CN104326485A - Ammonia refining treatment process - Google Patents
Ammonia refining treatment process Download PDFInfo
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- CN104326485A CN104326485A CN201410533910.6A CN201410533910A CN104326485A CN 104326485 A CN104326485 A CN 104326485A CN 201410533910 A CN201410533910 A CN 201410533910A CN 104326485 A CN104326485 A CN 104326485A
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- Prior art keywords
- ammonia
- liquid
- gas
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- allowing
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- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 title claims abstract description 222
- 229910021529 ammonia Inorganic materials 0.000 title claims abstract description 105
- 238000000034 method Methods 0.000 title claims abstract description 38
- 238000007670 refining Methods 0.000 title claims abstract description 17
- 239000007789 gas Substances 0.000 claims abstract description 42
- 238000005406 washing Methods 0.000 claims abstract description 24
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 12
- 238000000746 purification Methods 0.000 claims abstract description 10
- 238000001179 sorption measurement Methods 0.000 claims abstract description 7
- 238000001816 cooling Methods 0.000 claims abstract description 5
- 238000003860 storage Methods 0.000 claims abstract description 5
- 238000011068 loading method Methods 0.000 claims abstract description 4
- 239000002994 raw material Substances 0.000 claims abstract description 4
- 238000002425 crystallisation Methods 0.000 claims description 6
- 239000012535 impurity Substances 0.000 claims description 6
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims description 4
- UCKMPCXJQFINFW-UHFFFAOYSA-N Sulphide Chemical compound [S-2] UCKMPCXJQFINFW-UHFFFAOYSA-N 0.000 claims description 4
- 229910052739 hydrogen Inorganic materials 0.000 claims description 4
- 239000001257 hydrogen Substances 0.000 claims description 4
- 230000008025 crystallization Effects 0.000 claims description 3
- 239000007791 liquid phase Substances 0.000 claims description 3
- 239000012530 fluid Substances 0.000 claims description 2
- RWSOTUBLDIXVET-UHFFFAOYSA-N Dihydrogen sulfide Chemical compound S RWSOTUBLDIXVET-UHFFFAOYSA-N 0.000 abstract description 14
- 229910000037 hydrogen sulfide Inorganic materials 0.000 abstract description 14
- 238000010521 absorption reaction Methods 0.000 abstract description 3
- 230000003009 desulfurizing effect Effects 0.000 abstract description 3
- 235000011114 ammonium hydroxide Nutrition 0.000 abstract description 2
- 238000007599 discharging Methods 0.000 abstract description 2
- 238000009834 vaporization Methods 0.000 abstract description 2
- 230000008016 vaporization Effects 0.000 abstract description 2
- 238000000926 separation method Methods 0.000 abstract 4
- 239000007788 liquid Substances 0.000 abstract 1
- 230000001105 regulatory effect Effects 0.000 abstract 1
- 229910052717 sulfur Inorganic materials 0.000 description 6
- 239000011593 sulfur Substances 0.000 description 6
- 238000005516 engineering process Methods 0.000 description 5
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical group [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 description 4
- 238000004140 cleaning Methods 0.000 description 2
- 238000004821 distillation Methods 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 230000007774 longterm Effects 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 description 1
- ISWSIDIOOBJBQZ-UHFFFAOYSA-N Phenol Chemical compound OC1=CC=CC=C1 ISWSIDIOOBJBQZ-UHFFFAOYSA-N 0.000 description 1
- 230000002378 acidificating effect Effects 0.000 description 1
- HIVLDXAAFGCOFU-UHFFFAOYSA-N ammonium hydrosulfide Chemical compound [NH4+].[SH-] HIVLDXAAFGCOFU-UHFFFAOYSA-N 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000003610 charcoal Substances 0.000 description 1
- 230000006835 compression Effects 0.000 description 1
- 238000007906 compression Methods 0.000 description 1
- 125000004122 cyclic group Chemical group 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 239000000428 dust Substances 0.000 description 1
- 238000005265 energy consumption Methods 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 150000002894 organic compounds Chemical class 0.000 description 1
- 239000000047 product Substances 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 239000013589 supplement Substances 0.000 description 1
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Abstract
An ammonia refining treatment process comprises the steps: cooling raw material gas ammonia containing hydrogen sulfide and water, and then allowing to go into a gas ammonia liquid-separation tank; allowing liquid gas ammonia flowing out of the gas ammonia liquid-separation tank to go into the bottom of a washing tower, and carrying out contact washing with concentrated ammonia liquor; after the washed gas ammonia passes through the washing tower, allowing to go into the bottom of an ammonia crystallizer from the tower top of the washing tower, and crystallizing; purifying sequentially through an adsorption tower, a desulfurizing tower and an impurity-removal liquid-separation tank; allowing the gas ammonia after purification to go into a heat regulator, and preheating; then allowing to go into an ammonia rectification unit; and then liquefying into liquid ammonia through a condensing cooler and an oil-separation tank, allowing the liquid ammonia to go to a liquid ammonia circulating tank, allowing a part of liquid ammonia to go to the washing tower and the ammonia crystallizer by self pressure, allowing the other part to go to a liquid ammonia storage tank, pressurizing by a liquid ammonia loading pump, and discharging out of the device. By using self-made liquid ammonia for vaporization, process temperatures of the absorption tower and the ammonia crystallizer are regulated, and the process has the advantages of easy availability of cold source, low cost, simple operation, and stable and reliable operation performance.
