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CN102218260A - Absorbent used for removing sulfides in malodorous gases - Google Patents

Absorbent used for removing sulfides in malodorous gases Download PDF

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Publication number
CN102218260A
CN102218260A CN2010101448182A CN201010144818A CN102218260A CN 102218260 A CN102218260 A CN 102218260A CN 2010101448182 A CN2010101448182 A CN 2010101448182A CN 201010144818 A CN201010144818 A CN 201010144818A CN 102218260 A CN102218260 A CN 102218260A
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weight
absorbent
component
sodium
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CN102218260B (en
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何庆生
张建成
刘献玲
曹玉红
田小峰
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China Petrochemical Corp
Sinopec Luoyang Guangzhou Engineering Co Ltd
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Sinopec Luoyang Petrochemical Engineering Corp
China Petrochemical Corp
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Abstract

The invention provides an absorbent used for removing sulfides in malodorous gases and a preparation method thereof, and aims at solving the problems that the existing desulfurization methods have high operating cost, poor desulfurization effects and high solvent cost. The absorbent is prepared from the following raw materials of water, sodium hydroxide or potassium hydroxide, a sodium salt of ethylene diamine tetra-acetic acid (EDTA) or sodium tartrate, p-benzoquinone or tannin, vanadium pentoxide or sodium metavanadate and ethanolamine according to the preparation method provided by the invention. The absorbent can absorb hydrogen sulfide, mercaptans, thioethers and other sulfur-containing acidic gases, and has low cost and a wide application range, the removal rate of hydrogen sulfide is more than 99% and the removal rate of other organic sulfurs is more than 90%.

