CN109569193A - It is a kind of to absorb the sulfur method synchronous with regeneration - Google Patents
It is a kind of to absorb the sulfur method synchronous with regeneration Download PDFInfo
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- CN109569193A CN109569193A CN201710895112.1A CN201710895112A CN109569193A CN 109569193 A CN109569193 A CN 109569193A CN 201710895112 A CN201710895112 A CN 201710895112A CN 109569193 A CN109569193 A CN 109569193A
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- gas
- regeneration
- sulfur
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- desulfurization
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D53/00—Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols
- B01D53/14—Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols by absorption
- B01D53/1456—Removing acid components
- B01D53/1468—Removing hydrogen sulfide
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D53/00—Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols
- B01D53/14—Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols by absorption
- B01D53/1425—Regeneration of liquid absorbents
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B17/00—Sulfur; Compounds thereof
- C01B17/02—Preparation of sulfur; Purification
- C01B17/04—Preparation of sulfur; Purification from gaseous sulfur compounds including gaseous sulfides
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D2252/00—Absorbents, i.e. solvents and liquid materials for gas absorption
- B01D2252/20—Organic absorbents
- B01D2252/202—Alcohols or their derivatives
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D2252/00—Absorbents, i.e. solvents and liquid materials for gas absorption
- B01D2252/20—Organic absorbents
- B01D2252/204—Amines
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D2252/00—Absorbents, i.e. solvents and liquid materials for gas absorption
- B01D2252/20—Organic absorbents
- B01D2252/204—Amines
- B01D2252/20478—Alkanolamines
- B01D2252/20489—Alkanolamines with two or more hydroxyl groups
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D2252/00—Absorbents, i.e. solvents and liquid materials for gas absorption
- B01D2252/20—Organic absorbents
- B01D2252/205—Other organic compounds not covered by B01D2252/00 - B01D2252/20494
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D2252/00—Absorbents, i.e. solvents and liquid materials for gas absorption
- B01D2252/20—Organic absorbents
- B01D2252/205—Other organic compounds not covered by B01D2252/00 - B01D2252/20494
- B01D2252/2053—Other nitrogen compounds
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D2257/00—Components to be removed
- B01D2257/30—Sulfur compounds
- B01D2257/304—Hydrogen sulfide
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Engineering & Computer Science (AREA)
- Analytical Chemistry (AREA)
- General Chemical & Material Sciences (AREA)
- Oil, Petroleum & Natural Gas (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Inorganic Chemistry (AREA)
- Gas Separation By Absorption (AREA)
- Treating Waste Gases (AREA)
- Industrial Gases (AREA)
Abstract
It is a kind of to absorb the sulfur method synchronous with regeneration, belong to gas purification technique field.Present invention process process is simple, and a step can be by H2S is converted to elementary sulfur, and elementary sulfur monomer exists in the form of the liquid sulfur being dissolved in desulfurization solvent, rather than solid sulfur granules, so the blistering in technique, blocking and other operational issues can be avoided effectively.The present invention can directly handle all kinds of high-low pressure sulfurous gas, process is simple, desulfuration efficiency is high, solution internal circulating load is low, Sulfur capacity is high, chemical cost is low, small investment, easy to operate, can wash the removing with H 2 S-containing gas such as Claus tail gases using refinery gas, natural gas, associated gas, coal gasification apparatus and synthesis ammonia plant process gas, amine method, low-temp methanol.
Description
Technical field
The invention belongs to gas purification technique fields, and in particular to a kind of sulfur removal technology and device that absorption and regeneration is synchronous,
Sulfide hydrogen unstripped gas and regeneration gas sulfur dioxide enter simultaneously in comprehensive absorption and regeneration tower, the removing of hydrogen sulfide and desulfurization solvent
Regeneration synchronous carry out.
Background technique
The industries such as oil and gas exploitation, refinery, coal chemical industry, water process, smelting can generate H to some extent2S, especially
It is natural gas extraction and biogas production, H2The removing of S is necessary production technology.As global environmental pollution is increasingly tight
Weight, countries in the world have all formulated stringent environmental regulation, have limited and discharge SO into atmosphere2、H2The toxic and harmful gas such as S, it would be highly desirable to open
Send out the H of clean and effective2S removal methods, to solve current H2The at high cost, sulphur that S removing is faced is stifled and secondary pollution problems.
Removing H at present2There are many method of S, but it is widely used mainly have dry desulfurization, wet oxidation desulfurization,
Alcohol amine desulfurization.Dry desulfurization since Sulfur capacity is limited, regeneration cycle use the problem of, be chiefly used in small-scale high-precision desulfurization.
