CN104437004A - Method suitable for controlling concentration of hydrogen sulfide tail gas in low-temperature methanol washing process - Google Patents
Method suitable for controlling concentration of hydrogen sulfide tail gas in low-temperature methanol washing process Download PDFInfo
- Publication number
- CN104437004A CN104437004A CN201410687078.5A CN201410687078A CN104437004A CN 104437004 A CN104437004 A CN 104437004A CN 201410687078 A CN201410687078 A CN 201410687078A CN 104437004 A CN104437004 A CN 104437004A
- Authority
- CN
- China
- Prior art keywords
- gas
- solution
- sulfide
- methanol
- reabsorber
- Prior art date
- 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.)
- Granted
Links
Classifications
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P70/00—Climate change mitigation technologies in the production process for final industrial or consumer products
- Y02P70/10—Greenhouse gas [GHG] capture, material saving, heat recovery or other energy efficient measures, e.g. motor control, characterised by manufacturing processes, e.g. for rolling metal or metal working
Landscapes
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
- Industrial Gases (AREA)
- Gas Separation By Absorption (AREA)
Abstract
The invention discloses a method suitable for controlling the concentration of hydrogen sulfide tail gas in a low-temperature methanol washing process. The method comprises the steps that a sulfur-bearing methanol rich solution dissolved with sulfide and carbon dioxide is subjected to flash evaporation via a medium-pressure flash evaporation tower; fuel gas such as CH4, CO and H2 dissolved in the solution is desorbed and recovered; the methanol solution after the flash evaporation is subjected to pressure reduction and gas stripping to allow a carbon dioxide component to be desorbed from the solution; sulfide is still dissolved in the methanol solution via secondary washing and absorption of the solution to achieve sulfide enrichment; the sulfur-bearing methanol rich solution is heated and then subjected to the flash evaporation; flash evaporation gas returns to a secondary absorption tower to strengthen the sulfide enrichment; the obtained sulfur-bearing methanol solution enters a heat regeneration tower to allow sulfide and residual CO2 to be fully desorbed by the action of steam stripping of methanol steam; and non-condensable gas, namely the acid sulfide tail gas is obtained by further condensation and cooling via a tail gas heat exchanger and a hydrogen sulfide tail gas chiller. The method has the advantages that the method is energy-saving and consumption-reducing, and can adapt to different sulfur recovery technology requirements.
Description
Technical field
The present invention relates to a kind of method controlling hydrogen sulfide tail gas concentration in applicable low-temperature rectisol process.
Background technology
Desulfurization in chemical process, the acid qi exhaustion of decarburization are except extensively adopting low-temp methanol washing process, and in low-temperature rectisol process for purifying process, the impurity compositions such as the carbon dioxide in raw material process gas and hydrogen sulfide are removed through methanol solvate washing absorption totally.Process gas after purification is used to rear operation and produces, and absorb the methanol solution of carbon dioxide and these impurity compositions of hydrogen sulfide through vacuum flashing, air lift, the regenerative process Posterior circle such as hot recycling use, produce carbon dioxide in the process, sulfide emission tail gas, wherein the acid tail gas of sulfide hydrogen component also should supporting sulfur recovery unit to meet environmental protection requirement and the byproduct such as Recovered sulphur or sulfuric acid, but different sulfur recovery technology has different requirement to the concentration of hydrogen sulfide in tail gas, particularly when in unstripped gas, sulfur content amplitude of variation is larger, in acid tail gas, concentration of hydrogen sulfide fluctuation can cause adverse effect to sulfur recovery operation.
Summary of the invention
The object of this invention is to provide a kind of energy-saving and cost-reducing, can adapt to the method controlling hydrogen sulfide tail gas concentration in the applicable low-temperature rectisol process of different sulfur recovery technical requirement.
The regeneration techniques of the methanol solution of hydrogen sulfide and carbon dioxide is absorbed in low-temperature rectisol process for purifying, this sulfur-bearing methanol solution is desorbed by impurity such as the hydrogen sulfide, carbon dioxide and other the micro-organic sulfurs that it are dissolved in absorption process after the regeneration measure of the technology of the present invention, makes solvent be regenerated and recycle.The sulfide component desorbed can according to downstream sulfur recovery technology requirement, hydrogen sulfide sour gas is obtained by a kind of method for concentration controlling concentration of component, adapt to the different operating modes of unstripped gas sulfur content fluctuation, the hydrogen sulfide acid tail gas concentration that low-temperature rectisol obtains is controlled flexibly, this sour gas meets the technic index requirement of sulfur recovery unit, so that better realize sulfur recovery process finally obtain sulphur or sulfuric acid by-products, the carbon dioxide component of separating sucking-off in regenerative process then meets environmental protection index and requires discharge or provide to make other purposes.