Description
Technical field
The invention belongs to technical field of petrochemical industry, be specifically related to a kind of Crude ammonia purification technique.
Background technology
In the gas ammonia that technical field of petrochemical industry acidic water stripping device reclaims, containing oil, hydrogen sulfide, water, phenol and other organic compound and solid dust, the task of ammonia refining improves purity, reduces impurity, especially will reduce hydrogen sulfide content.Namely thick ammonia is purified.Existing thick ammonia purification processes technique mainly contains following three kinds.
The first strong aqua circulation cleaning method: strong aqua circulation cleaning method is through washing tower by moisture for stripping sulfur-bearing out gas ammonia unstripped gas, with recycle pump, strong aqua is beaten to tower top, the impurity such as the hydrogen sulfide below 10 DEG C in absorbing ammonia, water, to reach the object of thick ammonia purification.German Patent DD255720, U.S. US4060591 adopt strong aqua circulation cleaning--and liquefied ammonia washing method is refined, obtain liquefied ammonia purity higher than 99.5%, hydrogen sulfide content can be controlled in below 10ppm, but this explained hereafter flow process is complicated, dynamic equipment used is many, not only operational difficulty, energy consumption is high, and hydrogen sulfide stripping is complete not.
The second crystallization-absorption-fine de-sulfur method: be that stripping sulfur-bearing out moisture gas ammonia unstripped gas is first sloughed most of hydrogen sulfide and water through liquefied ammonia crystallisation by cooling, then through r-Al
2o
3or charcoal absorption, compression, then further refiningly remove remaining hydrogen sulfide, finally reach the object of thick ammonia purification.Adopt crystallization-absorption-fine desulfurizing technology to refine gas ammonia, the liquefied ammonia hydrogen sulfide content of gained can be controlled in below 10ppm.But the shortcoming of this technique is hydrogen sulfide and water to be removed not exclusively, it is not high, understable that gained refines liquefied ammonia purity, and flow operations is loaded down with trivial details, and intensity is large.
The third is that Chinese patent specification sheets CN1047366C discloses a kind of gas ammonia process for refining, adopt washing-crystallization-absorption-fine desulfurizing technology flow process, after the gas ammonia of stripper plant stripping sulfide hydrogen out and water is cooled to less than 40 DEG C separatory, make the hydrogen sulfide in gas ammonia and water-content be stabilized in about 1 % by weight and enter washing tower, the temperature of washing tower controls below 10 DEG C, in the rear gas ammonia of washing, the content of hydrogen sulfide and water is lower than 200ppm, enter crystallisation adsorption tank again, finally carry out fine de-sulfur, the purity of the refining liquefied ammonia obtained can reach 99.8%, hydrogen sulfide content is at below 1ppm.The shortcoming of this technique is that the gas ammonia temperature owing to entering washing tower is higher, cause the hydrogen sulfide in gas ammonia and water-content higher, the cyclic ammonia water concentration of washing is reduced, for ensureing washing effect, often must supplement liquefied ammonia, the sulfur-bearing strong aqua of simultaneously discharging is also more, increases the quantity discharged of sulfur-bearing strong aqua, sour water load is increased.This technique also exists crystallisation adsorption in addition needs interruption discharge opeing, and operating process is complicated, and required equipment is more, and floor space is large, and ammonia compressor also often occurs all kinds of fault in actual moving process, can not the effective guarantee device shortcoming run steady in a long-term.