Wet oxidation desulfurization is its advantage is that sulphur can be directly translated by the hydrogen sulfide in gas.But there is also its equipment volume Pangs
Greatly, process flow is long, equipment investment is big, solution internal circulating load is big, blocking and mist, operation difficulty are big, driving and parking is difficult etc. easily occurs
Problem limits application of the wet desulphurization in middle and small scale especially Oil & gas field in sulfur and selexol process.The alcohol ammonia process of desulfurization
Still there is sour gas generation during later regeneration, to increase subsequent sulfur recovery unit.
The technique of these methods all uses absorption plant and regenerating unit to combine.Desulfurizing agent need to be continuously replenished in sweetening process,
And it is more and big there are appliance arrangement, it takes up a large area, process flow is complicated, and required auxiliary facility is more, and maintenance and maintenance difficulty are big,
The problems such as energy consumption is high, operating cost is high, desulfurizing agent number of dropouts is big.Therefore need to develop that desulfurization process is simple, desulfuration efficiency
Height, small investment, easy to operate recovery technology of sulfur, to meet the desulfurization demand of different process gas.
Summary of the invention
It is an object of the invention to provide a kind of synchronous sulfur methods of absorption and regeneration.
The synchronous sulfur removal technology of absorption and regeneration of the present invention, its main feature is that process flow is simple, a step can be by H2S
It is converted to elementary sulfur, elementary sulfur monomer exists in the form of the liquid sulfur being dissolved in desulfurization solvent, rather than solid sulfur granules, institute
Can effectively avoid blistering, blocking and the other operational issues in technique.
The method of the present invention mainly includes following process engineering:
(1) sulfide hydrogen unstripped gas and regeneration gas sulfur dioxide after pretreatment, while entering comprehensive absorption and regeneration tower bottom
And along tower and on, by organic phase desulfurization solvent bubble absorption, spray-absorption, packing section absorb after, hydrogen sulfide and desulfurization solvent
It is removed in conjunction with the polysulfide for forming protonation, the purified gas after removing hydrogen sulfide is vented after entering gas-liquid separator by tower top
Or it is outer defeated；
(2) the regeneration gas sulfur dioxide for being desulfurized solvent absorption during hydrogen sulfide stripping and the protonation in solvent
Polysulfide synchronizes regenerative response, and polysulfide is transformed into elementary sulfur and is dissolved in organic desulfurization solvent, and organic desulfurization is molten
Agent is regenerated, and sulphur crystallization is precipitated in elementary sulfur after cooling in refrigerated separation slot.Organic desulfurization that sulphur is precipitated is molten
Agent enters each section of circulation desulfurization of integrated absorption tower after being pumped up heater heating；
(3) the cooling crystallization sulphur being precipitated, which reaches a certain amount of, to be periodically discharged by refrigerated separation slot.
In present invention process, the comprehensive absorption and regeneration tower contains bubbling segment, spray section and packing section, can be according to specific
Working condition selects a kind of or Multiple Combination to absorb；Absorption and regeneration temperature is at 35~85 DEG C, and preferably 50~70 DEG C.
The regeneration gas sulfur dioxide can be transformed by hydrogen sulfide or sulfur burning.
The organic phase desulfurization solvent is a kind of water-free compounding organic solution, and effective Sulfur capacity is 2.0~8.5g/L.
The organic phase desulfurization solvent includes desulfurizing agent, promotees steady agent and mutual solvent；Desulfurizing agent includes tertiary amines, PHX, N-
One of methyl cyclohexylamine, triethanolamine and their derivative or a variety of mixtures；Promoting steady agent includes benzyl alcohol, benzyl carbinol
And one of their derivative or a variety of mixtures；Mutual solvent include diarylethane, N-Methyl pyrrolidone, tetraether,
Sulfide hydrogen unstripped gas described in pyridine and the one or more mixtures of their derivative and regeneration gas sulfur dioxide can be distinguished
Gas distributor into comprehensive absorption and regeneration tower, can also enter a gas distributor simultaneously.
The refrigerated separation slot must have two or more parallel installation, can not influence entire technique when sulphur is crystallized and is discharged
Normal operation.
The a small amount of water generated in absorption and regeneration reaction process forms steam discharge after heating.
The charge proportion of hydrogen sulfide and regeneration gas sulfur dioxide is 2: 1~2: 1.4, preferably 2: 1.1~2 in the unstripped gas
∶1.2。
Apparatus of the present invention equipment is simple, and the mesh of desulfurization progress synchronous with solvent reclamation is reached using comprehensive absorption and regeneration tower
, without increasing regenerating unit.And desulphurization reaction process is single, the sulphur of generation is dissolved in desulfurization solvent, effectively prevents it
The problems such as sulphur existing for his method is stifled and blisters；The sulphur crystallized out can also be used as desulfurization material, and operating cost is low.
