the heavy constituent of polymer, then enter back into Analytic Tower and parse to obtain thick ammonia flow and poor ammonium absorbing liquid, Analytic Tower operation
Temperature is 190 DEG C, and stripping gas is water vapour.Poor ammonium absorbing liquid returns to chilling tower and is used to absorb unreacted ammonia.Thick ammonia flow
Into CWO reactor, poor ammonium absorbing liquid and wet oxidation tail are obtained after removing ammonia nitrogen under Ru catalytic action
Gas, reaction temperature are 280 DEG C, reaction pressure 11MPa, and oxygen-containing gas is 50v% oxygen.Circulated without ammonia logistics available for device
Use water.
For ease of comparing, technological condition and result are listed in table 1, table 2.
【Embodiment 5】
High ammonolysis product air-flow from ammoxidation of propylene reactor contacts in chilling tower with poor ammonium absorbing liquid absorbs unreacted
Ammonia obtain low ammonolysis product air-flow and rich ammonium absorbing liquid, S/P mol ratios are 0.3 in poor ammonium absorbing liquid, and P elements mass content is
6.0%, absorbing liquid pH value is 6.5, and the temperature of poor ammonium absorbing liquid is 65 DEG C, ammonia in the low ammonolysis product air-flow obtained by absorption
Content is detected as 0.Rich ammonium absorbing liquid enters separator in stripper after nitrogen stripping, removes light component and including catalysis
Agent and/or the heavy constituent of polymer, then enter back into Analytic Tower and parse to obtain thick ammonia flow and poor ammonium absorbing liquid, Analytic Tower operation
Temperature is 170 DEG C, and stripping gas is water vapour.Poor ammonium absorbing liquid returns to chilling tower and is used to absorb unreacted ammonia.Thick ammonia flow
Into CWO reactor, no ammonia logistics, reaction temperature 230 are obtained after removing ammonia nitrogen under Pt catalytic action
DEG C, reaction pressure 9MPa, oxygen-containing gas is 35v% oxygen.It can be used for device cycling use of water without ammonia logistics.
For ease of comparing, technological condition and result are listed in table 1, table 2.
【Embodiment 6】
High ammonolysis product air-flow from ammoxidation of propylene reactor contacts in chilling tower with poor ammonium absorbing liquid absorbs unreacted
Ammonia obtain low ammonolysis product air-flow and rich ammonium absorbing liquid, S/P mol ratios are 0.5 in poor ammonium absorbing liquid, and P elements mass content is
3.3%, absorbing liquid pH value is 5.0, and the temperature of poor ammonium absorbing liquid is 70 DEG C, ammonia in the low ammonolysis product air-flow obtained by absorption
Content is detected as 0.Rich ammonium absorbing liquid enters separator in stripper after air strips, and removes light component and including catalysis
Agent and/or the heavy constituent of polymer, then enter back into Analytic Tower and parse to obtain thick ammonia flow and poor ammonium absorbing liquid, Analytic Tower operation
Temperature is 165 DEG C, and stripping gas is water vapour.Poor ammonium absorbing liquid returns to chilling tower and is used to absorb unreacted ammonia.Thick ammonia flow
Into CWO reactor, no ammonia logistics, reaction temperature 270 are obtained after removing ammonia nitrogen under Pt catalytic action
DEG C, reaction pressure 11MPa, oxygen-containing gas is 40v% oxygen.It can be used for device cycling use of water without ammonia logistics.
For ease of comparing, technological condition and result are listed in table 1, table 2.
【Comparative example 1】
Difference from Example 4 is that the property of poor ammonium absorbing liquid is：S/P mol ratios are 0, pH 5, temperature 80
DEG C, P content 6.5wt%；Other process conditions are same as Example 4.Specially：
High ammonolysis product air-flow from ammoxidation of propylene reactor contacts in chilling tower with poor ammonium absorbing liquid absorbs unreacted
Ammonia obtain low ammonolysis product air-flow and rich ammonium absorbing liquid, the content of ammonia is detected as in the low ammonolysis product air-flow obtained by absorption
0.2wt%.Rich ammonium absorbing liquid enters separator in stripper after air strips, remove light component and including catalyst and/
Or the heavy constituent of polymer, then enter back into Analytic Tower and parse to obtain thick ammonia flow and poor ammonium absorbing liquid, Analytic Tower operation temperature
For 190 DEG C, stripping gas is water vapour.Poor ammonium absorbing liquid returns to chilling tower and is used to absorb unreacted ammonia.Thick ammonia flow enters
CWO reactor, poor ammonium absorbing liquid and wet oxidation tail gas are obtained after removing ammonia nitrogen under Ru catalytic action, instead
It is 280 DEG C, reaction pressure 11MPa to answer temperature, and oxygen-containing gas is 50v% oxygen.It can be used for device cycling use of water without ammonia logistics.
