CN1024123C - Method for producing concentrated ammonia water or anhydrous ammonia by recovering ammonia - Google Patents
Method for producing concentrated ammonia water or anhydrous ammonia by recovering ammonia Download PDFInfo
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- CN1024123C CN1024123C CN 90103868 CN90103868A CN1024123C CN 1024123 C CN1024123 C CN 1024123C CN 90103868 CN90103868 CN 90103868 CN 90103868 A CN90103868 A CN 90103868A CN 1024123 C CN1024123 C CN 1024123C
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- Prior art keywords
- ammonia
- tower
- desorption tower
- desorption
- rectifying
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- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
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- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 title claims abstract description 114
- 229910021529 ammonia Inorganic materials 0.000 title claims abstract description 48
- 235000011114 ammonium hydroxide Nutrition 0.000 title abstract description 13
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 title abstract description 5
- 238000004519 manufacturing process Methods 0.000 title abstract description 3
- 238000003795 desorption Methods 0.000 claims abstract description 53
- 238000000034 method Methods 0.000 claims abstract description 12
- 238000010992 reflux Methods 0.000 claims abstract description 11
- MNNHAPBLZZVQHP-UHFFFAOYSA-N diammonium hydrogen phosphate Chemical compound [NH4+].[NH4+].OP([O-])([O-])=O MNNHAPBLZZVQHP-UHFFFAOYSA-N 0.000 claims abstract description 6
- 239000004254 Ammonium phosphate Substances 0.000 claims abstract description 5
- 229910000148 ammonium phosphate Inorganic materials 0.000 claims abstract description 5
- 235000019289 ammonium phosphates Nutrition 0.000 claims abstract description 5
- QLULGSLAHXLKSR-UHFFFAOYSA-N azane;phosphane Chemical compound N.P QLULGSLAHXLKSR-UHFFFAOYSA-N 0.000 claims description 17
- 238000010521 absorption reaction Methods 0.000 claims description 6
- 239000007788 liquid Substances 0.000 claims description 6
- 239000003034 coal gas Substances 0.000 abstract description 7
- 238000010438 heat treatment Methods 0.000 abstract description 7
- 239000000571 coke Substances 0.000 abstract description 2
- 230000009615 deamination Effects 0.000 abstract description 2
- 238000006481 deamination reaction Methods 0.000 abstract description 2
- 239000007789 gas Substances 0.000 description 10
- 239000000243 solution Substances 0.000 description 9
- XKMRRTOUMJRJIA-UHFFFAOYSA-N ammonia nh3 Chemical compound N.N XKMRRTOUMJRJIA-UHFFFAOYSA-N 0.000 description 5
- 239000002351 wastewater Substances 0.000 description 5
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 5
- LELOWRISYMNNSU-UHFFFAOYSA-N hydrogen cyanide Chemical compound N#C LELOWRISYMNNSU-UHFFFAOYSA-N 0.000 description 4
- UHOVQNZJYSORNB-UHFFFAOYSA-N Benzene Chemical compound C1=CC=CC=C1 UHOVQNZJYSORNB-UHFFFAOYSA-N 0.000 description 3
- RWSOTUBLDIXVET-UHFFFAOYSA-N Dihydrogen sulfide Chemical compound S RWSOTUBLDIXVET-UHFFFAOYSA-N 0.000 description 3
- 238000009833 condensation Methods 0.000 description 3
- 230000005494 condensation Effects 0.000 description 3
- 238000005516 engineering process Methods 0.000 description 3
- 230000001105 regulatory effect Effects 0.000 description 3
- QGZKDVFQNNGYKY-UHFFFAOYSA-O Ammonium Chemical compound [NH4+] QGZKDVFQNNGYKY-UHFFFAOYSA-O 0.000 description 2
- 241000282326 Felis catus Species 0.000 description 2
- YFYIWIZSIVZILB-UHFFFAOYSA-N N.[P] Chemical compound N.[P] YFYIWIZSIVZILB-UHFFFAOYSA-N 0.000 description 2
- NBIIXXVUZAFLBC-UHFFFAOYSA-N Phosphoric acid Chemical compound OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 description 2
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 description 2
- 239000003513 alkali Substances 0.000 description 2
- 230000004087 circulation Effects 0.000 description 2
- 229910000037 hydrogen sulfide Inorganic materials 0.000 description 2
