CN106939172A - A kind of oxidized regenerating method of sulfur-bearing alkali lye - Google Patents
A kind of oxidized regenerating method of sulfur-bearing alkali lye Download PDFInfo
- Publication number
- CN106939172A CN106939172A CN201610005777.6A CN201610005777A CN106939172A CN 106939172 A CN106939172 A CN 106939172A CN 201610005777 A CN201610005777 A CN 201610005777A CN 106939172 A CN106939172 A CN 106939172A
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- Prior art keywords
- alkali lye
- sulfur
- disulphide
- oxygen
- bearing
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Classifications
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- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10G—CRACKING HYDROCARBON OILS; PRODUCTION OF LIQUID HYDROCARBON MIXTURES, e.g. BY DESTRUCTIVE HYDROGENATION, OLIGOMERISATION, POLYMERISATION; RECOVERY OF HYDROCARBON OILS FROM OIL-SHALE, OIL-SAND, OR GASES; REFINING MIXTURES MAINLY CONSISTING OF HYDROCARBONS; REFORMING OF NAPHTHA; MINERAL WAXES
- C10G19/00—Refining hydrocarbon oils in the absence of hydrogen, by alkaline treatment
- C10G19/08—Recovery of used refining agents
-
- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10G—CRACKING HYDROCARBON OILS; PRODUCTION OF LIQUID HYDROCARBON MIXTURES, e.g. BY DESTRUCTIVE HYDROGENATION, OLIGOMERISATION, POLYMERISATION; RECOVERY OF HYDROCARBON OILS FROM OIL-SHALE, OIL-SAND, OR GASES; REFINING MIXTURES MAINLY CONSISTING OF HYDROCARBONS; REFORMING OF NAPHTHA; MINERAL WAXES
- C10G2300/00—Aspects relating to hydrocarbon processing covered by groups C10G1/00 - C10G99/00
- C10G2300/20—Characteristics of the feedstock or the products
- C10G2300/201—Impurities
- C10G2300/202—Heteroatoms content, i.e. S, N, O, P
-
- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10G—CRACKING HYDROCARBON OILS; PRODUCTION OF LIQUID HYDROCARBON MIXTURES, e.g. BY DESTRUCTIVE HYDROGENATION, OLIGOMERISATION, POLYMERISATION; RECOVERY OF HYDROCARBON OILS FROM OIL-SHALE, OIL-SAND, OR GASES; REFINING MIXTURES MAINLY CONSISTING OF HYDROCARBONS; REFORMING OF NAPHTHA; MINERAL WAXES
- C10G2300/00—Aspects relating to hydrocarbon processing covered by groups C10G1/00 - C10G99/00
- C10G2300/40—Characteristics of the process deviating from typical ways of processing
- C10G2300/44—Solvents
Abstract
The present invention provides a kind of for the oxidized regenerating method containing low concentration mercaptan soda lye, its mercaptan sodium content≤0.1wt% of the mercaptan soda lye;Alkali lye respectively enters supergravity reactor with oxygen-enriched air and reacted;Under conditions of without catalyst, sodium mercaptides oxidation generation disulphide, at least part disulphide is volatized into tail gas during being somebody's turn to do;Alkali lye logistics after regeneration is with carrying the off-gas stream of gas phase disulphide respectively away from supergravity reactor.This method replaces traditional oxidizing tower using supergravity reactor, realizes the deep oxidation of sodium mercaptides;Using the oxygen-enriched air of oxygen percent by volume >=35% as oxidant, oxidation rate is further increased;Without Cobalt Phthalocyanine class catalyst, catalyst cost is saved;Realize that disulphide and alkali lye are efficiently separated using big gas liquid ratio under steady state conditions, a reactor, save disulphide separation link, process is nearly free from spent lye.
Description
Technical field
The present invention relates to a kind of method of alkali liquid regeneration, specifically a kind of alkali lye containing sodium mercaptides and disulphide
Oxidized regenerating method.
Background technology
Mercaptan is a kind of sulfide with off-odor, is present in liquefied gas and other light-end products more.