Method of the present invention comprises the steps:
(1) pressure flash distillation in
From the sulfur-bearing methyl alcohol rich solution having dissolved sulfide and carbon dioxide of low-temperature rectisol gas purification absorptive unit, first enter middle pressure flash column from middle part and carry out vacuum flashing, object is through the fuel gas CH that flash distillation will be dissolved in solution
4, CO, H
2reclaimed etc. desorbing.Flashing pressure general control in 0.5-1.8MPa (Pa represents absolute pressure) scope, part H in the process
2s, CO
2also be flashed out, in order to improve CH
4, CO, H
2the concentration of these combustible gas components, is conducive to recycling, will enters middle pressure flash column to CO on a small quantity without sulphur methyl alcohol semi lean solution from top
2, H
2s carries out washing absorption, therefrom press flash column top out containing CH
4, CO, H
2flashed vapour can be used as fuel gas carrying device or returns unstripped gas system and is recovered utilization, and the methanol solution after flash distillation is therefrom pressed extraction bottom flash column to enter reabsorber and processed further;
(2) air lift and absorbing again
The object of this step makes carbon dioxide component desorb from solution by decompression, air lift measure, and sulfide wherein is then absorbed by solution secondary washing and makes it still dissolve in the solution thus reach the effect of sulfide enrichment.
Entering in the middle part of reabsorber from the methanol solution bottom middle pressure flash column, in this section by being decompressed to 0.12 to 0.2MPa further, discharging CO
2, H
2the gases such as S; Reabsorber top is again absorber portion, and object is absorbed the methyl alcohol semi lean solution secondary washing sprayed of the sulfide in flashed vapour, and methyl alcohol semi lean solution enters from reabsorber top in order to absorb the H risen stripping gas in the middle part of reabsorber
2s, object is absorbed the methyl alcohol semi lean solution secondary washing sprayed of the sulfide in flashed vapour in the process, makes CO
2component major part is flashed solution sucking-off, and H
2s component is by absorbing and being concentrated in methanol solution; Reabsorber bottom is stripping section, passes into low-pressure nitrogen air lift from reabsorber bottom, makes the CO dissolved in methanol solution
2desorb is more complete, makes H
2s is further concentrated, and the low-pressure nitrogen pressure that air lift adopts is generally 0.3-0.6MPa, simultaneously from flash evaporation groove top containing H
2s rich gas returns to reabsorber bottom, to reach H
2s further enrichment in the solution;
Most of CO is desorbed in sulfur-bearing methyl alcohol rich solution
2discharge from reabsorber top, discharge or send outside and be made for other purposes, containing sulfide and fraction CO after discharge gas/heat-lightening vapor heat exchanger and the heat exchange to normal temperature of heat-lightening steam
2sulfur-bearing methyl alcohol rich solution discharge by bottom reabsorber, enter the process of subsequent thermal flash steps;
(3) flash evaporation
This step is passed through flash distillation again after the heating of sulfur-bearing methyl alcohol rich solution, and flashed vapour returns reabsorber and forms circulation, regulates sulfur-bearing rich solution medium sulphide content concentration, meet the requirement of subsequent technique to sour gas concentration to control final acid tail gas medium sulphide content concentration with this.
From reabsorber sulfur-bearing methyl alcohol rich solution through flash evaporation feed pump be transported in lean/rich heat exchange of methanol device with from hot recycling tower the heat exchange of hot poor methanol liquid and be heated to 70-85 DEG C, then be sent to flash evaporation groove and carry out vacuum flashing, the control range of flashing pressure at 0.2-2.0MPa, by these means by the CO in sulfur-bearing methyl alcohol rich solution
2and H
2s flashes off again, obtains containing CO
2with the heat-lightening steam of sulfide, this heat-lightening steam from flash tank top flow out through the heat exchange of flash evaporation condenser to normal temperature, then this flashed vapour again through discharge gas/heat-lightening vapor heat exchanger heat exchange, by the heat exchange of discharge gas to normal temperature to reclaim its cold, flashed vapour is then turned back to reabsorber bottom after heat exchange, by the circulation of this step, sulfide is concentrated in the solution further, the flow of circulation flashed vapour controls by regulating flashing pressure, improve flashing pressure, the circulating flow rate then returned reduces, to reduce sulfide concentrating degree; Reduce flashing pressure, then the circulating flow rate returned increases, and to strengthen sulfide concentrating degree, flash evaporation trench bottom sulfur-bearing methanol solution out enters heat step process again;
(4) hot recycling
The sulfur-bearing methanol solution come from flash evaporation trench bottom enters in the middle part of hot recycling tower, makes the sulfide that dissolves in solution and remaining CO under the stripping effect of methanol steam
2under the stripping effect of methanol steam, all solutions sucks out, this stripping gas acid cut is discharged from hot recycling top of tower, hot recycling institute calorific requirement is provided by low-pressure steam indirect by reboiler, hot recycling tower operating pressure scope 0.2-0.5MPa, hot recycling tower tower reactor operating temperature is 85-110 DEG C.The poor methanol liquid of discharging from hot recycling tower bottom obtains holomorphosis, through lean pump conveying and the absorptive unit being sent to low temperature washing device for methanol after lower the temperature with cold sulfur-bearing methyl alcohol rich solution heat exchange in lean/rich heat exchange of methanol device recycle, the sour gas fraction leaving hot recycling top of tower enters sulfide cut and cools and reflow treatment;
(5) cooling of sulfide cut and backflow
The sour gas fraction leaving hot recycling top of tower is recycled cooling water heat exchange to 35-45 DEG C through hot recycling condenser, enter reflux splitter afterwards, from reflux splitter top, gaseous phase materials is out divided into two strands, one is connected to and returns in the flash evaporation gas pipeline of reabsorber, play the effect that strengthening sulphide cycle is concentrated, this measure is also one of means of adjustment of acidity tail gas medium sulphide content concentration, returns internal circulating load and adjusts with the requirement of final sour gas concentration index in 0-80% scope; Remainder then enters tail gas heat exchanger and hydrogen sulfide tail gas deep freezer by further condensation and cooling, temperature is reduced to-25 to-40 DEG C, by the methyl alcohol carried secretly in sour gas fraction from hydrogen sulfide tail gas deep freezer condensation separation out, condensate liquid is collected in reflux splitter, bottom reflux splitter out methanol solution reflux pump pressurization after be back to hot recycling top of tower;
Be the heat exchange tail gas heat exchanger of sulfide acid tail gas from hydrogen sulfide tail gas deep freezer on-condensible gas out and reclaim cold, battery limit (BL) is sent as the acid gas of sulfur recovery unit after temperature is raised to normal temperature, the concentration of its medium sulphide content by meet after controlling measurement recited above the requirement of supporting sulfur recovery unit technological operation index, its concentration range is at 20-50% (v).