- 229910052698 phosphorus Inorganic materials 0.000 description 2
- 239000011574 phosphorus Substances 0.000 description 2
- 238000003825 pressing Methods 0.000 description 2
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 description 1
- 229910000831 Steel Inorganic materials 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 230000006978 adaptation Effects 0.000 description 1
- 229910000147 aluminium phosphate Inorganic materials 0.000 description 1
- LFVGISIMTYGQHF-UHFFFAOYSA-N ammonium dihydrogen phosphate Chemical compound [NH4+].OP(O)([O-])=O LFVGISIMTYGQHF-UHFFFAOYSA-N 0.000 description 1
- 238000005915 ammonolysis reaction Methods 0.000 description 1
- 235000011089 carbon dioxide Nutrition 0.000 description 1
- 239000003245 coal Substances 0.000 description 1
- 230000001276 controlling effect Effects 0.000 description 1
- 238000001816 cooling Methods 0.000 description 1
- 230000007812 deficiency 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
- 230000005611 electricity Effects 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 238000000746 purification Methods 0.000 description 1
- 150000003839 salts Chemical class 0.000 description 1
- 239000008234 soft water Substances 0.000 description 1
- 239000010959 steel Substances 0.000 description 1
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Abstract
The present invention is an improved process for preparing concentrated ammonia water or anhydrous ammonia. The method adopts ammonium phosphate solution to absorb ammonia, and produces the product through pressure desorption or rectification. The desorption tower is provided with a reflux device; the desorption and rectification processes adopt 0.78-1.18MPa steam for indirect heating and are two independent systems. After deamination, the content of the coal gas in the tower can reach 0.1g/Nm3The ammonia content of the concentrated ammonia water is 18-30%, and the mass of anhydrous ammonia is more than 99.6%. The method is suitable for recovering ammonia in coke oven gas of a coke-oven plant.
Description
The present invention is applied to the coke oven gas purification field.
The invention relates to a kind of ammonia that from coke-oven gas, reclaims and produce improving one's methods of strong aqua or anhydrous ammonia.
Not Sa mother (PHOSAM) law technology (U.S. Pat P3024090, USP3186795) of at present existing United States Steel Corporation exploitation is to adopt phosphorus ammonia liquation to reclaim ammonia from coke-oven gas, this method is suitability for industrialized production, use the above middle pressure steam of 2.1MPa, desorption tower and rectifying tower are the open steam heating, and anhydrous ammonia is unique product of this technology.When desorption pressures was 1.38MPa, the ammonia vapour concentration was 29% in this technology; When desorption pressures was 0.69MPa, the ammonia vapour concentration was 17%; When desorption pressures was lower than 0.69MPa, the dilution of ammonia concentration disproportionately increased in the steam; When under the normal pressure during desorb, the content that leaves ammonia in the desorption tower overhead vapor only is 11%.This ammonia steam or directly introduce rectifying tower perhaps is condensed into ammoniacal liquor and pumps into rectifying tower rectifying.When desorption tower pressure was low, anhydrous ammonia was produced in obviously a large amount of lower title ammoniacal liquor rectifying of concentration, not only make the corresponding increase of rectifying device, and product is single, had simultaneously also correspondingly increased steam, water and power consumption.
For overcoming above-mentioned deficiency, the present invention can not only can produce the strong aqua of 18-30% concentration but also can further produce the anhydrous ammonia product not being subjected to reclaim ammonia under the situation that the desorption tower working pressure changes and steam condition limits from coke-oven gas.
