CN102452955A - Method for recycling unreacted ammonia in acrylonitrile reaction device - Google Patents
Method for recycling unreacted ammonia in acrylonitrile reaction device Download PDFInfo
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- CN102452955A CN102452955A CN2010105136404A CN201010513640A CN102452955A CN 102452955 A CN102452955 A CN 102452955A CN 2010105136404 A CN2010105136404 A CN 2010105136404A CN 201010513640 A CN201010513640 A CN 201010513640A CN 102452955 A CN102452955 A CN 102452955A
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- absorption liquid
- ammonia
- tower
- ammonium
- unreacted ammonia
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- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 title claims abstract description 123
- 229910021529 ammonia Inorganic materials 0.000 title claims abstract description 59
- 238000000034 method Methods 0.000 title claims abstract description 30
- NLHHRLWOUZZQLW-UHFFFAOYSA-N Acrylonitrile Chemical compound C=CC#N NLHHRLWOUZZQLW-UHFFFAOYSA-N 0.000 title claims abstract description 24
- 238000004064 recycling Methods 0.000 title abstract description 6
- 238000006243 chemical reaction Methods 0.000 title abstract description 4
- 238000010521 absorption reaction Methods 0.000 claims abstract description 47
- QGZKDVFQNNGYKY-UHFFFAOYSA-O Ammonium Chemical compound [NH4+] QGZKDVFQNNGYKY-UHFFFAOYSA-O 0.000 claims abstract description 45
- 239000007788 liquid Substances 0.000 claims abstract description 45
- 238000010791 quenching Methods 0.000 claims abstract description 12
- 239000012495 reaction gas Substances 0.000 claims abstract description 9
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 8
- 238000000926 separation method Methods 0.000 claims abstract description 4
- 239000000470 constituent Substances 0.000 claims description 15
- 239000007789 gas Substances 0.000 claims description 8
- NBIIXXVUZAFLBC-UHFFFAOYSA-N Phosphoric acid Chemical compound OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 claims description 6
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 4
- 239000003054 catalyst Substances 0.000 claims description 4
- 230000003647 oxidation Effects 0.000 claims description 4
- 238000007254 oxidation reaction Methods 0.000 claims description 4
- 229910000147 aluminium phosphate Inorganic materials 0.000 claims description 3
- LFVGISIMTYGQHF-UHFFFAOYSA-N ammonium dihydrogen phosphate Chemical compound [NH4+].OP(O)([O-])=O LFVGISIMTYGQHF-UHFFFAOYSA-N 0.000 claims description 3
- 239000000203 mixture Substances 0.000 claims description 3
- 229910052757 nitrogen Inorganic materials 0.000 claims description 2
- 229920006395 saturated elastomer Polymers 0.000 claims description 2
- 238000005265 energy consumption Methods 0.000 abstract description 5
- 230000000171 quenching effect Effects 0.000 abstract description 2
- 238000010438 heat treatment Methods 0.000 abstract 1
- 238000009279 wet oxidation reaction Methods 0.000 description 9
- 230000000052 comparative effect Effects 0.000 description 6
- 239000000243 solution Substances 0.000 description 6
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 description 5
- 238000005516 engineering process Methods 0.000 description 5
- 238000011084 recovery Methods 0.000 description 5
- 239000004254 Ammonium phosphate Substances 0.000 description 4
- 229910000148 ammonium phosphate Inorganic materials 0.000 description 4
- 235000019289 ammonium phosphates Nutrition 0.000 description 4
- MNNHAPBLZZVQHP-UHFFFAOYSA-N diammonium hydrogen phosphate Chemical compound [NH4+].[NH4+].OP([O-])([O-])=O MNNHAPBLZZVQHP-UHFFFAOYSA-N 0.000 description 4
- 238000004519 manufacturing process Methods 0.000 description 4
- -1 alkene nitrile Chemical class 0.000 description 3
- HIVLDXAAFGCOFU-UHFFFAOYSA-N ammonium hydrosulfide Chemical compound [NH4+].[SH-] HIVLDXAAFGCOFU-UHFFFAOYSA-N 0.000 description 3
- 230000004087 circulation Effects 0.000 description 3
- 229910019142 PO4 Inorganic materials 0.000 description 2
- 239000007864 aqueous solution Substances 0.000 description 2
- 239000010452 phosphate Substances 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- GYCMBHHDWRMZGG-UHFFFAOYSA-N Methylacrylonitrile Chemical compound CC(=C)C#N GYCMBHHDWRMZGG-UHFFFAOYSA-N 0.000 description 1
- 150000001412 amines Chemical class 0.000 description 1
- 238000005915 ammonolysis reaction Methods 0.000 description 1
- 238000002425 crystallisation Methods 0.000 description 1
- 230000008025 crystallization Effects 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 238000002715 modification method Methods 0.000 description 1
- 239000003921 oil Substances 0.000 description 1
- 229920000620 organic polymer Polymers 0.000 description 1
- 230000001590 oxidative effect Effects 0.000 description 1