The present invention compared with prior art tool has the following advantages:
1 the present invention adopts the multiple combination measures such as flash distillation, air lift, double absorption, hot recycling, circulation, simple to operate, is convenient to control.
2 are adapted to different material sulfur content and have in the low-temp methanol washing process process of fluctuation change operating mode the requirement of sulfide concentration technology.
3 are adapted to the different requirements of different sulfur recovery technology to low-temperature rectisol acid tail gas medium sulphide content concentration index.
4 process optimizations, energy-saving and cost-reducing, be conducive to meeting environmental protection requirement.
Accompanying drawing explanation
Fig. 1 is flow chart of the present invention.
As shown in the figure, flash column is pressed in 1-; 2-reabsorber; 3-flash evaporation feed pump; 4-discharges gas/heat-lightening vapor heat exchanger; The lean/rich heat exchange of methanol device of 5-; 6-flash evaporation condenser; 7-lean pump; 8-flash evaporation groove; 9-hot recycling tower; 10-hot recycling condenser; 11-reboiler; 12-reflux pump; 13-reflux splitter; 14-tail gas heat exchanger; 15-hydrogen sulfide tail gas deep freezer.
Detailed description of the invention
Embodiment 1
In the present embodiment 1, from the sulfur-bearing rich solution 84m of low-temperature rectisol absorptive unit
3/ h, temperature :-23 DEG C, pressure: 3.52MPa, specifically consists of:
| Composition | H 2 | CO | CO 2 | CH 4 | N 2 | H 2S | COS | CH 3OH | ∑ |
| wt％ | 0.01 | 0.20 | 24.46 | 19ppm | 0.01 | 0.37 | 0.03 | 74.92 | 100.0 |
(1) pressure flash distillation in
From the sulfur-bearing methyl alcohol rich solution having dissolved sulfide and carbon dioxide of low-temperature rectisol gas purification absorptive unit, first enter middle pressure flash column 1 from middle part and carry out vacuum flashing, object is through the fuel gas CH that flash distillation will be dissolved in solution
4, CO, H
2reclaimed etc. desorbing.Flashing pressure controls in 1.2MPa (Pa represents absolute pressure) scope, part H in the process
2s, CO
2also be flashed out, in order to improve CH
4, CO, H
2the concentration of these combustible gas components, is conducive to recycling, will enters middle pressure flash column 1 couple of CO on a small quantity without sulphur methyl alcohol semi lean solution from top
2, H
2s carries out washing absorption, therefrom press flash column 1 top out containing CH
4, CO, H
2flashed vapour can be used as fuel gas carrying device or returns unstripped gas system and is recovered utilization, and the methanol solution after flash distillation is therefrom pressed extraction bottom flash column 1 to enter reabsorber 2 and processed further;
(2) air lift and absorbing again
Entering in the middle part of reabsorber 2 from the methanol solution bottom middle pressure flash column 1, in this section by being decompressed to 0.13 further, discharging CO
2, H
2the gases such as S; Reabsorber 2 top is again absorber portion, and object is absorbed the methyl alcohol semi lean solution secondary washing sprayed of the sulfide in flashed vapour, and methyl alcohol semi lean solution enters from reabsorber 2 top in order to absorb the H risen stripping gas in the middle part of reabsorber 2
2s, object is absorbed the methyl alcohol semi lean solution secondary washing sprayed of the sulfide in flashed vapour in the process, makes CO
2component major part is flashed solution sucking-off, and H
2s component is by absorbing and being concentrated in methanol solution; Reabsorber 2 bottom is stripping section, passes into low-pressure nitrogen air lift, make the CO dissolved in methanol solution from reabsorber 2 bottom
2desorb is more complete, makes H
2s is further concentrated, and the low-pressure nitrogen pressure that air lift adopts is 0.5MPa, simultaneously from flash evaporation groove 8 top containing H
2s rich gas returns to reabsorber 2 bottom, to reach H
2s further enrichment in the solution, to make bottom reabsorber 2 total sulfur (H in methyl alcohol rich solution
2s+COS) concentration accounting for total solution gas is 9.8% (v).