The present invention be a kind of be absorption liquid with the ammonium phosphate solution, from coke-oven gas, absorb ammonia, produce strong aqua through pressing and desorption, or strong aqua is produced the method for anhydrous ammonia again through rectifying, the characteristics of this method are that desorption tower is provided with reflux and controls ammonia concn, desorption tower and rectifying tower adopt indirect steam heating (vapor pressure is 0.78-1.18MPa), and desorb and rectifying are respectively two independent systems.To introduce desorption tower behind the heat-eliminating medium of part phosphorus ammonium pregnant liquor as reflux, all the other phosphorus ammonia rich solutions are directly introduced desorption tower, and regulate the size of directly introducing the phosphorus ammonium pregnant liquor amount of desorption tower and control ammonia concn.Be provided with reflux at the pressing and desorption top of tower among the present invention, the ammonia steam that leaves the desorption tower cat head is through desorption tower partial condenser partial condensation, the concentration of ammonia is further concentrated in the steam, phlegma is back to the desorption tower top, and uncooled ammonia steam cools off the strong aqua product that obtains 18-30% in the ammoniacal liquor condensate cooler.Need the phosphorus ammonium pregnant liquor of desorb to be divided into two partly, the a part of desorption tower of directly introducing, another partly carries out heat exchange through desorption tower partial condenser and desorption tower tower top outlet ammonia steam, with the condensation of ammonia vapor portion, the ammonia vapour concentration of leaving the desorption tower partial condenser is improved.How much controlling of the phosphorus ammonium pregnant liquor of the size of quantity of reflux by introducing the desorption tower partial condenser perhaps regulated the size of directly introducing the phosphorus ammonium pregnant liquor amount of desorption tower and controlled.The concentration of strong aqua product can be regulated with the size of quantity of reflux.Desorption tower, rectifying tower are the heating of well heater indirect steam, and vapor pressure can be more than 0.78MPa.The desorption tower working pressure is 0.49-0.78MPa.Phosphorus ammonium pregnant liquor obtains 18-30% normal pressure strong aqua product through desorb.The rectifying tower working pressure is 1.37-1.57MPa, and strong aqua obtains 99.6% above anhydrous ammonia through rectifying.Pressure between desorb and the rectifying falls and makes desorption process and rectifying be respectively two independent systems.The wastewater temperature of discharging at the bottom of the rectifying Tata is introduced this wastewater of rectification in weak ammonia ammonia still among the present invention more than 170 ℃ and certain pressure is arranged, and vacuum flashing has 15% to become steam approximately, and flash section is not incorporated in the weak ammonia ammonia still.
Characteristics of the present invention have tangible advantage: the concentration of product strong aqua can be controlled by regulating quantity of reflux, and the result can make the working pressure of desorption tower reduce or can improve the ammonia concn of desorption tower when low voltage operated.If want desorb to obtain 29% strong aqua, the desorption tower working pressure can be reduced to about 0.8MPa by original 1.38MPa.And original under 0.69MPa pressure desorb only can obtain the ammoniacal liquor of 17% concentration, concentration can bring up to 26% now.When producing the 18-30% strong aqua, can reduce the working pressure of desorption tower.Employing indirect steam heating makes desorb, rectifying more extensive to the adaptation of vapor pressure condition, has the above steam of 0.78MPa and just can satisfy processing requirement, has enlarged the process application scope.Owing to improved ammonia concn, when further producing anhydrous ammonia again, help the operation of rectifying tower, also can reduce the consumption of steam in the rectifying, water, electricity.Desorb and rectifying are divided into two independent systems, can make corresponding flexible operation, convenience.Also changed simultaneously the kind of ammonolysis product, both can produce the strong aqua product of 18-30%, can as required or produce strong aqua again or produce anhydrous ammonia.