Mercaptan can accelerate oil oxidation to generate colloid as a kind of oxidizing initiators, make under the quality and stability of oil product
Drop.In addition, mercaptan has an effect on sensitivity of the oil product to additives such as antioxidant, anti-knock agents.For lightweight
The removing of mercaptan in oil product, industrial at present generally to use lye extraction desulfurization alcohol technique, its technological process is such as
Under:Gasoline containing mercaptan and agent aqueous slkali (i.e. sulfonated phthalocyanine cobalt alkali lye) counter current contacting in extraction tower,
Mercaptan generates sodium mercaptides with NaOH reaction and is transferred in alkali lye;Alkali lye containing sodium mercaptides enters oxidation
System, sodium mercaptides are oxidized to disulphide in the presence of oxygen in catalyst and air;Alkali after regeneration
Liquid is separated with disulphide into disulphide knockout drum by gravitational settling, and the alkali lye after separation is returned
Extraction unit is recycled.
The content analysis of sodium mercaptides in alkali lye is shown, the sodium mercaptides changed in alkali alkali lye at initial stage maintain relatively low dense
Degree, generally in below 0.1wt%, with the increase of circular regeneration number of times, sodium mercaptides are built up in alkali lye.
Product mercaptan and total sulfur content after extracting are also stepped up, and cyclically-varying is presented with the alkali time is changed, on
State problem generally by the way of removable parts or whole alkali lye to alleviate, the replacement cycle is typically at one to three
Month, when serious within one month.Spent lye containing catalyst is difficult to handle due to stink and color, leads
Cause environmental protection pressure larger.There are the following problems in the process of running for conventional lye extraction desulfurization alcohol technique:
1. sodium mercaptides conversion ratio is relatively low in regenerative process, sodium mercaptides conversion ratio generally only has about in oxidizing tower
30%~50%, cause sodium mercaptides in circulation alkali liquor gradually to accumulate, be mainly shown as that product mercaptans content is high.
2. product disulphide removal efficiency is low, due to microemulsified and disulphide and the alkali lye two of disulphide
Person's difference in specific gravity is smaller, can not be still clearly separated after gravitational settling.Circulation alkali liquor is caused to carry a large amount of two sulphur
Compound, is finally carried into oil product in extraction system by back suction, is mainly shown as that product total sulfur is exceeded.
3. Cobalt Phthalocyanine class catalyst easy aggregation inactivation in alkali lye, need to frequently add catalyst, catalyst into
This of a relatively high (about 40~600,000 yuan/ton), increase operating cost.
Chinese patent CN200710071004.9 discloses a kind of liquid gas sweetening alkali liquor oxidized regeneration method
And device.This method by after removal of mercaptans alkali lye fraction carry out oxidation regeneration obtain regenerate alkali lye, then with greatly
The unregenerated alkali lye in part merges blending circulation and removes sweetening reaction device, and disulphide in regeneration alkali lye is controlled with this
Content.This method does not carry out substantial improvements to oxidation unit and separator, and due to de- only to part
Mercaptan alkali lye, which carries out regeneration, causes circulation alkali liquor of low quality, influence regeneration alkali lye extraction effect.
Chinese patent CN201410454906.0 discloses two sulphur of a kind of desulfurization alcoholic lye deep oxidation and separation
The method and device of compound.Alkali lye to be generated and air are distributed by this method respectively through liquid distribution trough and air
Device enters oxidizing tower, and extracts contactor depth extraction disulphide by tunica fibrosa, improves regeneration alkali lye matter
Amount.This method is only improving the conversion ratio of sodium mercaptides in oxidizing tower to a certain degree, is applied to by tunica fibrosa
During the extraction of disulphide, because filament is very strict to medium purity requirements, if catalyst
Dissolubility it is bad or it is unstable assemble, filter or pipeline can all blocked, it is impossible to realize two
Sulfide is effectively removed.
Chinese patent CN200710100287.5 discloses a kind of method of hot-soda washing desulfurization, and this method is used
Disulphide in stable gasoline alkali lye carries out back suction and carried, and improves removal efficiency.But it is molten in actual motion
The anti-extraction process of agent oil only has about 10%~30% to the removal efficiency of disulphide, and separating effect is limited.