Most of CO is desorbed in sulfur-bearing methyl alcohol rich solution
2discharge from reabsorber 2 top, discharge or send outside after discharge gas/heat-lightening vapor heat exchanger 4 with the heat exchange to normal temperature of heat-lightening steam and be made for other purposes, containing sulfide and fraction CO
2sulfur-bearing methyl alcohol rich solution by bottom reabsorber 2 discharge, enter the process of subsequent thermal flash steps;
(3) flash evaporation
From reabsorber 2 sulfur-bearing methyl alcohol rich solution through flash evaporation feed pump 3 be transported in lean/rich heat exchange of methanol device 5 with from hot recycling tower 9 the heat exchange of hot poor methanol liquid and be heated to 72 DEG C, then be sent to flash evaporation groove 8 and carry out vacuum flashing, flashing pressure controls at 0.21MPa, by these means by the CO in sulfur-bearing methyl alcohol rich solution
2and H
2s flashes off again, obtains containing CO
2with the heat-lightening steam of sulfide, this heat-lightening steam from flash tank 8 top flow out through flash evaporation condenser 6 heat exchange to normal temperature, then this flashed vapour again through discharge gas/heat-lightening vapor heat exchanger 4 heat exchange, by the heat exchange of discharge gas to normal temperature to reclaim its cold, flashed vapour is then turned back to reabsorber 2 bottom after heat exchange, by the circulation of this step, sulfide is concentrated in the solution further, the flow of circulation flashed vapour controls by regulating flashing pressure, improve flashing pressure, the circulating flow rate then returned reduces, to reduce sulfide concentrating degree; Reduce flashing pressure, then the circulating flow rate returned increases, and to strengthen sulfide concentrating degree, bottom flash evaporation groove 8, sulfur-bearing methanol solution out enters heat step process again;
(4) hot recycling
The sulfur-bearing methanol solution come bottom flash evaporation groove 8 enters in the middle part of hot recycling tower 9, makes the sulfide that dissolves in solution and remaining CO under the stripping effect of methanol steam
2under the stripping effect of methanol steam, all solutions sucks out, this stripping gas acid cut is discharged from hot recycling tower 9 top, hot recycling institute calorific requirement is provided by low-pressure steam indirect by reboiler 11, hot recycling tower 9 operating pressure 0.25MPa, and hot recycling tower 9 tower reactor operating temperature is 92 DEG C.The poor methanol liquid of discharging bottom hot recycling tower 9 obtains holomorphosis, to carry and the absorptive unit being sent to low temperature washing device for methanol after lowering the temperature with cold sulfur-bearing methyl alcohol rich solution heat exchange in lean/rich heat exchange of methanol device 5 recycles through lean pump 7, the sour gas fraction leaving hot recycling tower 9 top enters the cooling of sulfide cut and reflow treatment;
(5) cooling of sulfide cut and backflow
The sour gas fraction leaving hot recycling tower 9 top is recycled cooling water heat exchange to 40 DEG C through hot recycling condenser 10, enter reflux splitter 13 afterwards, two strands are divided into from reflux splitter 13 top gaseous phase materials out, one is connected to and returns in the flash evaporation gas pipeline of reabsorber 2, play the effect that strengthening sulphide cycle is concentrated, this measure is also one of means of adjustment of acidity tail gas medium sulphide content concentration, return that internal circulating load accounts for total amount 63.5%, remainder then enters tail gas heat exchanger 14, hydrogen sulfide tail gas deep freezer 15 is by further condensation and cooling, temperature is reduced to-35 DEG C, by the methyl alcohol carried secretly in sour gas fraction from hydrogen sulfide tail gas deep freezer 15 condensation separation out, condensate liquid is collected in reflux splitter 13, bottom reflux splitter 13, methanol solution reflux pump 12 is out back to hot recycling tower 9 top after pressurizeing,
Be the heat exchange tail gas heat exchanger 14 of sulfide acid tail gas from hydrogen sulfide tail gas deep freezer 15 on-condensible gas out and reclaim cold, battery limit (BL) is sent as the acid gas of sulfur recovery unit after temperature is raised to normal temperature, the concentration of its medium sulphide content by meet after controlling measurement recited above the requirement of supporting sulfur recovery unit technological operation index, total sulfur (H in acid tail gas
2s+COS) content's index is 31.2% (v).
Embodiment 2
In the present embodiment 2, from the sulfur-bearing rich solution 182m of low-temperature rectisol absorptive unit
3/ h, temperature :-20 DEG C, pressure: 3.28MPa, specifically consists of:
| Composition | H 2 | CO | CO 2 | CH 4 | N 2 | H 2S | COS | CH 3OH | ∑ |
| wt％ | 98ppm | 0.20 | 20.9 | 155ppm | 109ppm | 0.70 | 0.12 | 78.08 | 100.0 |
In the present embodiment, process step is identical with embodiment 1.According to the change of starting materials contain sulfur rich solution condition, for reaching sulfur recovery unit technological requirement, part operation parameter respective change is as follows:
Middle pressure flash column 1 flashing pressure is 0.75MPa;
In reabsorber 2, pressure is 0.19MPa;
Air lift low-pressure nitrogen pressure is 0.4MPa;
Total sulfur (H in methyl alcohol rich solution solution gas bottom reabsorber 2 after concentrated
2s+COS) content is 15.9% (v);
The temperature that methyl alcohol rich solution enters flash evaporation groove 8 is 85 DEG C;
Flash evaporation groove 8 flashing pressure is 1.6MPa;
In hot recycling tower 9 tower, operating pressure is 0.4MPa, and tower reactor operating temperature is 104 DEG C;
Leave in the gaseous phase materials of reflux splitter 13, one returning reabsorber 2 accounts for 28.0% of total amount;
The temperature of acid tail gas after tail gas heat exchanger 14, hydrogen sulfide tail gas deep freezer 15 heat exchange is-38 DEG C;
Go out total sulfur (H in device acid tail gas
2s+COS) content is 45.3% (v).