Accompanying drawing is the block diagram of drawing according to the present invention.Coke-oven gas after cold, electric fishing just enters ammonia absorption tower 2, absorbs ammonia in the coal gas with two sections circulations of ammonium phosphate solution, behind the deamination coal gas to eventually cold, take off benzene after operation handle.Phosphorus ammonium pregnant liquor behind the suction ammonia enters desorption tower [6] through poor rich liquid heat exchanger [4], contactor [5], desorption tower partial condenser [8].The phosphorus ammonium pregnant liquor desorb provides thermal source by the heating of desorption tower bottom heater [7] indirect steam.Ammonia in the phosphorus ammonium pregnant liquor is steamed by desorb in desorption tower [6], through desorption tower partial condenser [8] partial condensation, passes back into desorption tower [6] top, and uncooled strong ammonia gas obtains the strong aqua product of 18-30% through ammoniacal liquor condensate cooler [9] cooling.The concentration of strong aqua can be controlled by the quantity of reflux size, and the size of quantity of reflux can by entering how much the adjusting of phosphorus ammonium pregnant liquor amount that desorption tower partial condenser [8] carries out heat exchange.Desorption tower [6] bottom phosphorus ammonium barren liquor returns ammonia absorption tower [2] through poor rich liquid heat exchanger [4], lean solution water cooler [3] and reuptakes ammonia in the coal vapour.Strong aqua is if further be processed into anhydrous ammonia, and then strong aqua is adding alkali after ammoniacal liquor preheater [10] enters rectifying tower [11].Rectifying tower is heated by bottom heater [12] indirect steam.The dense ammonia that leaves rectifying tower [11] top after the rectifying is cooled to the anhydrous ammonia product through total condenser [13], is partly refluxed to rectifying tower [11] top.The waste water of rectifying tower [11] bottom is delivered to weak ammonia ammonia still [1] as the thermal source that claims ammoniacal liquor ammonia still process.Distilled ammonia wastewater goes biochemical treatment after heat exchange.Leaving sour gas such as hydrogen sulfide that ammonia, hydrogen sulfide, the prussic acid gas of weak ammonia ammonia still [1] cat head decomposites with contactor [5], prussic acid, carbonic acid gas sends into and inhales gas line before the ammonia.
The embodiment that the present invention provides is as follows: with the coal gas treatment scale is 14,500Nm
3The coke-oven plant of/h is an example, and ammonia content is 9g/Nm in the raw gas
3Two sections circulations of ammonium phosphate solution absorb the ammonia in the coal gas in ammonia absorption tower [2].It is 40 ℃ that lean solution is gone into the tower temperature, and primary ammonium phosphate and Secondary ammonium phosphate are 322g/l at salt total concn C in the lean solution, and the mol ratio R of its ammonia and phosphoric acid is 1.25.When phosphorus ammonium pregnant liquor went out tower, C was 345g/l in the rich solution, and R is 1.75.Coal gas is gone into 40 ℃ of tower temperature, and 45 ℃ of tower exit temperatures go out in the tower coal gas ammonia content less than 0.1g/Nm
3
Phosphorus ammonium pregnant liquor ℃ is sent into contactor [5] through poor rich liquid heat exchanger [4] heat exchange to 95, and the contactor service temperature is 98 ℃.Reduce sourness behind the gas, phosphorus ammonium pregnant liquor ℃ enters the desorption tower [6] of 30 blocks of column plates through desorption tower partial condenser [8] heat exchange to 145.Desorption tower [6] working pressure is 0.5-0.8MPa, and the bottom is heated with the 0.78-1.18MPa indirect steam by well heater [7].The ammonia vapour that desorption tower [6] top is 150 ℃ is condensed to 90 ℃ through desorption tower partial condenser [8], and phlegma passes back into desorption tower [6] top.It is 35 ℃ that uncooled strong ammonia gas further is cooled to temperature at ammoniacal liquor condensate cooler [9], and concentration is 30% strong aqua product.The 170 ℃ of phosphorus ammonium barren liquors in desorption tower [6] bottom are cooled to 100 ℃ through poor rich liquid heat exchanger [4] heat exchange, further are cooled to 40 ℃ through lean solution water cooler [3] again and return ammonia absorption tower [2].C is 322g/l in the phosphorus ammonium barren liquor, and R is 1.25, and the about 345kg/h of the water that loses in the system replenishes in the epimere recycle system with soft water.