- 239000000376 reactant Substances 0.000 description 1
- 238000005201 scrubbing Methods 0.000 description 1
- 239000001117 sulphuric acid Substances 0.000 description 1
- 235000011149 sulphuric acid Nutrition 0.000 description 1
- 230000001839 systemic circulation Effects 0.000 description 1
- 238000010792 warming Methods 0.000 description 1
- 239000002351 wastewater Substances 0.000 description 1
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Abstract
The invention relates to a method for recycling unreacted ammonia in an acrylonitrile reaction device, which mainly solves the problem of high energy consumption in the prior art. The method comprises the steps of (1) enabling reaction gas I to contact unreacted ammonia with poor ammonium absorption liquid I in a quench tower to obtain rich ammonium absorption liquid II and reaction gas II without ammonia; (2) stripping the ammonium-rich absorption liquid II in a stripping tower, and then carrying out oil-water separation treatment to obtain an ammonium-rich absorption liquid III; then heating the rich ammonium absorption liquid III in an analytical tower, carrying out steam stripping to obtain an ammonia gas flow III and a poor ammonium absorption liquid IV, and returning the poor ammonium absorption liquid IV to the quenching tower for absorbing unreacted ammonia; (3) the ammonia gas flow III is rectified and separated in the ammonia rectifying tower to obtain high-purity ammonia IV, and the high-purity ammonia IV returns to the ammoxidation reactor for reaction, so that the technical scheme better solves the problem and can be used in an industrial device of acrylonitrile.
Description
Technical field
The present invention relates to the method for unreacted ammonia recovery recycling in a kind of acrylonitrile reactor device.
Background technology
In the acrylonitrile process process, having unreacted ammonia about 10% need be absorbed from reactant flow and separate.Though have technology can reduce the content of reactor outlet ammonia, still have the existence of a large amount of unreacted ammonia.Thereby production technique mainly is to absorb unreacted ammonia through sulfuric acid scrubbing at present, and amine wastewater of sulphuric acid directly injects deep-well to be handled, or reclaims crystallization sulphur ammonium through sulphur ammonium recycle section, or SO is processed in the burning of sulphur ammonium
3, process sulfuric acid through absorption again and return the systemic circulation use.Also there is partial monopoly to pass through in phosphoric acid, primary ammonium phosphate or the two mixture and recovery unreacted ammonia.
Patent CN1204620A discloses a kind of being used for and has flowed out the method that reclaims unreacted ammonia the back from producing the reactor drum that alkene nitrile or methacrylonitrile reaction zone obtain; With the above-mentioned reactor effluent of ammonium phosphate solution quenching; Wherein, The ratio of the ammonium ion in said solution and phosphate anion is about 0.7～1.3, is preferably 1.0～1.2.In order to remove the useless surplus organism in the absorption liquid, added the wet oxidation unit in the method, wet oxidation reaction carries out under the pressure of about 200 ℃～650 ℃ temperature and 600～3000 pounds/square inch.
Patent CN101027252A discloses a kind of from vapour stream, the recovery and the modification method of circulation ammonia, and this method is included in two stages the aqueous solution quench reactor elute with ammonium phosphate at least, thereby catches the ammonia components in the elute.Can reclaim the ammonia of catching in year through the heated phosphoric aqueous ammonium, then with this ammonium phosphate solution circulation.Before circulation, can remove pollutent contained in the ammonium phosphate solution through wet oxidation.
More than in two patents for removing contained organism in the aqueous solution, be provided with the wet oxidation operation, wet oxidation needs higher temperature and pressure, energy consumption is high, production cost is high.Adopt two-part to absorb unreacted ammonia among the patent CN101027252A, one section ammonium ion is 1.3～2 with the ratio of phosphate anion in fact, acidity a little less than, organic polymer is serious in the absorption liquid, can reduce the productive rate of title product vinyl cyanide.
Summary of the invention
Technical problem to be solved by this invention is that the available technology adopting wet oxidation causes the high problem of energy consumption, provides that unreacted ammonia reclaims the method for recycling in a kind of new acrylonitrile reactor device.This method has advantage of low energy consumption.
