CN103045289A - Comprehensive treatment method of liquid hydrocarbon alkali residue waste liquid - Google Patents
Comprehensive treatment method of liquid hydrocarbon alkali residue waste liquid Download PDFInfo
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- CN103045289A CN103045289A CN2011103133139A CN201110313313A CN103045289A CN 103045289 A CN103045289 A CN 103045289A CN 2011103133139 A CN2011103133139 A CN 2011103133139A CN 201110313313 A CN201110313313 A CN 201110313313A CN 103045289 A CN103045289 A CN 103045289A
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Abstract
The invention relates to a comprehensive treatment method of liquid hydrocarbon alkali residue waste liquid. The comprehensive treatment method comprises the steps of: (1) acidizing the liquid hydrocarbon alkali residue waste liquid by a N2/SO2 gas mixture, wherein sulfide in the waste liquid volatilizes in the form of H2S along with the continuous increase of the acidity of the waste liquid; and stopping acidizing when the pH value of the waste liquid reaches 2-6; (2) sending tail gases discharged in the acidizing process in the step (1) into a sulphur production device for preparing sulphur; (3) subsiding the waste liquid generated after the acidizing process in the step (1), and recovering an oil phase, wherein the oil phase mainly contains crude phenol which can be further recovered; and (4) regenerating the waste liquid without the oil phase by using lime, wherein the regenerated waste liquid can be recycled for refinement process of liquid hydrocarbon alkali after precipitates are separated out from the regenerated waste liquid. The comprehensive treatment method is low in investment; the process is simple and flexible; operation conditions are mild; due to the application of the comprehensive treatment method, the alkali residue waste liquid is recycled, the impact of high-concentration waste water on a sewage treatment plant is avoided, simultaneously the sulfide and crude phenol in the alkali residue waste liquid can be recycled, and certain economic benefit is achieved.
Description
Technical field
The present invention relates to a kind for the treatment of process of alkaline residue waste liquid, particularly the integrated conduct method of the alkaline residue waste liquid of liquid alkali cleaning treating process generation.
Background technology
In Refinery Oil alkali cleaning treating process, generation contains the alkaline waste liquor of high density pollution thing, the quantity discharged of its COD, sulfide and phenol accounts for more than 40% ~ 50% of this type of pollutant discharge amount of refinery, mainly is comprised of ordinary pressure diesel alkaline residue, FCC gasoline caustic sludge, liquid hydrocarbon alkaline residue etc.These alkaline residue waste liquids, such as direct discharging, the meeting serious environment pollution if it is delivered to the sewage-farm, will have a strong impact on the normal running in sewage-farm, makes sewage be difficult to qualified discharge, and severe corrosion equipment.The alkaline residue problem is at the refinery ubiquity.In the last few years, along with national environmental protection rules, standard are increasingly complete and strict, and people were more and more higher to the cry that improves environmental quality, and alkaline residue is processed and more and more come into one's own.
In these several alkaline residues, what sulfide content was the highest is FCC gasoline caustic sludge and liquid hydrocarbon alkaline residue, generally use at present wet oxidation to process, the oxidation waste liquid neutralizes with sulfuric acid, reclaims phenol, petroleum acid, produces in the alkaline residue and water, but COD is still very high, can reach 30000mg/L ~ 60000mg/L, and in oxidation and N-process, produce a large amount of salt, impact very large to the sewage-farm of Petrochemical Enterprises.The ordinary pressure diesel alkaline residue mainly contains petroleum acid, generally adopts in the sulfuric acid and the processing of recovery naphthenic acid, produces in the diesel alkaline residue and water, and COD is relatively low, but salt concn is very high, needs just can enter the sewage-farm behind the Macrodilution.
Along with the development of oil refining process for refining, diesel oil and gasoline gradually adopt hydrofining technology, can avoid like this producing the alkaline residue waste liquid.But liquid hydrocarbon can produce the alkaline residue waste liquid of the high COD of corresponding high sulfur content still take the alkali cleaning process for refining as main.
For the processing of the alkaline residue waste liquid of the high COD of high sulfur content, some patent has proposed treatment technology, and hydrolysis method, oxidation style, biological process, extraction process, evaporation burning method etc. are arranged.CN98121081.3 discloses a kind for the treatment of process of salkali waste waste liquid, adopts the method for wet oxidation+intermittent activated sludge process (SBR) combination treatment alkaline residue.But because COD concentration is still very high in the waste water after the wet oxidation, and inorganic salt content is also quite high (contains 200g/L ~ 300g/L) in the alkaline residue that has.Inorganic salt have toxic action to microorganism, and the microorganism in the SBR method generally can be stood the inorganic salt content less than 30 g/L, surpass after this value, and microorganism begins to disintegrate and come-up, finally causes active sludge to run off, and reactor moves unsuccessfully.Therefore when adopting the SBR method to process the alkaline residue waste liquid, adopt the sewage in more fresh water or other source that former water is diluted, to satisfy in the water inlet inorganic salt content less than the requirement of 30 g/L.Like this, the consumption of fresh water is generally 10 times of former water yields when above, just can enter the sbr reactor pond, and the surplus sludge volume of this technique is more in addition, needs regularly to discharge excess sludge, has increased the aftertreatment expense.