If strong aqua further is processed as anhydrous ammonia, be 35 ℃ then with temperature, concentration is 30% strong aqua, adds alkali before pump, remove acid composition after, be heated to 150 ℃ through ammoniacal liquor preheater [10] again, enter the rectifying tower [11] of 40 blocks of column plates.Rectifying tower [11] working pressure is 1.6MPa, adopts 0.78-1.18MPa steam indirect heating by well heater [12] at the bottom of the tower.The dense ammonia that rectifying tower [11] top is 38 ℃ is cooled to anhydrous ammonia under the normal temperature through total condenser [13].Part liquefied ammonia is back to rectifying tower [11] top.Finally obtain the 130kg/h ammonia content approximately at the liquefied ammonia product more than 99.6%.The waste water of rectifying tower [11] bottom is delivered to weak ammonia ammonia still [1] as thermal source utilization or processing.
Claims (1)
1, a kind of is that absorption liquid absorbs ammonia is produced strong aqua through desorb method with the ammonium phosphate solution from coke-oven gas, be characterised in that altogether desorption tower is provided with reflux, introduce desorption tower behind the heat-eliminating medium of part phosphorus ammonium pregnant liquor as reflux, all the other phosphorus ammonium pregnant liquors are directly introduced desorption tower, and regulate the size of directly introducing the phosphorus ammonium pregnant liquor amount of desorption tower and control ammonia concn; Desorption tower adopts between steam and heats, and vapor pressure is 0.78-1.18MPa.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 90103868 CN1024123C (en) | 1990-05-24 | 1990-05-24 | Method for producing concentrated ammonia water or anhydrous ammonia by recovering ammonia |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 90103868 CN1024123C (en) | 1990-05-24 | 1990-05-24 | Method for producing concentrated ammonia water or anhydrous ammonia by recovering ammonia |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN1056665A CN1056665A (en) | 1991-12-04 |
| CN1024123C true CN1024123C (en) | 1994-04-06 |
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| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN 90103868 Expired - Lifetime CN1024123C (en) | 1990-05-24 | 1990-05-24 | Method for producing concentrated ammonia water or anhydrous ammonia by recovering ammonia |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN1024123C (en) |
Families Citing this family (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1043135C (en) * | 1995-09-18 | 1999-04-28 | 宗立海 | Process for recovering high purity liquid ammonia from oil-refining waste water |
| CN101544380B (en) * | 2009-04-29 | 2010-12-01 | 宝钢工程技术集团有限公司 | System for producing strong ammonia water by absorbing ammonia in air |
| CN104211244B (en) * | 2013-06-03 | 2016-02-03 | 洁海瑞泉膜技术（北京）有限公司 | Renewable and the gaseous state embrane method process of by-product strong aqua of a kind of absorption agent is containing the method for ammonia feed liquid or waste water |
| CN104355321B (en) * | 2014-10-23 | 2016-06-08 | 中冶焦耐工程技术有限公司 | Process and device for producing concentrated ammonia water by washing ammonia with ammonium phosphate with controllable concentration of product ammonia water |
| CN110280104A (en) * | 2019-06-24 | 2019-09-27 | 天华化工机械及自动化研究设计院有限公司 | A kind of phosphorus ammonium method processing catalyst ammonia-contaminated gas and ammonia reclaiming process |
| CN110745842B (en) * | 2019-10-31 | 2023-05-02 | 韶关凯鸿纳米材料有限公司 | Deamination heat exchange recovery system and use method |
| CN111087004A (en) * | 2019-12-23 | 2020-05-01 | 首钢水城钢铁（集团）有限责任公司 | Method for treating residual ammonia water in coal gasification production and recovery of coke oven |
-
1990
- 1990-05-24 CN CN 90103868 patent/CN1024123C/en not_active Expired - Lifetime
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| Publication number | Publication date |
|---|---|
| CN1056665A (en) | 1991-12-04 |
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