Inventive desulfurization process flow is simple, desulfuration efficiency is high, solution internal circulating load is low, chemical cost is low, small investment, behaviour
Facilitate, device has preferable operability, there is preferable economical and environmentally friendly benefit.
Detailed description of the invention
Fig. 1 is the process flow chart of the embodiment of the present invention.
In figure, 1 --- gas-liquid separator 2 --- comprehensive absorption and regeneration tower 3,4 --- crystallization sulphur refrigerated separation slot
5 --- pump 6 --- heaters.
Specific embodiment
Below with reference to embodiment and attached drawing, the invention will be further described.
Embodiment 1: unstripped gas tolerance 1.0m3/ h, hydrogen sulfide content~80g/m3, regeneration gas tolerance~27L/h such as attached drawing 1
It is shown, sulfide hydrogen unstripped gas and regeneration gas sulfur dioxide, while enter comprehensive 2 bottom of absorption and regeneration tower and along tower and on, warp
After crossing organic phase desulfurization solvent bubble absorption, spray-absorption, packing section absorption, the purified gas after removing hydrogen sulfide is entered by tower top
Emptying or outer defeated after gas-liquid separator 1.It is anti-that protonation polysulfide in regeneration gas sulfur dioxide and solvent synchronizes regeneration
It answers, polysulfide is transformed into elementary sulfur and is dissolved in organic desulfurization solvent, and the organic desulfurization solvent of sulfur-bearing passes through refrigerated separation slot 3,
Sulphur crystallization is precipitated in elementary sulfur after cooling, and desulfurization solvent is squeezed into heater 6 by pump 5 and heated, and enters back into comprehensive absorb again
Raw tower circulation desulfurization.Desulfurization results are as follows:
| Serial number | It absorbs temperature (DEG C) | Unstripped gas H2S(g/m3) | Purified gas H2S(mg/m3) |
| 1 | 50 | 78.5 | 26 |
| 2 | 60 | 80.2 | 15 |
| 3 | 70 | 77.8 | 5 |
| 4 | 80 | 79.0 | 3 |
Embodiment 2: unstripped gas tolerance 1.0m3/ h, hydrogen sulfide content~80g/m3, absorb temperature 70 C.
As shown in Fig. 1, sulfide hydrogen unstripped gas and regeneration gas sulfur dioxide, while entering comprehensive 2 bottom of absorption and regeneration tower
Portion and along tower and on, by organic phase desulfurization solvent bubble absorption, spray-absorption, packing section absorb after, remove hydrogen sulfide after
Purified gas is entered after gas-liquid separator 1 by tower top to be vented or outer defeated.Protonation in regeneration gas sulfur dioxide and solvent vulcanizes more
Object synchronizes regenerative response, and polysulfide is transformed into elementary sulfur and is dissolved in organic desulfurization solvent, the organic desulfurization solvent of sulfur-bearing
By refrigerated separation slot 3, sulphur crystallization is precipitated in elementary sulfur after cooling, and desulfurization solvent is squeezed into heater 6 by pump 5 and heated,
Enter back into comprehensive absorption and regeneration tower circulation desulfurization.Desulfurization results are as follows:
Claims (10)
1. a kind of absorb the sulfur method synchronous with regeneration, it is characterised in that:
(1) sulfide hydrogen unstripped gas and regeneration gas sulfur dioxide after pretreatment, while entering comprehensive absorption and regeneration tower bottom
And along tower and on, by organic phase desulfurization solvent bubble absorption, spray-absorption, packing section absorb after, hydrogen sulfide and desulfurization solvent
It is removed in conjunction with the polysulfide for forming protonation, the purified gas after removing hydrogen sulfide is vented after entering gas-liquid separator by tower top
Or it is outer defeated；
(2) the regeneration gas sulfur dioxide for being desulfurized solvent absorption during hydrogen sulfide stripping and the protonation in solvent
Polysulfide synchronizes regenerative response, and polysulfide is transformed into elementary sulfur and is dissolved in organic desulfurization solvent, and organic desulfurization is molten
Agent is regenerated, and sulphur crystallization is precipitated in elementary sulfur after cooling in refrigerated separation slot；Organic desulfurization that sulphur is precipitated is molten
Agent enters each section of circulation desulfurization of integrated absorption tower after being pumped up heater heating；
(3) the cooling crystallization sulphur being precipitated is discharged by refrigerated separation slot.
2. according to the method described in claim 1, it is characterized in that the refrigerated separation slot is two or more parallel is installed.
3. according to the method described in claim 1, it is characterized by: comprehensive absorption and regeneration tower contain bubbling segment, spray section and
Packing section；Absorption and regeneration temperature is 35~85 DEG C.