In order to solve the problems of the technologies described above, the technical scheme that the present invention adopts is following: unreacted ammonia recycle and reuse method in a kind of acrylonitrile reactor device may further comprise the steps:
The reaction gas I of (1) from ammonia oxidation reactor, coming out in quench tower with poor ammonium absorption liquid I absorbing contacting reaction gas in unreacted ammonia, obtain rich ammonium absorption liquid II and not ammoniated reaction gas II;
(2) rich ammonium absorption liquid II stripping in stripping tower is removed volatile organic constituent, in an oily-water seperating equipment, carry out separating treatment again, remove contained organism and superpolymer in the solution, obtain rich ammonium absorption liquid III; In Analytic Tower, heat rich ammonium absorption liquid III then, stripping obtains ammonia flow III and poor ammonium absorption liquid IV, and poor ammonium absorption liquid IV is returned the absorption that quench tower is used for unreacted ammonia;
(3) ammonia flow III rectifying separation in the ammonia rectifying tower obtains highly purified ammonia IV, returns ammonia oxidation reactor and reacts.
In the technique scheme, poor ammonium absorption liquid I or III are phosphoric acid, primary ammonium phosphate or its mixture, and the N/P mol ratio of poor ammonium absorption liquid is 0.5～1.5: 1, and preferable range is 0.7～1.3: 1, and more preferably scope is 0.9～1.2: 1.The temperature of poor ammonium absorption liquid I is 50～85 ℃.The pH value of poor ammonium absorption liquid I is 2～6.5, and preferable range is 2.5～4.Wherein the oily-water seperating equipment upper outlet is removed light organic constituent, the heavy constituent that superpolymer and catalyst fines are removed in following outlet.The Analytic Tower temperature is 150～250 ℃, and pressure is the saturated vapor pressure of the solution under the relevant temperature.Used stripping gas is for to be inert gasses to the stripping thing in the Analytic Tower, and preferred version is for being selected from water vapor, air or nitrogen.The ammonia rectifying tower also can unite two into one with Analytic Tower, becomes associated plant.
Before rich ammonium absorption liquid gets into Analytic Tower, need not warming and pressurizing in the inventive method, handle polymkeric substance, need not handle through the wet oxidation operation.And wet oxidation need be carried out under HTHP, and energy consumption is higher, causes production cost to raise; Because operational condition is harsh, require also higher simultaneously to reactor material.So adopt present method to cut down the consumption of energy, reduce production costs.
Description of drawings
Fig. 1, Fig. 2 are process flow diagram of the present invention.
Among Fig. 1,1 is quench tower, and 2 is rich ammonium absorption liquid, and 3 is stripping tower, and 4 is light organic constituent; 5 is gaseous components such as vinyl cyanide, and 6 is stripping gas, and 7 is light organic constituent, and 8 is tripping device, 9 attach most importance to organic constituent and catalyst fineses; 10 is rich ammonium absorption liquid, and 11 is Analytic Tower, and 12 is poor ammonium absorption liquid, and 13 is thick ammonia; 14 is the ammonia rectifying tower, and 15 is rectifying still liquid, and 16 is anhydrous ammonia, and 17 is acrylonitrile reactor.
Among Fig. 2,1 is quench tower, and 2 is rich ammonium absorption liquid, and 3 is stripping tower; 4 is light organic constituent, and 5 is gaseous components such as vinyl cyanide, and 6 is stripping gas, and 7 is light organic constituent; 8 is tripping device, 9 attach most importance to organic constituent and catalyst fineses, and 10 is rich ammonium absorption liquid, 11 for resolving rectifying tower; 12 is poor ammonium absorption liquid, and 13 is anhydrous ammonia, and 14 is acrylonitrile reactor.
As shown in Figure 1; Acrylonitrile reactor gas obtains not ammoniated reaction gas 5 and rich ammonium absorption liquid 2 at quench tower 1 and the unreacted ammonia of poor ammonium absorption liquid 12 absorbing contacting; Rich ammonium absorption liquid 2 is removed light organic constituent 7 and heavy constituent 9 such as catalyzer, polymkeric substance obtain rich ammonium absorption liquid 10 through stripping gas 5 strippings to light organic constituent 4 back entering particular oils water separation device 8 at stripping tower 3; And then get into Analytic Tower 11 and resolve and obtain thick ammonia flow 13 and poor ammonium absorption liquid 12, poor ammonium absorption liquid 12 turns back to quench tower and is used to absorb unreacted ammonia.Thick ammonia flow 13 obtains anhydrous ammonia 16 at rectifying tower 14 and returns acrylonitrile reactor 17 and carry out oxidative ammonolysis after rectifying.