Description

A kind of absorbent that removes sulfide in the foul gas
Technical field
The invention belongs to the master gas technical field, relate to a kind of absorbent that removes sulfide in the foul gas specifically.
Background technology
Petroleum refining industry is the key industry that produces odor pollution, and the chemical reaction of complexity can produce a large amount of H in the petroleum refining process 2Odorants such as S, COS, mercaptan, thioether.These materials enter atmosphere in modes such as discharging, volatilization, leakages in production, transporting procedures, cause the pollution sources different odor pollution of degree on every side.In recent years, more and more enterprises begins the processing foreign sour crude.It is more outstanding that especially odor pollution problem of environmental pollution becomes.The surrounding environment of each oil plant all faces the trend that odor pollution increases the weight of day by day.
The method that removes these stench sulfide is a lot, is divided into two kinds of dry desulfurization and wet desulphurizations.The method of wet desulphurization both at home and abroad mainly contains at present: anthraquinone disulphonate method (ADA), tannin extract method (TV method), phthalocyanine cobalt sulfonate method, complexing iron, amine method desulfurization etc.
Patent documentation CN1421264 discloses a kind of absorption liquid that removes sulfide from admixture of gas, and this absorption liquid comprises (1) main absorbent, is made up of sterically hindered amines (I) and N methyldiethanol amine (II); (2) cosolvent (III).Adopt this absorption liquid, can be simultaneously with H 2S, COS, mercaptan, thioether sulfides remove.This absorption liquid is based on organic amine, the operating cost costliness, and organic solvent amine itself is degraded easily, need remove heat stable salt.
Patent documentation CN1384046 discloses a kind of desulfurizing tanning extract process, and this technology is squeezed into the solution circulating slot with alkaline tannin extract solution, and the self-loopa groove comes out, and enters splitting of system after the pressurization after filtration and takes off tower, absorbs the H in the gas 2S takes off solution that tower comes out and enters to split and take off regenerator by splitting, the good solution of regeneration by tower bottom flow to the solution circulating slot, pressurized circulation use after filtration; Desulfuration solution comes out to take off tower after filter-press is delivered to become from circulating slot, absorbs the H in the gas 2S takes off solution that tower comes out by change and enters and become precipitation liquid regenerator, and the solution that regeneration is good takes off regenerator by change and comes out, and enters to become precipitation liquid circulating slot, and pressurization after filtration so recycles again.This method is formed complexity for the foul gas of some cell arrangement discharging of petrochemical enterprise, contains multiple complicated organic matter, and hydrogen sulfide, organic sulfur content are all higher.Utilize existing desulfurizing agent and method, be difficult to effective desulfurization.
Patent documentation CN1887406 discloses a kind of H that removes from gaseous mixture 2The solvent of S, this solvent are that the organic amine that adds a kind of secondary amine and have space steric effect in based on the N methyldiethanol amine solution of water or sulfolane is as activator, in order to from containing or do not contain CO 2Mist in remove the method for hydrogen sulfide.The invention provides two groups of solution formulas: (1) is suitable for never containing in organic sulfur or the low organic sulfur compound gas and removes H 2The solution formula of S is: N methyldiethanol amine 30~50 weight %, secondary amine 1~10 weight %, sterically hindered amines 1~15 weight %, and all the other components are water; (2) be suitable for from contain volatile sulfur gases, removing H 2The solution formula of S and part organic sulfur is: N methyldiethanol amine 30~40 weight %, secondary amine 1~5 weight %, sterically hindered amines 1~15 weight %, water 5 weight %, all the other components are sulfolane.This solvent is the organic amine solvent, hydrogen sulfide and organic sulfur are all had removal effect preferably, but solvent cost is very high.
Summary of the invention
In order to solve the high problem of operating cost height, bad desulfurization effects, solvent cost that exists in the above-mentioned sulfur method, the invention provides a kind of absorbent that can remove sulfide in the foul gas.Sulfur-bearing sour gas such as this absorbent energy absorbing hydrogen sulphide, mercaptan, thioether do not produce secondary pollution after the absorption, waste liquid is easily handled, and does not contain elemental sulfur in the product, has avoided reactor plugs.
The raw material that removes the absorbent of sulfide in the foul gas provided by the invention form and content as follows:
(A) diluent 67~85 weight %,
(B) strong inorganic base 10~30 weight %,
(C) complex compound cosolvent 0.5~2 weight %,
(D) catalyst 0.1~1 weight %,