4. according to the method described in claim 3, it is characterized by: absorption and regeneration temperature is 50~70 DEG C.
5. according to the method described in claim 1, it is characterized by: regeneration gas sulfur dioxide is converted by hydrogen sulfide or sulfur burning
?；The organic phase desulfurization solvent is water-free compounding organic solution, and effective Sulfur capacity is 2.0~8.5g/L.
6. method according to claim 1 or 5, it is characterised in that: the organic phase desulfurization solvent includes desulfurizing agent, promotees
Steady agent and mutual solvent；The desulfurizing agent includes in tertiary amines, PHX, N-methylcyclohexylamine, triethanolamine and their derivative
One or more mixtures；It includes one of benzyl alcohol, benzyl carbinol, phenol and their derivative or a variety of mixed for promoting steady agent
Close object；Mutual solvent includes diarylethane, pyrrolidinone compounds, tetraether, pyridine and the one or more mixtures of their derivative.
7. according to the method described in claim 1, it is characterized by: sulfide hydrogen unstripped gas after pretreatment and regeneration gas two
Sulfur oxide respectively enters the gas distributor in comprehensive absorption and regeneration tower, or enters in a gas distributor simultaneously.
8. according to the method described in claim 1, it is characterized by: a small amount of water generated in absorption and regeneration reaction process,
Steam discharge is formed after heating.
9. according to the method described in claim 1, it is characterized by: in unstripped gas hydrogen sulfide and regeneration gas sulfur dioxide charging
Ratio is 2: 1~2: 1.4.
10. according to the method described in claim 9, it is characterized by: in unstripped gas hydrogen sulfide and regeneration gas sulfur dioxide into
Material ratio 2: 1.1~2: 1.2.
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| CN201710895112.1A CN109569193B (en) | 2017-09-28 | 2017-09-28 | Desulfurization method with synchronous absorption and regeneration |
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| CN109569193B CN109569193B (en) | 2021-10-29 |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110756002A (en) * | 2019-10-23 | 2020-02-07 | 中国石油化工股份有限公司 | Absorption liquid and method for recovering sulfur from gas containing hydrogen sulfide and sulfur dioxide |
| CN112138527A (en) * | 2019-06-27 | 2020-12-29 | 中国石化工程建设有限公司 | Synthetic oil reaction tail gas treatment device and method |
| CN113134284A (en) * | 2020-01-19 | 2021-07-20 | 中国石油天然气股份有限公司 | Gas desulfurization discharging equipment |
| CN114177759A (en) * | 2021-12-23 | 2022-03-15 | 江西自立环保科技有限公司 | Method for removing polysulfide ions in organic amine absorption liquid |
| CN115445421A (en) * | 2022-08-05 | 2022-12-09 | 中国石油化工股份有限公司 | Double-enhanced sulfur tail gas absorption method |
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| CN103771347A (en) * | 2012-10-22 | 2014-05-07 | 中国石油化工股份有限公司 | Method for converting hydrogen sulfide into crystalline sulfur by using anhydrous solvent |
| CN104548934A (en) * | 2013-10-22 | 2015-04-29 | 中国石油化工股份有限公司 | Oxidative desulfurization process for continuous regeneration of desulfurizing agent |
| CN204380492U (en) * | 2014-12-08 | 2015-06-10 | 北京智创环绿科技有限公司 | The treatment facility of a kind of sulfide hydrogen and ammonia foul gas |
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| US4440551A (en) * | 1980-08-01 | 1984-04-03 | Bergwerksverband Gmbh | Method for the adsorptive removal of hydrogen sulfide from gas mixtures |
| JPH11276841A (en) * | 1998-03-31 | 1999-10-12 | Nippon Steel Chem Co Ltd | Device for submerged regeneration in wet desulfurizing |
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112138527A (en) * | 2019-06-27 | 2020-12-29 | 中国石化工程建设有限公司 | Synthetic oil reaction tail gas treatment device and method |
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| CN113134284A (en) * | 2020-01-19 | 2021-07-20 | 中国石油天然气股份有限公司 | Gas desulfurization discharging equipment |
| CN113134284B (en) * | 2020-01-19 | 2022-08-30 | 中国石油天然气股份有限公司 | Gas desulfurization discharging equipment |
| CN114177759A (en) * | 2021-12-23 | 2022-03-15 | 江西自立环保科技有限公司 | Method for removing polysulfide ions in organic amine absorption liquid |
| CN114177759B (en) * | 2021-12-23 | 2023-11-03 | 江西自立环保科技有限公司 | Method for removing polysulfide ions in organic amine absorption liquid |
| CN115445421A (en) * | 2022-08-05 | 2022-12-09 | 中国石油化工股份有限公司 | Double-enhanced sulfur tail gas absorption method |
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