CN02130781.4 proposes a kind for the treatment of process of refining oil alkaline residue, comprise: the oil refining alkaline residue that contains evaporation accelerators 101-115 ℃ of lower evaporation, the gaseous condensate that evaporates recycles, and the alkaline residue after concentrating advances incinerator and generates yellow soda ash and sodium sulfate 750-950 ℃ of lower burning.But volatile organism and Stenchy sulfides can send in the process of evaporation in a large number in the alkaline residue waste liquid, cause the gaseous condensate Pollutant levels very high, and evaporation and to burn energy consumption very large.
CN00110702.X has proposed a kind of purifying method of alkaline residue waste liquid, and it is lower to be included in the active sludge existence, and the alkaline residue waste liquid contacts with oxygen-containing gas, and water outlet is discharged by membrane filtration after purifying, and employed film is microfiltration membrane or ultra-filtration membrane.This patent is only applicable to influent COD＜12000mg/L, inorganic salt content＜50mg/L.For in most of alkaline residue and the COD of water all far above this index, still need the fresh water dilution.
CN200510041778.8 has introduced the method for a kind of Alkaline Residue complexometric extraction dephenolize, use two kinds of mixed extractant I and II, successively mixed complexometric extraction with alkaline residue, obtain the three phase extraction system, one is extracting phase mutually, with NaOH back extraction phase I, is extracted agent I and phenol, heating back extraction phase II, can remove the sulfide in the phase II, be extracted the agent II, play the effect of simultaneously desulfurization and phenol.But processing in the alkaline residue back extraction process, the method can produce alkaline waste liquor.
Summary of the invention
The invention provides the integrated conduct method of the high COD liquid hydrocarbon of a kind of high sulfur content alkaline residue waste liquid, can remove efficiently the sulfide in the alkaline residue waste liquid, reduce the COD of waste water, reclaim crude phenols, after causticization regeneration, treating oil by alkali washing is carried out in reuse, can make high-risk unmanageable alkaline residue resource utilization, has greatly reduced environmental pollution.
The integrated conduct method of liquid hydrocarbon alkaline residue waste liquid of the present invention comprises following content:
(1) with N
2/ SO
2Gas mixture liquid towards hydrocarbon alkaline residue waste liquid carries out acidifying, constantly strengthens along with waste liquid is acid, and the sulfide in the waste liquid is with H
2The S form evaporates, and when the pH of waste liquid value reaches 2～6, is preferably at 3～4 o'clock, and stopping acidification is processed;
(2) tail gas that discharges in the acidification process in the step (1) is sent to sulphur production installation and is used for producing sulphur;
(3) waste liquid after step (1) acidification carries out sedimentation, reclaims oil phase, is mainly crude phenols in the oil phase, and crude phenols can further reclaim;
(4) waste liquid that separates in the step (3) behind the oil phase is regenerated with lime, isolate throw out after, be cycled to used in liquid hydrocarbon soda finishing process.
In the inventive method, step (1) N
2/ SO
2In the gas mixture, N
2/ SO
2Mol ratio be 50:1～100:1, SO
2Can be any source, be preferably that isolated throw out (is mainly CaSO in the step (4)
3) carry out the SO that Roasting Decomposition obtains
2The acidification process of step (1) can be with the sulfide clearance 99%(quality in the alkaline residue waste liquid) more than.
In the inventive method, remove N in the tail gas that obtains in the step (2)
2Outward, mainly be hydrogen sulfide, also have a small amount of organic sulfide and sulfurous gas, can be used as the raw material of sulphur production installation, perhaps remove the raw material that is re-used as sulphur production installation behind the organic sulfide wherein.
In the inventive method, after the operation of separation crude phenols, the clearance of phenol can reach the 80%(quality in the step (3)) more than, COD can reach more than 60% by clearance.
In the inventive method, the lime that uses in the step (4) can be white lime or unslaked lime, and the material that works when regenerative response occurs is Ca (OH)
2This step can precipitate and remove 85% inferior sulfate radical in regeneration alkali lye, and basicity can return to more than 40% of former alkaline residue waste liquid, can replenish behind the fresh soda as the refining alkali lye for the treatment of oil by alkali washing.
In the inventive method, liquid hydrocarbon alkaline residue waste liquid is the alkaline residue waste liquid that liquid hydrocarbon soda finishing process produces.
The method of comprehensive utilization of the high COD liquid hydrocarbon of high sulfur content of the present invention alkaline residue waste liquid has following features:
(1) can reclaim sulfide and phenol, reduce COD, make the alkaline residue effluent resource after the causticization regeneration.
The inventive method technique has comprised recovery sulfide and phenol, after causticization regeneration and desalination, can add fresh alkali lye as the refining alkali lye for the treatment of oil by alkali washing by certain proportion.Reclaim the principal pollutant matter of alkaline residue waste liquid, make the alkaline residue effluent resource, have good economic benefit.
(2) technique is succinct, flexible operation, and the investment operation expense is low.