(E) oxidant 0.5~2 weight %,
(F) strengthen absorbent 1~4 weight %.
Above-mentioned raw materials mixed, reacts by following preparation method can make absorbent of the present invention:
(1) calculates the required weight of each component according to the proportional meter of each component in the raw material;
(2) elder generation adds in container and should add 60%~80% of component (A) total amount, add the component (C) of capacity afterwards, and be stirred to dissolving fully, add the component (B) of capacity then, and be stirred to dissolving, dissolve, react in the adding container with the component (D) of capacity with (E) at last;
(3) treat in the container all components all dissolving and temperature reduced to below 40 ℃ after, in container, add component (F), replenish simultaneously and add remaining component (A) and also mix, absorbent preparation is so far finished.
Wherein, described diluent (A) is pure water or running water, is used for diluting the active ingredient in the absorbent;
Described strong inorganic base (B) is NaOH or potassium hydroxide, preferred NaOH, and this component is main chemical absorbing component, and sulfide is sour gas, and most component all can react with highly basic;
Described complex compound cosolvent (C) is the sodium salt (EDTA) or the sodium potassium tartrate tetrahydrate of ethylenediamine tetra-acetic acid, or both mixtures, and main effect is a complexing part metals ion, prevents that a small amount of ion from producing precipitation, shields some active metallic ion and participates in reaction;
Described catalyst (D) is 1,4-benzoquinone or tannin, plays catalytic action, and itself can be an oxidizing substance by dioxygen oxidation, has the function of catching oxygen in the foul gas;
Described oxidant (E) is vanadic anhydride or sodium metavanadate, plays oxidation, and itself can be by the reduction of the sulfide in the foul gas, and the low price vanadium of Sheng Chaning can be oxidized to the high price vanadium by oxygen and catalyst (D) simultaneously;
Described reinforcement absorbent (F) is a monoethanolamine, and the process of absorbing hydrogen sulphide is the Physical Absorption process.
According to double-film theory, absorb resistance in the Physical Absorption process and comprise air film resistance and liquid-film resistance, the gas phase total absorption coefficient is:
1 K G = 1 k G + 1 Hk L
In MODEL OF CHEMICAL ABSORPTION PROCESS, chemical reaction velocity has great influence to absorption process, divides according to chemical reaction velocity, and may there be three kinds of reactions in MODEL OF CHEMICAL ABSORPTION PROCESS: transient response, fast reaction and long response time.
Component among the present invention (B) absorbing hydrogen sulphide is irreversible chemical reaction at a slow speed, when component (B) when concentration ratio is higher, can be considered irreversible chemical reaction at a slow speed.The MODEL OF CHEMICAL ABSORPTION PROCESS resistance can be similar to Physical Absorption.But component (F) absorbing hydrogen sulphide is instantaneous reversible reaction, can greatly strengthen absorption process with component (F) solution absorbing hydrogen sulphide.Component (F) boiling point substance height, good stability are difficult for decomposing.The reaction of component (F) absorbing hydrogen sulphide generates salt, and is with component (B) reaction, born more again.Like this, in component (B), add component (F), can in absorption process, play the effect of similar catalyst.
The principle that this absorbent absorbs oxidation of sulfureted hydrogen, mercaptan, thioether is as follows:
H 2S+2OH -→S 2-+2H 2O S 2-+4[O]+OH→SO 4 2-+H 2O
RSH+OH -→RS -+H 2O RSH+[O]+OH -→(RS) 2+H 2O
(RS) 2+[O]+OH -→SO 4 2-+H 2O+RCOO -
Absorbent of the present invention is the special-purpose absorbent of a kind of volatility gases containing stench sulphureous gases of function admirable, can be applicable to refine oil, the foul waste gas of factories such as chemical industry, natural gas administers.Sulfur-bearing sour gas such as this absorbent can absorbing hydrogen sulphide, mercaptan, thioether, do not produce secondary pollution after the absorption, promptly do not produce DMDS, the product that generates is high price sulfate radical, inferior sulfate radical, thiosulfate anion etc., waste liquid is easily handled, do not contain elemental sulfur in the product, avoided reactor plugs.This absorbent cost is low, nontoxic, the scope of application is wide, remove in the waste gas hydrogen sulfide content from several milligrams/cubic metres to thousands of milligram/cubic meters, other organic sulfur contents can both reach satisfied effect from several milligrams/cubic metres to hundreds of milligram/cubic meters, the hydrogen sulfide stripping rate is more than 99%, and other organic sulfur removal rates are more than 90%.
The specific embodiment:
The present invention will be further described below in conjunction with specific embodiment, and embodiment 1~6 is the preparation example of absorbent of the present invention, and embodiment 7 is the effect example of absorbent of the present invention.
Embodiment 1