Embodiment 3
In the present embodiment 3, from the sulfur-bearing rich solution 120m of low-temperature rectisol absorptive unit
3/ h, temperature :-27 DEG C, pressure: 2.54MPa, specifically consists of:
| Composition | H 2 | CO | CO 2 | CH 4 | N 2 | H 2S | COS | CH 3OH | C 2H 6 | C 3H 8 | ∑ |
| wt％ | 91ppm | 0.1 | 20.5 | 0.1 | 72ppm | 0.8 | 280ppm | 78.0 | 557ppm | 0.4 | 100.0 |
In an embodiment, process step is identical with embodiment 1.According to the change of starting materials contain sulfur rich solution condition, for reaching sulfur recovery unit technological requirement, part operation parameter respective change is as follows:
Middle pressure flash column 1 flashing pressure is 0.6MPa;
In reabsorber 2, pressure is 0.15MPa;
Total sulfur (H in methyl alcohol rich solution solution gas bottom reabsorber 2 after concentrated
2s+COS) content is 10.2% (v);
The temperature that methyl alcohol rich solution enters flash evaporation groove 8 is 77.5 DEG C;
Flash evaporation groove 8 flashing pressure is 0.9MPa;
In hot recycling tower 9 tower, operating pressure is 0.31MPa, and tower reactor operating temperature is 95 DEG C;
Leave the gaseous phase materials of reflux splitter 13, the amount returning reabsorber 2 is 0, does not namely return.
The temperature of acid tail gas after tail gas heat exchanger 14, hydrogen sulfide tail gas deep freezer 15 heat exchange is-30 DEG C;
Go out total sulfur (H in device acid tail gas
2s+COS) content is 33.0% (v).
Claims (1)
1. control a method for hydrogen sulfide tail gas concentration in applicable low-temperature rectisol process, it is characterized in that comprising the steps:
(1) pressure flash distillation in
From the sulfur-bearing methyl alcohol rich solution having dissolved sulfide and carbon dioxide of low-temperature rectisol gas purification absorptive unit, first enter middle pressure flash column from middle part and carry out vacuum flashing, flashing pressure controls in 0.5-1.8MPa scope, will enter middle pressure flash column to CO on a small quantity without sulphur methyl alcohol semi lean solution from top
2, H
2s carries out washing absorption, therefrom press flash column top out containing CH
4, CO, H
2flashed vapour is as fuel gas carrying device or return unstripped gas system and be recovered utilization, and the methanol solution after flash distillation is therefrom pressed to draw bottom flash column and entered reabsorber and process further;
(2) air lift and absorbing again
Entering in the middle part of reabsorber from the methanol solution bottom middle pressure flash column, in this section by being decompressed to 0.12 to 0.2MPa further, discharging CO
2, H
2the gases such as S; Reabsorber top is again absorber portion, and methyl alcohol semi lean solution enters from reabsorber top in order to absorb the H risen stripping gas in the middle part of reabsorber
2s; Reabsorber bottom is stripping section, passes into low-pressure nitrogen air lift from reabsorber bottom, and the low-pressure nitrogen pressure that air lift adopts is 0.3-0.6MPa, simultaneously from flash evaporation groove top containing H
2s rich gas returns to reabsorber bottom, to reach H
2s further enrichment in the solution;
Most of CO is desorbed in sulfur-bearing methyl alcohol rich solution
2discharge from reabsorber top, discharge or send outside and be made for other purposes after discharge gas/heat-lightening vapor heat exchanger and the heat exchange to normal temperature of heat-lightening steam, the CO containing sulfide and fraction
2sulfur-bearing methyl alcohol rich solution discharge by bottom reabsorber, enter the process of subsequent thermal flash steps;
(3) flash evaporation
From reabsorber sulfur-bearing methyl alcohol rich solution through flash evaporation feed pump be transported in lean/rich heat exchange of methanol device with from hot recycling tower the heat exchange of hot poor methanol liquid and be heated to 70-85 DEG C, then be sent to flash evaporation groove and carry out vacuum flashing, the control range of flashing pressure, at 0.2-2.0MPa, obtains containing CO
2with the heat-lightening steam of sulfide, this heat-lightening steam flows out from flash tank top and after discharge gas/heat-lightening vapor heat exchanger heat exchange, turns back to reabsorber bottom through the heat exchange of flash evaporation condenser again to normal temperature, then this flashed vapour, and flash evaporation trench bottom sulfur-bearing methanol solution out enters heat step process again;
(4) hot recycling
The sulfur-bearing methanol solution come from flash evaporation trench bottom enters in the middle part of hot recycling tower, makes the sulfide that dissolves in solution and remaining CO under the stripping effect of methanol steam