Summary of the invention
Technological deficiencies such as the present invention is directed to prior art and there is flow process complexity, remove not exclusively, the large and actually operating of occupation area of equipment is difficult, on the basis of fully receiving existing gas ammonia process for refining advantage, distillation technology is combined with thick ammonia purification technique, forms following technical scheme.
A kind of ammonia refining treatment process, by the raw material gas ammonia of sulfide hydrogen and water, enters gas ammonia and divides flow container after cooling; The liquid phase gas ammonia that gas ammonia divides flow container to flow out enters wash tower bottoms and contacts with strong aqua and wash; Gas ammonia after washing carries out crystallization by entering ammonia crystalliser feet by tower top after washing tower; Flow container is divided to purify by adsorption tower, thionizer and removal of impurities successively again; Gas ammonia after purification enters into heat regulator and carries out preheating; Then ammonia rectification cell is entered into; Enter into liquefied ammonia circulation tank by being liquefied as liquefied ammonia after condensate cooler, point oil tank again, wherein a part of liquefied ammonia self-pressure removes washing tower and ammonia crystallizer, and another part then goes in liquid ammonia storage tank, after the pressurization of liquefied ammonia Loading Pump, go out device.
Further, a kind of ammonia rectification cell of ammonia refining treatment process comprises side cooler, gas ammonia compressor, heat exchanger.
Further, a kind of ammonia rectification cell quantity of ammonia refining treatment process is at least 2.
Further, a kind of ammonia crystallizer of ammonia refining treatment process is 2.
Further, a kind of heat regulator of ammonia refining treatment process adopts circulating backwater as hot-fluid.
The beneficial effect that the present invention compared with prior art produces is embodied in:
1, be mainly distillation technology to combine with thick ammonia purification technique, form the washing having more technical superiority--crystallization--the COMBINED PROCESS flow process of absorption--fine de-sulfur--rectifying.
2, utilize the present invention to make liquid ammonia vaporization by oneself to realize the regulation and control of absorption tower and ammonia crystallizer process temperature, there is low-temperature receiver and be easy to get, the effect of low cost, do not need additional input liquefied ammonia.
3, present invention process flow process equipment used is chemical industry common equipment, and its stable performance is relatively higher, and actually operating difficulty also relatively more simply easily, is more suitable for ensureing normal production steady in a long-term.
4, utilize the present invention not only hydrogen sulfide remove fully thoroughly, technique actually operating difficulty is little, and equipment is chemical industry common equipment, and operating performance is reliable and stable, and counter investment cost is also less.
Accompanying drawing explanation
Fig. 1 is process flow sheet of the present invention;
Fig. 2 is another kind of process flow sheet of the present invention;
Wherein: 1 gas ammonia divides flow container, 2 washing towers, 3 ammonia crystallizers, 4 adsorption towers, 5 thionizers, 6 removal of impurities to divide flow container, 7 heat regulators, 8 ammonia rectification cells, 81 side coolers, 82 gas ammonia compressors, 83 heat exchangers, 84 gas ammonia compressors, 9 condensate coolers, 10 points of oil tanks, 11 liquefied ammonia circulation tanks, 12 liquid ammonia storage tanks, 13 products pots.
Embodiment
By the raw material gas ammonia of sulfide hydrogen and water, enter gas ammonia after cooling and divide flow container; The liquid phase gas ammonia that gas ammonia divides flow container to flow out enters wash tower bottoms and contacts with strong aqua and wash; Gas ammonia after washing carries out crystallization by entering ammonia crystalliser feet by tower top after washing tower; Flow container is divided to purify by adsorption tower, thionizer and removal of impurities successively again; Gas ammonia after purification enters into heat regulator and carries out preheating; Then ammonia rectification cell is entered into; Enter into liquefied ammonia circulation tank by being liquefied as liquefied ammonia after condensate cooler, point oil tank again, wherein a part of liquefied ammonia self-pressure removes washing tower and ammonia crystallizer, and another part then goes in liquid ammonia storage tank, after the pressurization of liquefied ammonia Loading Pump, go out device.