It is to solve disulphide separation problem row to improve note air quantity to promote disulphide gasification to be volatized into tail gas
Effective method.Disulphide is at utmost converted into gas phase, its efficiently separating with alkali lye can be achieved.
, typically can only be by note air quantity increase but conventional oxidation tower and other mixing apparatus are due to the limitation of operating condition
5-10 times, injection air utilization ratio is low and is difficult stable operation.
Chinese patent CN201110401464.X discloses a kind of method that disulphide is separated from alkali lye,
Supergravity reactor is applied to the removing of disulphide in alkali lye after regeneration by this method, can be by two in alkali lye
Sulfide content is down within 5ppmw, and this method does not enter sodium mercaptides oxidation with disulphide subtractive process
Row coupling, process not enough optimizes.Chinese patent CN201310655920.2 discloses one kind and contains mercaptides
The oxidized regenerating method of alkali lye, by sodium mercaptides oxidation and disulphide separation process in same hypergravity equipment
It is middle to be coupled, splendid alkali liquid regeneration effect, the condition that reaction need to exist in oxidation catalyst can be reached
It is lower to carry out.
High-gravity technology is a kind of typical chemical process reinforcement technique, has been widely used at home at present
In terms of nano material preparation and sour gas vent gas treatment, achievement is notable.Supergravity reactor passes through simulation
Super gravity field realizes the reinforcing to microcosmic mixing and alternate transmission in heterogeneous reaction process, can be to a certain extent
Conventional oxidation tower is overcome the shortcomings of in mass transport process, improves sodium mercaptides reaction depth.Sodium mercaptides are in alkali lye
Homogeneous system is formed, as oxidant normal temperature oxidation reaction can occur for molecular oxygen using in air.In its content dimension
Hold in reduced levels, reaction can reach more than 90% turn without catalyst under excess oxygen
Rate.The present invention provides a kind of operation more optimized on the basis of Chinese patent CN201310655920.2.
Supergravity reactor another advantage is that larger gas liquid ratio can be provided, such as at steady state operation
100~200:1, the maximum gas liquid ratio that can be reached much larger than oxidizing tower.The spy for strengthening mass transfer using hypergravity
Point improves sodium mercaptides reaction depth, while promote product disulphide to separate using its big gas liquid ratio condition, will
Sodium mercaptides are aoxidized and disulphide separation process is coupled, and production efficiency can be greatly improved, and simplify operation stream
Journey.
The content of the invention
It is an object of the invention to provide a kind of oxidized regenerating method of sulfur-bearing alkali lye, sulphur in regenerative process is improved
The enrichment of sulphur, extends alkali lye cycle period, realizes carrying for operational efficiency in sodium alkoxide oxidation efficiency, reduction alkali lye
Rise the reduction with operating cost.
To reach above-mentioned purpose, the present invention provides a kind of oxidized regenerating method of sulfur-bearing alkali lye, the sulfur-bearing alkali lye
Middle mercaptan sodium content≤0.1wt%, sulfur-bearing alkali lye respectively enters supergravity reactor with oxygen-enriched air and carried out instead
Should, sodium mercaptides oxidation generation disulphide, part disulphide is volatized into tail gas;Alkali lye after regeneration is taken
Tail gas of the band containing disulphide leaves supergravity reactor.
The oxidized regenerating method of sulfur-bearing alkali lye of the present invention, these, it is preferred to, the oxygen-enriched air
In oxygen content >=35v%.
The oxidized regenerating method of sulfur-bearing alkali lye of the present invention, wherein, gas-liquid in the supergravity reactor
Two-phase is preferably with adverse current, cocurrent or baffling formal operations.
The oxidized regenerating method of sulfur-bearing alkali lye of the present invention, wherein, the oxygen-enriched air and sulfur-bearing alkali lye
Input material volume ratio be 50~500:1, sulfur-bearing alkali lye feeding temperature is 30~70 DEG C, the supergravity reactor
Interior reaction condition is:Pressure is normal pressure~0.5MPa, and rotating speed is 200~2000 revs/min.