Raw material composition and content are as follows:
(A) running water of 76.5 weight %;
(B) NaOH of 20 weight %;
(C) sodium potassium tartrate tetrahydrate of 1 weight %;
(D) 1,4-benzoquinone of 0.5 weight %;
(E) sodium metavanadate of 1 weight %;
(F) monoethanolamine of 1 weight %.
Above-mentioned raw materials is prepared by preparation method of the present invention can makes absorbent of the present invention.
Embodiment 2
Raw material composition and content are as follows:
(A) running water of 76 weight %;
(B) NaOH of 20 weight %;
(C) sodium potassium tartrate tetrahydrate of 1 weight %;
(D) 1,4-benzoquinone of 1 weight %;
(E) sodium metavanadate of 1 weight %;
(F) monoethanolamine of 1 weight %.
Above-mentioned raw materials is prepared by preparation method of the present invention can makes absorbent of the present invention.
Embodiment 3
Raw material composition and content are as follows:
(A) running water of 76.5 weight %;
(B) NaOH of 20 weight %;
(C) EDTA of 1 weight %;
(D) 1,4-benzoquinone of 1 weight %;
(E) sodium metavanadate of 0.5 weight %;
(F) monoethanolamine of 1 weight %.
Above-mentioned raw materials is prepared by preparation method of the present invention can makes absorbent of the present invention.
Embodiment 4
Raw material composition and content are as follows:
(A) running water of 76 weight %;
(B) NaOH of 20 weight %;
(C) EDTA of 1 weight %;
(D) tannin of 1 weight %;
(E) vanadic anhydride of 1 weight %;
(F) monoethanolamine of 1 weight %.
Above-mentioned raw materials is prepared by preparation method of the present invention can makes absorbent of the present invention.
Embodiment 5
Raw material composition and content are as follows:
(A) running water of 76.5 weight %;
(B) NaOH of 20 weight %;
(C) EDTA of 1 weight %;
(D) tannin of 1 weight %;
(E) vanadic anhydride of 0.5 weight %;
(F) monoethanolamine of 1 weight %.
Above-mentioned raw materials is prepared by preparation method of the present invention can makes absorbent of the present invention.
Embodiment 6
Raw material composition and content are as follows:
(A) running water of 73 weight %;
(B) NaOH of 20 weight %;
(C) EDTA of 1 weight %;
(D) tannin of 1 weight %;
(E) vanadic anhydride of 1 weight %;
(F) monoethanolamine of 4 weight %.
Above-mentioned raw materials is prepared by preparation method of the present invention can makes absorbent of the present invention.The absorbent color of each embodiment and character pair ratio see Table 1.
The color of table 1 embodiment and proterties
Project Color Proterties
Embodiment 1 Rufous A small amount of white solid
Embodiment 2 Rufous A small amount of white solid
Embodiment 3 Rufous Solution is more transparent
Embodiment 4 Bronzing A small amount of brown solid
Embodiment 5 Bronzing A small amount of brown solid
Embodiment 6 Bronzing A small amount of brown solid
Solid particle among embodiment 1 and the embodiment 2 is the solid precipitation that metal ions such as small amount of calcium, magnesium do not have complete complexing dissolving to generate.Mixture after embodiment 4, embodiment 5 and embodiment 6 produce is the bronzing transparency liquid, and a spot of sediment is arranged at the solution bottom, and the inert impurities in this sediment catalyst is not produced novel substance with other substance reactions, does not influence desulfurized effect.
Embodiment 7
With the common fillers tower is absorption equipment, and absorbent of the present invention is carried out hydrogen sulfide absorption effect contrast test, and the concentration of hydrogen sulfide of foul gas is 1500~5000mg/m 3, test result sees Table 2.
The absorbent of each embodiment of table 2 removes the effect of hydrogen sulfide
Project Embodiment 1 Embodiment 2 Embodiment 3 Embodiment 4 Embodiment 5 Embodiment 6
Air inlet H 2S content, mg/m 3 3260 2160 3650 3780 3490 3150
H gives vent to anger 2S content, mg/m 3 10.8 9.5 11.2 5.9 7.1 2.6
H 2The S removal efficiency, % 99.7 99.6 99.7 99.8 99.8 99.9
By the tables of data behind the analytical test 2 as can be seen: embodiment 4, embodiment 5 and embodiment 6 assimilation effects obviously are better than embodiment 1, embodiment 2 and embodiment 3; Comparative example 4 and embodiment 6 strengthen the content height of absorbent, good absorbing effect as can be seen.
Form also discovery by the material after the further analysis absorption: the absorption product Central Asia sulfate concentration of embodiment 4 and embodiment 6 is starkly lower than other embodiment, by analyzing possible reason be: 1,4-benzoquinone generates a spot of hydroquinones in the process that participates in reaction, and hydroquinones has stabilization to sulphite; The a little higher than sodium metavanadate of the oxidation effectiveness of vanadic anhydride.
The desulfurization oxidation effectiveness of comprehensive comparative analysis embodiment 6 is better, and embodiment 6 has been carried out the test of mercaptan assimilation effect, and test result sees Table 3.
The absorbent of table 3 embodiment 6 removes the effect of mercaptan
The air inlet mercaptans content, mg/m 3 207.5 134.4 121.9
The mercaptans content of giving vent to anger, mg/m 3 0 0 0
The mercaptan removal efficiency, % 100 100 100