Claims (5)
1. an ammonia refining treatment process, is characterized in that:
By the raw material gas ammonia of sulfide hydrogen and water, enter gas ammonia after cooling and divide flow container; The liquid phase gas ammonia that gas ammonia divides flow container to flow out enters wash tower bottoms and contacts with strong aqua and wash; Gas ammonia after washing carries out crystallization by entering ammonia crystalliser feet by tower top after washing tower; Flow container is divided to purify by adsorption tower, thionizer and removal of impurities successively again; Gas ammonia after purification enters into heat regulator and carries out preheating; Then ammonia rectification cell is entered into; Enter into liquefied ammonia circulation tank by being liquefied as liquefied ammonia after condensate cooler, point oil tank again, wherein a part of liquefied ammonia self-pressure removes washing tower and ammonia crystallizer, and another part then goes in liquid ammonia storage tank, after the pressurization of liquefied ammonia Loading Pump, go out device.
2. ammonia refining treatment process according to claim 1, is characterized in that: described ammonia rectification cell comprises side cooler, gas ammonia compressor, heat exchanger.
3. ammonia refining treatment process according to claim 1, is characterized in that: described ammonia rectification cell quantity is at least 2.
4. ammonia refining treatment process according to claim 1, is characterized in that: described ammonia crystallizer is 2.
5. ammonia refining treatment process according to claim 1, is characterized in that: described heat regulator adopts circulating backwater as hot-fluid.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201410533910.6A CN104326485A (en) | 2014-10-12 | 2014-10-12 | Ammonia refining treatment process |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201410533910.6A CN104326485A (en) | 2014-10-12 | 2014-10-12 | Ammonia refining treatment process |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN104326485A true CN104326485A (en) | 2015-02-04 |
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| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201410533910.6A Pending CN104326485A (en) | 2014-10-12 | 2014-10-12 | Ammonia refining treatment process |
Country Status (1)
| Country | Link |
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| CN (1) | CN104326485A (en) |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105645358A (en) * | 2016-03-14 | 2016-06-08 | 衢州市鼎盛化工科技有限公司 | Method for preparing hydrogen fluoride from fluosilicic acid |
| CN106115736A (en) * | 2016-06-29 | 2016-11-16 | 王文领 | Decarbonization and desulfurization method for crude ammonia gas stripped by coal chemical conversion condensate |
| CN106395857A (en) * | 2016-08-29 | 2017-02-15 | 北方华锦化学工业集团有限公司 | Liquid ammonia refining decolorization system and method |
| CN107946687A (en) * | 2017-12-08 | 2018-04-20 | 天齐锂业股份有限公司 | A kind of system and technique for continuously recycling waste and old ternary lithium ion battery |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1167084A (en) * | 1996-05-14 | 1997-12-10 | 中国石化茂名石油化工公司 | Technology for refining ammonia |
| CN1587045A (en) * | 2004-08-16 | 2005-03-02 | 中国石油化工集团公司 | Ammonia refining combined process |
-
2014
- 2014-10-12 CN CN201410533910.6A patent/CN104326485A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1167084A (en) * | 1996-05-14 | 1997-12-10 | 中国石化茂名石油化工公司 | Technology for refining ammonia |
| CN1587045A (en) * | 2004-08-16 | 2005-03-02 | 中国石油化工集团公司 | Ammonia refining combined process |
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105645358A (en) * | 2016-03-14 | 2016-06-08 | 衢州市鼎盛化工科技有限公司 | Method for preparing hydrogen fluoride from fluosilicic acid |
| CN106115736A (en) * | 2016-06-29 | 2016-11-16 | 王文领 | Decarbonization and desulfurization method for crude ammonia gas stripped by coal chemical conversion condensate |
| CN106115736B (en) * | 2016-06-29 | 2018-02-27 | 王文领 | Decarbonization and desulfurization method for crude ammonia gas stripped by coal chemical conversion condensate |
| CN106395857A (en) * | 2016-08-29 | 2017-02-15 | 北方华锦化学工业集团有限公司 | Liquid ammonia refining decolorization system and method |
| CN107946687A (en) * | 2017-12-08 | 2018-04-20 | 天齐锂业股份有限公司 | A kind of system and technique for continuously recycling waste and old ternary lithium ion battery |
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| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| C02 | Deemed withdrawal of patent application after publication (patent law 2001) | ||
| WD01 | Invention patent application deemed withdrawn after publication |
Application publication date: 20150204 |