2under the stripping effect of methanol steam, all solutions sucks out, this stripping gas acid cut is discharged from hot recycling top of tower, hot recycling institute calorific requirement is provided by low-pressure steam indirect by reboiler, hot recycling tower operating pressure scope 0.2-0.5MPa, hot recycling tower tower reactor operating temperature is 85-110 DEG C, the poor methanol liquid of discharging from hot recycling tower bottom obtains holomorphosis, through lean pump conveying and the absorptive unit being sent to low temperature washing device for methanol after lowering the temperature with cold sulfur-bearing methyl alcohol rich solution heat exchange in lean/rich heat exchange of methanol device recycle, the sour gas fraction leaving hot recycling top of tower enters the cooling of sulfide cut and reflow treatment,
(5) cooling of sulfide cut and backflow
The sour gas fraction leaving hot recycling top of tower is recycled cooling water heat exchange to 35-45 DEG C through hot recycling condenser, enter reflux splitter afterwards, from reflux splitter top, gaseous phase materials is out divided into two strands, one is connected to and returns in the flash evaporation gas pipeline of reabsorber, return internal circulating load in 0-80% scope, another stock then enters tail gas heat exchanger and hydrogen sulfide tail gas deep freezer by further condensation and cooling, temperature is reduced to-25 DEG C to-40 DEG C, by the methyl alcohol carried secretly in sour gas fraction from hydrogen sulfide tail gas deep freezer condensation separation out, condensate liquid is collected in reflux splitter, bottom reflux splitter out methanol solution reflux pump pressurization after be back to hot recycling top of tower,
Cold is reclaimed from the heat exchange tail gas heat exchanger of the acid on-condensible gas tail gas of hydrogen sulfide tail gas deep freezer sulfide out, send battery limit (BL) as the acid gas of sulfur recovery unit after temperature is raised to normal temperature, the volume concentration range of its medium sulphide content is at 20-50%.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201410687078.5A CN104437004B (en) | 2014-11-25 | 2014-11-25 | The method of hydrogen sulfide tail gas concentration is controlled in a kind of applicable low-temperature rectisol process |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201410687078.5A CN104437004B (en) | 2014-11-25 | 2014-11-25 | The method of hydrogen sulfide tail gas concentration is controlled in a kind of applicable low-temperature rectisol process |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN104437004A true CN104437004A (en) | 2015-03-25 |
| CN104437004B CN104437004B (en) | 2016-04-06 |
Family
ID=52884219
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201410687078.5A Active CN104437004B (en) | 2014-11-25 | 2014-11-25 | The method of hydrogen sulfide tail gas concentration is controlled in a kind of applicable low-temperature rectisol process |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN104437004B (en) |
Cited By (17)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104984634A (en) * | 2015-07-15 | 2015-10-21 | 天津大学 | Treating device for waste gas containing volatile organic matters |
| CN105523524A (en) * | 2015-12-29 | 2016-04-27 | 大连百傲化学股份有限公司 | Apparatus and method for producing highly pure hydrogen sulfide |
| CN106281476A (en) * | 2016-08-31 | 2017-01-04 | 上海倍能化工技术有限公司 | A kind of low temperature washing device for methanol and a kind of remove the method for sour gas in synthesis gas |
| CN106318475A (en) * | 2015-06-15 | 2017-01-11 | 上海东化环境工程有限公司 | Improvement technology of low temperature methanol washing |
| CN107754558A (en) * | 2016-08-19 | 2018-03-06 | 中国石油化工股份有限公司 | A kind of NHD desulfurization concentrating method |
| CN107890748A (en) * | 2017-10-27 | 2018-04-10 | 中石化宁波工程有限公司 | A kind of pre- extracting and concentrating technology of medium temperature sour gas |
| CN108057319A (en) * | 2018-01-10 | 2018-05-22 | 上海朴力节能环保科技有限公司 | Unstripped gas recovery method and device |
| CN109078349A (en) * | 2018-08-14 | 2018-12-25 | 中国石油化工股份有限公司 | A kind of low-temp methanol washes energy saver and technique |
| CN110448995A (en) * | 2019-08-19 | 2019-11-15 | 福建中融科技有限公司 | Liquefied air purification methanol deodorant and its preparation and application |
| CN110548370A (en) * | 2019-09-04 | 2019-12-10 | 大连理工大学 | Acid gas purification process and device for producing hydrogen sulfide with various purities |
| CN110548369A (en) * | 2019-08-01 | 2019-12-10 | 中石化宁波工程有限公司 | Control method for CO content in tail gas generated by removing acid gas |
| CN111659147A (en) * | 2019-03-08 | 2020-09-15 | 大连佳纯气体净化技术开发有限公司 | Recovery of CO from low-temperature methanol washing process2And a recycling system |