Flow process shown in Figure 2 and Fig. 1 basically identical, difference are that Analytic Tower and ammonia rectifying tower unite two into one, and resolve the bottom of tower, and rectifying is carried out on top.This technology can make spatial design compact.
Through embodiment the present invention is done further elaboration below.
Embodiment
[embodiment 1～6]
Embodiment by above processing condition are carried out all can be to the effective recycle that absorbs and can realize ammonia of the unreacted ammonia in the acrylonitrile reactor gas.
[comparative example 1～4]
Comparative example 1～4 is by the requirement method operation of patent CN1204620A institute, concrete processing condition such as following table.
Comparative example 1, comparative example 2 processing condition are identical with embodiment 3,4 respectively, but the too low desired temperature of wet oxidation reaction that do not reach of temperature, organism can't effectively be removed, and finally can't realize the recovery of unreacted ammonia.Comparative example 3 has been realized the recycling of ammonia, but the recovery of unreacted ammonia is lower than the embodiment 2 of same process condition, and comparative example 4 has reached the recovering effect identical with embodiment, and is temperature required but temperature is higher than embodiment far away.
Claims (8)
1. unreacted ammonia recycle and reuse method in the acrylonitrile reactor device may further comprise the steps:
The reaction gas I of (1) from ammonia oxidation reactor, coming out in quench tower with poor ammonium absorption liquid I absorbing contacting reaction gas in unreacted ammonia, obtain rich ammonium absorption liquid II and not ammoniated reaction gas II;
(2) rich ammonium absorption liquid II stripping in stripping tower is removed volatile organic constituent, in an oily-water seperating equipment, carry out separating treatment again, remove contained organism and superpolymer in the solution, obtain rich ammonium absorption liquid III; In Analytic Tower, heat rich ammonium absorption liquid III then, stripping obtains ammonia flow III and poor ammonium absorption liquid IV, and poor ammonium absorption liquid IV is returned the absorption that quench tower is used for unreacted ammonia;
(3) ammonia flow III rectifying separation in the ammonia rectifying tower obtains highly purified ammonia IV, returns ammonia oxidation reactor and reacts.
2. unreacted ammonia recycle and reuse method in the acrylonitrile reactor device according to claim 1 is characterized in that the oily-water seperating equipment upper outlet removes light organic constituent, the heavy constituent that superpolymer and catalyst fines are removed in following outlet.
3. unreacted ammonia recycle and reuse method in the acrylonitrile reactor device according to claim 1; It is characterized in that poor ammonium absorption liquid I and III are phosphoric acid, primary ammonium phosphate or its mixture; N/P mol ratio in the poor ammonium absorption liquid I is 05～1.5: 1; The pH value is 2～6.5, and temperature is 50～85 ℃.
4. unreacted ammonia recycle and reuse method is characterized in that in the acrylonitrile reactor device according to claim 3, the N/P mol ratio 0.7～1.3: 1 in poor ammonium absorption liquid I and the III, and the pH value is 2.5～4.
5. unreacted ammonia recycle and reuse method in the acrylonitrile reactor device according to claim 4 is characterized in that the N/P mol ratio in the poor ammonium absorption liquid I is 0.9～1.2: 1.
6. unreacted ammonia recycle and reuse method in the acrylonitrile reactor device according to claim 1, used stripping gas is for to be inert gasses to the stripping thing in the Analytic Tower.
7. unreacted ammonia recycle and reuse method in the acrylonitrile reactor device according to claim 6 is characterized in that used stripping gas is water vapor, air or nitrogen in the Analytic Tower.
8. unreacted ammonia recycle and reuse method in the acrylonitrile reactor device according to claim 1 is characterized in that the Analytic Tower temperature is 150～250 ℃, and pressure is the saturated vapor pressure of the solution under the relevant temperature.