For ease of comparing, technological condition and result are listed in table 1, table 2.
【Comparative example 2】
Difference from Example 4 is that the property of poor ammonium absorbing liquid is：Absorbent is sulfuric acid, without P, pH 5, temperature
For 80 DEG C；Other process conditions are same as Example 4.Specially：
High ammonolysis product air-flow from ammoxidation of propylene reactor contacts in chilling tower with poor ammonium absorbing liquid absorbs unreacted
Ammonia obtain low ammonolysis product air-flow and rich ammonium absorbing liquid, the content of ammonia is detected as in the low ammonolysis product air-flow obtained by absorption
0.1wt%.Rich ammonium absorbing liquid enters separator in stripper after air strips, remove light component and including catalyst and/
Or the heavy constituent of polymer, then enter back into Analytic Tower and parse to obtain thick ammonia flow and poor ammonium absorbing liquid, Analytic Tower operation temperature
For 190 DEG C, stripping gas is water vapour.Poor ammonium absorbing liquid returns to chilling tower and is used to absorb unreacted ammonia.Thick ammonia flow enters
CWO reactor, poor ammonium absorbing liquid and wet oxidation tail gas are obtained after removing ammonia nitrogen under Ru catalytic action, instead
It is 280 DEG C, reaction pressure 11MPa to answer temperature, and oxygen-containing gas is 50v% oxygen.It can be used for device cycling use of water without ammonia logistics.
For ease of comparing, technological condition and result are listed in table 1, table 2.
Only with the absorbent containing S or only with the absorbent containing P be not so good as using simultaneously the absorbent containing S and P it is good, this from
Comparative example 1 and 2 and embodiment 4 it is year-on-year in can be seen more clearly.
Table 1
Table 2
Claims (10)
1. the processing method of unreacted ammonia, comprises the following steps in acrylonitrile reactor device：
High ammonolysis product air-flow (6) from ammonia oxidation reactor out contacts absorption in chilling tower (1) with poor ammonium absorbing liquid (14)
Unreacted ammonia in high ammonolysis product air-flow, obtain rich ammonium absorbing liquid (8) and low ammonolysis product air-flow (7)；Rich ammonium absorbing liquid (8) is existed
Through stripper stripping gas (9) stripping volatile organic component (10) in stripper (2), then separated in separator (3)
Remove supernatant light component (11) and be sunken to the heavy constituent (12) of lower floor, then heated in Analytic Tower (4) and parsing
Tower stripping gas (13) stripping obtains thick ammonia flow (15) and poor ammonium absorbing liquid (14), and poor ammonium absorbing liquid (14) returns to chilling tower (1)
Absorption for unreacted ammonia；Thick ammonia flow (15) obtains nothing with oxygen-containing gas (16) after wet oxidation reactor (5) reaction
Ammonia logistics (17)；
Wherein, the absorbent in poor ammonium absorbing liquid includes：(a) at least one of phosphoric acid and ammonium dihydrogen phosphate, and (b) sulfuric acid.
2. according to the method for claim 1, it is characterised in that separator (3) have discharge light component (11) on go out
Mouthful.
3. according to the method for claim 1, it is characterised in that separator (3) has to go out under discharge heavy constituent (12)
Mouthful.
4. according to the method for claim 1, it is characterised in that the temperature of poor ammonium absorbing liquid is 50-85 DEG C.
5. according to the method for claim 1, it is characterised in that stripper stripping gas (9) and/or Analytic Tower stripping gas (13)
For the gas inert to stripping thing.
6. according to the method for claim 5, it is characterised in that the gas inert to stripping thing is water vapour, air and nitrogen
At least one of gas.
7. according to the method described in claim 1, it is characterised in that the heavy constituent (12) is high polymer and/or catalyst fines.
8. according to the method described in claim 1, it is characterised in that the poor ammonium absorbing liquid (14) is using water as solvent.
9. according to the method for claim 1, it is characterised in that Analytic Tower temperature is 150-250 DEG C.
10. according to the method for claim 1, it is characterised in that wet oxidation reaction used catalyst is to include Pt, Pd, Ru
With the loaded catalyst that at least one of Rh is active component.
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