The oxidized regenerating method of sulfur-bearing alkali lye of the present invention, wherein, the sodium mercaptides are preferably methyl mercaptan
Sodium or/and ethyl mercaptan sodium.
Compared with prior art, the advantage of the invention is that:This method replaces tradition using supergravity reactor
Oxidizing tower, realize the deep oxidation of sodium mercaptides;Use oxygen percent by volume for oxygen-enriched air conduct
Oxidant, further increases oxidation rate;Without Cobalt Phthalocyanine class catalyst, catalyst cost is saved;
Behaviour realizes that disulphide and alkali lye are efficiently separated using big gas liquid ratio under steady state conditions, a reactor, saves disulphide point
From link, process is nearly free from spent lye.
Embodiment
With reference to specific embodiment, the present invention is further detailed explanation.
Comparative example 1
Alkali lye containing sodium mercaptides and disulphide is regenerated, cobalt sulfonated phthalocyanine content is
10ppmw, 50 DEG C of alkali lye feeding temperature, using compressed air, heat-exchange temperature is up to entering hypergravity at 50 DEG C
Reactor, overweight 1200 revs/min of machine rotating speed, operating pressure is normal pressure, and gas-liquid volume ratio is 100:1.
The contrast of alkali lye property is shown in Table 1 before and after regeneration.
Table 1
Raw material alkali lye | Regenerate alkali lye | |
Sodium mercaptides, wt% | 0.1 | 0.01 |
Disulphide, ppmw | 60 | < 1 |
Embodiment 1
Sulfur-bearing alkali lye containing sodium mercaptides and disulphide is regenerated, without catalyst, sulfur-bearing alkali lye
Feeding temperature is 50 DEG C, and using the oxygen rich gas that oxygen content is 50v%, gas-liquid volume ratio is 100:1, change
Enter supergravity reactor during 50 DEG C of Re Wenduda, overweight machine rotating speed is 1000 revs/min, and operating pressure is
Normal pressure, gas-liquid two-phase is operated with countercurrent flow.The contrast of alkali lye property is shown in Table 2 before and after regeneration.
Table 2
Raw material alkali lye | Regenerate alkali lye | |
Sodium mercaptides, wt% | 0.1 | 0.01 |
Disulphide, ppmw | 60 | < 1 |
Embodiment 2
Sulfur-bearing alkali lye containing sodium mercaptides and disulphide is regenerated, without catalyst, sulfur-bearing alkali lye
Feeding temperature is 50 DEG C, using the oxygen rich gas that oxygen content is 35v%, and gas-liquid specific volume is 100:1, change
Enter supergravity reactor during 50 DEG C of Re Wenduda, overweight machine rotating speed is 1200 revs/min, and operating pressure is
Normal pressure, gas-liquid two-phase is with baffling formal operations.The contrast of alkali lye property is shown in Table 3 before and after regeneration.
Table 3
Raw material alkali lye | Regenerate alkali lye | |
Sodium mercaptides, wt% | 0.05 | < 0.001 |
Disulphide, ppmw | 60 | < 1 |
Embodiment 3
Sulfur-bearing alkali lye containing sodium mercaptides and disulphide is regenerated, without catalyst, sulfur-bearing alkali lye
Feeding temperature is 45 DEG C, using the oxygen rich gas that oxygen content is 75v%, and gas-liquid specific volume is 200:1, change
Enter supergravity reactor during 45 DEG C of Re Wenduda, overweight machine rotating speed is 1200 revs/min, and operating pressure is
Normal pressure, gas-liquid two-phase is with cocurrent formal operations.The contrast of alkali lye property is shown in Table 4 before and after regeneration.
Table 4
Raw material alkali lye | Regenerate alkali lye | |
Sodium mercaptides, wt% | 0.01 | < 0.001 |
Disulphide, ppmw | 60 | < 1 |
Certainly, the present invention can also have other various embodiments, without departing substantially from spirit of the invention and its essence
In the case of, those of ordinary skill in the art can make various corresponding changes and change according to the present invention
Shape, but these corresponding changes and deformation should all belong to protection scope of the present invention.