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| Application Number | Priority Date | Filing Date | Title |
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| CN2010105136404A CN102452955A (en) | 2010-10-21 | 2010-10-21 | Method for recycling unreacted ammonia in acrylonitrile reaction device |
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| CN2010105136404A CN102452955A (en) | 2010-10-21 | 2010-10-21 | Method for recycling unreacted ammonia in acrylonitrile reaction device |
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Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103524380A (en) * | 2012-07-03 | 2014-01-22 | 中国石油化工股份有限公司 | Method for lowering organic matter content in absorption liquid during acrylonitrile non-ammonium-sulfate process |
| CN103521034A (en) * | 2012-07-03 | 2014-01-22 | 中国石油化工股份有限公司 | Improved method for resolving ammonium salt in acrylonitrile non-ammonium-sulfate process |
| CN103664693A (en) * | 2012-09-05 | 2014-03-26 | 中国石油化工股份有限公司 | Method for decomposing ammonium salt based on ammonium sulfate removal process by virtue of acrylonitrile reaction device |
| CN103664694A (en) * | 2012-09-05 | 2014-03-26 | 中国石油化工股份有限公司 | Method for lowering content of organic matters in absorption liquid in ammonium sulfate-free acrylonitrile technology |
| CN103739517A (en) * | 2012-10-17 | 2014-04-23 | 中国石油化工股份有限公司 | Improvement method for recycling and reusing unreacted ammonia in acrylonitrile reaction apparatus |
| CN106565538A (en) * | 2016-11-07 | 2017-04-19 | 上海东化环境工程有限公司 | Purification technology for acrylonitrile reaction gas |
| CN105668590B (en) * | 2014-11-20 | 2018-04-06 | 中国石油化工股份有限公司 | The absorption process of unreacted ammonia in acrylonitrile reactor device |
| CN109437099A (en) * | 2018-11-14 | 2019-03-08 | 李洁 | High-purity nitrogen technique is extracted in a kind of ammonia-contaminated gas |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1204620A (en) * | 1997-07-04 | 1999-01-13 | 标准石油公司 | Process for recovery and recycle of ammonia from acrylonitrile reactor efflvent stream using ammonium phosphate quench system |
| CN1324763A (en) * | 2000-05-23 | 2001-12-05 | 罗姆和哈斯公司 | Method for recovering and recirculating amonium from outflow from reactor |
| CN101027252A (en) * | 2004-07-22 | 2007-08-29 | 伊内奥斯美国公司 | Process for recovery and recycle of ammonia from a vapor stream |
| CN101092265A (en) * | 2006-06-21 | 2007-12-26 | 中国石油化工股份有限公司 | Method for treating wastewater of dilute thiamine |
-
2010
- 2010-10-21 CN CN2010105136404A patent/CN102452955A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1204620A (en) * | 1997-07-04 | 1999-01-13 | 标准石油公司 | Process for recovery and recycle of ammonia from acrylonitrile reactor efflvent stream using ammonium phosphate quench system |
| CN1324763A (en) * | 2000-05-23 | 2001-12-05 | 罗姆和哈斯公司 | Method for recovering and recirculating amonium from outflow from reactor |
| CN101027252A (en) * | 2004-07-22 | 2007-08-29 | 伊内奥斯美国公司 | Process for recovery and recycle of ammonia from a vapor stream |
| CN101092265A (en) * | 2006-06-21 | 2007-12-26 | 中国石油化工股份有限公司 | Method for treating wastewater of dilute thiamine |
Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103524380A (en) * | 2012-07-03 | 2014-01-22 | 中国石油化工股份有限公司 | Method for lowering organic matter content in absorption liquid during acrylonitrile non-ammonium-sulfate process |
| CN103521034A (en) * | 2012-07-03 | 2014-01-22 | 中国石油化工股份有限公司 | Improved method for resolving ammonium salt in acrylonitrile non-ammonium-sulfate process |
| CN103664693A (en) * | 2012-09-05 | 2014-03-26 | 中国石油化工股份有限公司 | Method for decomposing ammonium salt based on ammonium sulfate removal process by virtue of acrylonitrile reaction device |
| CN103664694A (en) * | 2012-09-05 | 2014-03-26 | 中国石油化工股份有限公司 | Method for lowering content of organic matters in absorption liquid in ammonium sulfate-free acrylonitrile technology |
| CN103739517A (en) * | 2012-10-17 | 2014-04-23 | 中国石油化工股份有限公司 | Improvement method for recycling and reusing unreacted ammonia in acrylonitrile reaction apparatus |
| CN105668590B (en) * | 2014-11-20 | 2018-04-06 | 中国石油化工股份有限公司 | The absorption process of unreacted ammonia in acrylonitrile reactor device |
| CN106565538A (en) * | 2016-11-07 | 2017-04-19 | 上海东化环境工程有限公司 | Purification technology for acrylonitrile reaction gas |
| CN106565538B (en) * | 2016-11-07 | 2019-03-15 | 上海东化环境工程有限公司 | A kind of purification process of acrylonitrile reactor gas |
| CN109437099A (en) * | 2018-11-14 | 2019-03-08 | 李洁 | High-purity nitrogen technique is extracted in a kind of ammonia-contaminated gas |
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Application publication date: 20120516 |