| CN112090221A (en) * | 2020-08-13 | 2020-12-18 | 河北正元氢能科技有限公司 | Method for purifying raw gas for ammonia synthesis and ammonia synthesis process based on method |
| CN112107875A (en) * | 2020-10-29 | 2020-12-22 | 上海华谊工程有限公司 | Flash evaporation stripping cooling system and treatment process for black water by using same |
| CN112892146A (en) * | 2021-01-26 | 2021-06-04 | 凯盛光伏材料有限公司 | Method and system for separating hydrogen sulfide from industrial tail gas |
| CN113654034A (en) * | 2021-07-20 | 2021-11-16 | 山东联盟化工股份有限公司 | Comprehensive recycling technology for low-grade steam containing acidic non-condensable gas |
| CN115364808A (en) * | 2022-07-26 | 2022-11-22 | 哈尔滨工业大学（深圳） | Continuous urea synthesis system |
Citations (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20090101007A1 (en) * | 2004-10-08 | 2009-04-23 | Rasmus Find | Method for recovery of carbon dioxide from a gas |
| CN101417183A (en) * | 2008-11-14 | 2009-04-29 | 上海惠生化工工程有限公司 | A kind of technology that reclaims methyl alcohol in the low-temperature methanol washing tail-gas |
| US20090270651A1 (en) * | 2008-04-29 | 2009-10-29 | Zinobile Raymond J | Methanol carbonylation system having absorber with multiple solvent options |
| GB2464368B (en) * | 2008-10-14 | 2011-02-09 | Cyril Timmins | High pressure physical absorption regeneration process |
| CN103320176A (en) * | 2013-06-20 | 2013-09-25 | 华南理工大学 | Low temperature methanol washing method and device with high CO2 yield |
| CN203429144U (en) * | 2013-06-20 | 2014-02-12 | 华南理工大学 | Low-temperature methanol washing device with high CO2 yield |
| CN203923123U (en) * | 2014-06-11 | 2014-11-05 | 上海国际化建工程咨询公司 | A kind of device that reduces low-temperature rectisol methane rate of loss |
-
2014
- 2014-11-25 CN CN201410687078.5A patent/CN104437004B/en active Active
Patent Citations (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20090101007A1 (en) * | 2004-10-08 | 2009-04-23 | Rasmus Find | Method for recovery of carbon dioxide from a gas |
| US20090270651A1 (en) * | 2008-04-29 | 2009-10-29 | Zinobile Raymond J | Methanol carbonylation system having absorber with multiple solvent options |
| GB2464368B (en) * | 2008-10-14 | 2011-02-09 | Cyril Timmins | High pressure physical absorption regeneration process |
| CN101417183A (en) * | 2008-11-14 | 2009-04-29 | 上海惠生化工工程有限公司 | A kind of technology that reclaims methyl alcohol in the low-temperature methanol washing tail-gas |
| CN103320176A (en) * | 2013-06-20 | 2013-09-25 | 华南理工大学 | Low temperature methanol washing method and device with high CO2 yield |
| CN203429144U (en) * | 2013-06-20 | 2014-02-12 | 华南理工大学 | Low-temperature methanol washing device with high CO2 yield |
| CN203923123U (en) * | 2014-06-11 | 2014-11-05 | 上海国际化建工程咨询公司 | A kind of device that reduces low-temperature rectisol methane rate of loss |
Cited By (25)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106318475A (en) * | 2015-06-15 | 2017-01-11 | 上海东化环境工程有限公司 | Improvement technology of low temperature methanol washing |
| CN104984634A (en) * | 2015-07-15 | 2015-10-21 | 天津大学 | Treating device for waste gas containing volatile organic matters |
| CN105523524A (en) * | 2015-12-29 | 2016-04-27 | 大连百傲化学股份有限公司 | Apparatus and method for producing highly pure hydrogen sulfide |
| CN107754558A (en) * | 2016-08-19 | 2018-03-06 | 中国石油化工股份有限公司 | A kind of NHD desulfurization concentrating method |
| CN107754558B (en) * | 2016-08-19 | 2020-10-20 | 中国石油化工股份有限公司 | Desulfurization and concentration method of polyethylene glycol dimethyl ether |
| CN106281476A (en) * | 2016-08-31 | 2017-01-04 | 上海倍能化工技术有限公司 | A kind of low temperature washing device for methanol and a kind of remove the method for sour gas in synthesis gas |
| CN106281476B (en) * | 2016-08-31 | 2019-05-24 | 上海倍能化工技术有限公司 | A kind of method of sour gas in low temperature washing device for methanol and a kind of removing synthesis gas |
| CN107890748A (en) * | 2017-10-27 | 2018-04-10 | 中石化宁波工程有限公司 | A kind of pre- extracting and concentrating technology of medium temperature sour gas |
| CN108057319A (en) * | 2018-01-10 | 2018-05-22 | 上海朴力节能环保科技有限公司 | Unstripped gas recovery method and device |
| CN108057319B (en) * | 2018-01-10 | 2023-08-04 | 上海朴力节能环保科技有限公司 | Raw material gas recovery method and device |
| CN109078349A (en) * | 2018-08-14 | 2018-12-25 | 中国石油化工股份有限公司 | A kind of low-temp methanol washes energy saver and technique |
| CN109078349B (en) * | 2018-08-14 | 2021-06-01 | 中国石油化工股份有限公司 | Low-temperature methanol washing energy-saving device and process |
| CN111659147A (en) * | 2019-03-08 | 2020-09-15 | 大连佳纯气体净化技术开发有限公司 | Recovery of CO from low-temperature methanol washing process2And a recycling system |
| CN110548369A (en) * | 2019-08-01 | 2019-12-10 | 中石化宁波工程有限公司 | Control method for CO content in tail gas generated by removing acid gas |