Claims (5)
1. mercaptan sodium content≤0.1wt% in a kind of oxidized regenerating method of sulfur-bearing alkali lye, the sulfur-bearing alkali lye, its
It is characterised by, sulfur-bearing alkali lye respectively enters supergravity reactor with oxygen-enriched air and reacted, sodium mercaptides oxidation
Disulphide is generated, part disulphide is volatized into tail gas;Alkali lye after regeneration is carried containing disulphide
Tail gas leaves supergravity reactor.
2. the oxidized regenerating method of sulfur-bearing alkali lye according to claim 1, it is characterised in that the richness
Oxygen content >=35v% in oxygen air.
3. the oxidized regenerating method of sulfur-bearing alkali lye according to claim 1, it is characterised in that described super
Gas-liquid two-phase is with adverse current, cocurrent or baffling formal operations in gravity reactor.
4. the oxidized regenerating method of sulfur-bearing alkali lye according to claim 1, it is characterised in that the richness
The input material volume ratio of oxygen air and sulfur-bearing alkali lye is 50~500:1, sulfur-bearing alkali lye feeding temperature is 30~70 DEG C,
Reaction condition is in the supergravity reactor:Pressure be normal pressure~0.5MPa, rotating speed be 200~2000 turns/
Minute.
5. the oxidized regenerating method of sulfur-bearing alkali lye according to claim 1, it is characterised in that the sulphur
Sodium alkoxide is sodium methyl mercaptide or/and ethyl mercaptan sodium.
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Cited By (1)
Publication number | Priority date | Publication date | Assignee | Title |
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CN108704480A (en) * | 2018-04-13 | 2018-10-26 | 中国石油天然气股份有限公司 | A kind of regeneration method of liquid gas sweetening alkali liquor |
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CN104694160A (en) * | 2013-12-06 | 2015-06-10 | 中国石油天然气股份有限公司 | A combined method of light gasoline desulphurization by alkali washing |
CN104694151A (en) * | 2013-12-06 | 2015-06-10 | 中国石油天然气股份有限公司 | An oxidation regeneration method for a thiolate-containing alkali solution |
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Patent Citations (3)
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CN104624033A (en) * | 2013-11-13 | 2015-05-20 | 中国石油天然气股份有限公司 | Combination method for deep desulfurization of liquefied gas |
CN104694160A (en) * | 2013-12-06 | 2015-06-10 | 中国石油天然气股份有限公司 | A combined method of light gasoline desulphurization by alkali washing |
CN104694151A (en) * | 2013-12-06 | 2015-06-10 | 中国石油天然气股份有限公司 | An oxidation regeneration method for a thiolate-containing alkali solution |
Cited By (6)
Publication number | Priority date | Publication date | Assignee | Title |
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CN108704480A (en) * | 2018-04-13 | 2018-10-26 | 中国石油天然气股份有限公司 | A kind of regeneration method of liquid gas sweetening alkali liquor |
WO2019196951A1 (en) * | 2018-04-13 | 2019-10-17 | 中国石油天然气股份有限公司 | Regeneration method for liquefied gas thiol-removing alkaline solution |
KR20200066701A (en) * | 2018-04-13 | 2020-06-10 | 페트로차이나 컴퍼니 리미티드 | Liquefied petroleum gas sweetening alkali solution regeneration method |
JP2021502896A (en) * | 2018-04-13 | 2021-02-04 | ペトロチャイナ カンパニー リミテッドPetrochina Company Limited | How to regenerate alkaline liquid by demercaptan of liquefied gas |
US11142716B2 (en) | 2018-04-13 | 2021-10-12 | Petrochina Company Limited | Regeneration method for liquefied petroleum gas sweetening caustic |
KR102496533B1 (en) | 2018-04-13 | 2023-02-06 | 페트로차이나 컴퍼니 리미티드 | Liquefied Petroleum Gas Sweetening Alkaline Liquid Regeneration Method |
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Application publication date: 20170711 |