Claims (2)

1. an absorbent that removes sulfide in the foul gas is characterized in that, the raw material composition and the content of this absorbent are as follows:
(A) diluent 67~85 weight %,
(B) strong inorganic base 10~30 weight %,
(C) complex compound cosolvent 0.5~2 weight %,
(D) catalyst 0.1~1 weight %,
(E) oxidant 0.5~2 weight %,
(F) strengthen absorbent 1~4 weight %;
This absorbent prepares by following preparation method:
(1) calculates the required weight of each component according to the proportional meter of each component in the raw sorbent;
(2) elder generation adds in container and should add 60%~80% of component (A) total amount, add the component (C) of capacity afterwards, and be stirred to dissolving fully, add the component (B) of capacity then, and be stirred to dissolving, dissolve, react in the adding container with the component (D) of capacity with (E) at last;
(3) treat in the step (2) all components all dissolving and temperature reduced to below 40 ℃ after, in container, add component (F), replenish simultaneously and add remaining component (A) and also mix;
Wherein, described diluent (A) is pure water or running water; Described strong inorganic base (B) is NaOH or potassium hydroxide; Described complex compound cosolvent (C) is the sodium salt (EDTA) or the sodium potassium tartrate tetrahydrate of ethylenediamine tetra-acetic acid, or both mixtures; Described catalyst (D) is 1,4-benzoquinone or tannin; Described oxidant (E) is vanadic anhydride or sodium metavanadate; Described reinforcement absorbent (F) is a monoethanolamine.
2. absorbent according to claim 1 is characterized in that described diluent is a running water, and strong inorganic base is a NaOH, and the complex compound cosolvent is the sodium salt of ethylenediamine tetra-acetic acid, and catalyst is a tannin, and oxidant is a sodium metavanadate.
CN 201010144818 2010-04-13 2010-04-13 Absorbent used for removing sulfides in malodorous gases Active CN102218260B (en)

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Cited By (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN103285714A (en) * 2013-06-17 2013-09-11 连云港盛和生物科技有限公司 Method for removing odor organic gas
CN103432883A (en) * 2013-07-09 2013-12-11 南京信息工程大学 Compound desulfurizer for flue gas
CN106823693A (en) * 2017-03-28 2017-06-13 中北大学 A kind of deep desulfuration absorbent for smoke-gas wet desulfurization
CN114790130A (en) * 2021-01-26 2022-07-26 山东新时代药业有限公司 Deodorization recovery method for organic waste liquid
CN115893711A (en) * 2022-10-26 2023-04-04 中国石油化工股份有限公司 Method for treating organic sulfur in fracturing flow-back fluid suitable for oil and gas field

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CN1887406A (en) * 2005-06-27 2007-01-03 成都华西化工研究所 Solvent for eliminating H2S from gas mixture
CN101249379A (en) * 2008-04-04 2008-08-27 中国石油化工集团公司 Malodorous gas processing assembly technique

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US4808765A (en) * 1987-07-17 1989-02-28 The Dow Chemical Company Sulfur removal from hydrocarbons
US5589149A (en) * 1993-11-09 1996-12-31 Union Carbide Chemicals & Plastics Technology Corporation Process for absorption of mercaptans
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CN101249379A (en) * 2008-04-04 2008-08-27 中国石油化工集团公司 Malodorous gas processing assembly technique

Cited By (9)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN103285714A (en) * 2013-06-17 2013-09-11 连云港盛和生物科技有限公司 Method for removing odor organic gas
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CN103432883A (en) * 2013-07-09 2013-12-11 南京信息工程大学 Compound desulfurizer for flue gas
CN103432883B (en) * 2013-07-09 2016-02-03 南京信息工程大学 A kind of flue gas laminated desulfurizer
CN106823693A (en) * 2017-03-28 2017-06-13 中北大学 A kind of deep desulfuration absorbent for smoke-gas wet desulfurization
CN106823693B (en) * 2017-03-28 2019-08-27 中北大学 A deep desulfurization absorbent for flue gas wet desulfurization
CN114790130A (en) * 2021-01-26 2022-07-26 山东新时代药业有限公司 Deodorization recovery method for organic waste liquid
CN115893711A (en) * 2022-10-26 2023-04-04 中国石油化工股份有限公司 Method for treating organic sulfur in fracturing flow-back fluid suitable for oil and gas field
CN115893711B (en) * 2022-10-26 2023-10-31 中国石油化工股份有限公司 Treatment method suitable for organic sulfur in fracturing flowback fluid of oil and gas field

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Address after: 100728 Beijing, Chaoyangmen, North Street, No. 22, No.

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