| CN110548369B (en) * | 2019-08-01 | 2022-02-15 | 中石化宁波工程有限公司 | Control method for CO content in tail gas generated by removing acid gas |
| CN110448995A (en) * | 2019-08-19 | 2019-11-15 | 福建中融科技有限公司 | Liquefied air purification methanol deodorant and its preparation and application |
| CN110548370A (en) * | 2019-09-04 | 2019-12-10 | 大连理工大学 | Acid gas purification process and device for producing hydrogen sulfide with various purities |
| CN112090221A (en) * | 2020-08-13 | 2020-12-18 | 河北正元氢能科技有限公司 | Method for purifying raw gas for ammonia synthesis and ammonia synthesis process based on method |
| CN112090221B (en) * | 2020-08-13 | 2022-03-22 | 河北正元氢能科技有限公司 | Method for purifying raw gas for ammonia synthesis and ammonia synthesis process based on method |
| CN112107875A (en) * | 2020-10-29 | 2020-12-22 | 上海华谊工程有限公司 | Flash evaporation stripping cooling system and treatment process for black water by using same |
| CN112107875B (en) * | 2020-10-29 | 2023-08-15 | 上海华谊工程有限公司 | Flash evaporation steam stripping cooling system and black water treatment process using same |
| CN112892146A (en) * | 2021-01-26 | 2021-06-04 | 凯盛光伏材料有限公司 | Method and system for separating hydrogen sulfide from industrial tail gas |
| CN113654034A (en) * | 2021-07-20 | 2021-11-16 | 山东联盟化工股份有限公司 | Comprehensive recycling technology for low-grade steam containing acidic non-condensable gas |
| CN113654034B (en) * | 2021-07-20 | 2023-08-29 | 山东联盟化工股份有限公司 | Comprehensive recycling method for low-grade steam containing acidic noncondensable gas |
| CN115364808A (en) * | 2022-07-26 | 2022-11-22 | 哈尔滨工业大学（深圳） | Continuous urea synthesis system |
Also Published As
| Publication number | Publication date |
|---|---|
| CN104437004B (en) | 2016-04-06 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN104437004B (en) | The method of hydrogen sulfide tail gas concentration is controlled in a kind of applicable low-temperature rectisol process | |
| CN101874967B (en) | Process for removing acid gas with low-temperature methanol solution | |
| CN101418246B (en) | Low temperature methanol washing integrated Claus sulfur recovery system and process | |
| CN100406106C (en) | Method for the selective removal of hydrogen sulphide and co2 from crude gas | |
| CN203139876U (en) | Low-temperature methanol washing process device | |
| CN101885993B (en) | Purification process for removing sulphur and carbon dioxide in gas by using two-step method | |
| CN101492616B (en) | Desulfurization and decarburization integrated absorption process for polyglycol dimethyl ether | |
| CN102433169B (en) | Low temperature methanol washing technology | |
| CN109999618B (en) | System and method for separating carbon dioxide from medium-high pressure gas source | |
| CN103657381A (en) | Flue gas pretreatment and carbon dioxide collecting, purifying and recycling device | |
| CN104293398A (en) | Energy-saving and production-increasing method and device adopting low temperature methanol cleaning technology | |
| CN112625761B (en) | Process for removing low-partial pressure acid gas in low-pressure feed gas by using low-temperature methanol | |
| CN107073388B (en) | Regeneration method of energy-saving solvent for carbon dioxide capture | |
| CN106281476A (en) | A kind of low temperature washing device for methanol and a kind of remove the method for sour gas in synthesis gas | |
| CN203781843U (en) | System for treating Claus sulfur recovery tail gas by low-temperature methanol washing hydrogen sulfide concentrating tower | |
| US11596897B2 (en) | Method for recovering CO2 in the Rectisol process and recovery system | |
| CN106311149A (en) | Absorbent used for natural gas decarburization | |
| CN107754568B (en) | Low-energy-consumption device for capturing and recovering carbon dioxide by flue gas and gas recovery process | |
| CN102489120B (en) | Low temperature methanol wash method and equipment | |
| CN102085445B (en) | Modification solution for removing acid gas of low-temperature methanol cleaning process | |
| CN101434872B (en) | Method for adding distilled ammonia vapor into desulfurized solution in ammonia desulphurization process and special equipment thereof | |
| CN105542876A (en) | Method for using low temperature methanol washing apparatus for removal of impurities in shift gas | |
| CN110639335A (en) | Energy-saving method and system for regeneration tower in deep decarburization of natural gas | |
| CN202355997U (en) | CO2 absorption tower and low-temperature methanol washing equipment comprising same | |
| CN104998517A (en) | Method for increasing concentrations of acid gas hydrogen sulfide and carbonyl sulfide in low-temperature methanol washing process |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| C14 | Grant of patent or utility model | ||
| GR01 | Patent grant |