The SO that relates among the present invention
2Acidifying and causticization regenerative operation are simple, need not large scale investment.Operational condition is gentle, does not relate to high-temperature high-pressure apparatus.Integral device investment and process cost are all lower.
Description of drawings
Fig. 1 is the process flow sheet of the inventive method.
Wherein: 1-slag waste liquid, 2-nitrogen, the 3-sulfur dioxide gas, the 4-acidification reactor, 5-acidifying tail gas is sent to the sulphur workshop, 6-dephenolize tank, 7-reclaims crude phenols, the water outlet of regenerating of 8-regeneration reactor, 9-lime/white lime, 10-reaction precipitation thing, 11-.
Embodiment
The comprehensive treating process of the high COD liquid hydrocarbon of high sulfur content of the present invention alkaline residue waste liquid utilizes method mainly to comprise the SO of alkaline residue
2Acidifying and causticization regeneration two portions.
In the inventive method, as shown in Figure 1, at first with N
2As carrier gas, SO carries under one's arms
2The alkaline residue waste liquid is carried out acidifying, reclaim sulfide and phenol in the waste water, sulfide clearance wherein can reach more than 99%, and the volatile phenol clearance can reach more than 80%.Use subsequently Ca (OH)
2Alkaline residue water after the acidifying is carried out causticization regeneration, can precipitate clearance simultaneously and can reach sulfite ion more than 85%.Alkali lye after the regeneration can add fresh alkali lye as the refining alkali lye for the treatment of oil by alkali washing by certain proportion.
Further illustrate the inventive method and effect below in conjunction with example, wherein percentage composition is take quality as benchmark.
Certain enterprise's alkali cleaning liquid hydrocarbon alkaline residue waste liquid, wherein COD is 1.27 * 10
5Mg/L, sulfide are 1.08 * 10
4Mg/L, volatile phenol 1.99 * 10
4Mg/L.Use the inventive method is processed, at first with N
2As carrier gas, SO carries under one's arms
2The alkaline residue waste liquid is carried out acidifying, N
2/ SO
2=100(mol ratio), until the pH of alkaline residue waste liquid is down to 3-4.Be sent to sulphur workshop Cross unit sulphur processed after using the organic sulfide in the desulfuration adsorbent absorption tail gas, sweetening agent can use by reprocessing cycle.Water after the acidifying leaves standstill the phenol that reclaims with water stratification.Acidified processing is removed sulfide more than 99.5%, removes phenol more than 80%, reduces COD more than 60%.
Use Ca (OH)
2Sour water behind the recovery phenol is precipitated regeneration, produce the calcium sulfite precipitation, the inferior sulfate radical clearance can reach more than 85%, and basicity returns to 50% of former alkaline residue waste liquid.Calcium sulfite can roasting obtains sulfurous gas and recycles.
Through the alkaline residue waste liquid after the inventive method processing, can add in proportion certain fresh alkali lye as the refining alkali lye reuse for the treatment of oil by alkali washing.
Certain enterprise's liquid hydrocarbon alkaline residue waste liquid, wherein COD is 1.25 * 10
5Mg/L, sulfide are 1.78 * 10
4Mg/L, volatile phenol 7.17 * 10
4Mg/L.Use the inventive method is processed, at first with N
2As carrier gas, SO carries under one's arms
2The alkaline residue waste liquid is carried out acidifying, N
2/ SO
2=50(mol ratio), until the pH of alkaline residue waste liquid is down to 3-4.Be sent to sulphur workshop Cross unit sulphur processed after using the organic sulfide in the desulfuration adsorbent absorption tail gas, sweetening agent can use by reprocessing cycle.Water after the acidifying leaves standstill the crude phenols that reclaim with water stratification.Acidified processing, phase sulfur compound clearance can reach more than 99.7%, and the phenol clearance can reach more than 80%, and COD can reduce more than 60%.
Use Ca (OH)
2Sour water behind the recovery phenol is precipitated regeneration, produce the calcium sulfite precipitation, the inferior sulfate radical clearance can reach more than 85%, and basicity returns to 50% of former alkaline residue waste liquid.
Through the alkaline residue waste liquid after the inventive method processing, can add in proportion certain fresh alkali lye as the refining alkali lye reuse for the treatment of oil by alkali washing.
Claims (10)
1. the integrated conduct method of a liquid hydrocarbon alkaline residue waste liquid is characterized in that comprising following content:
(1) with N
2/ SO
2Gas mixture liquid towards hydrocarbon alkaline residue waste liquid carries out acidifying, constantly strengthens along with waste liquid is acid, and the sulfide in the waste liquid is with H
2The S form evaporates, and when the pH of waste liquid value reached 2～6, stopping acidification was processed;
(2) tail gas that discharges in the acidification process in the step (1) is sent to sulphur production installation and is used for producing sulphur;
(3) waste liquid after step (1) acidification carries out sedimentation, reclaims oil phase, is mainly crude phenols in the oil phase, and crude phenols can further reclaim;
(4) waste liquid that separates in the step (3) behind the oil phase is regenerated with lime, isolate throw out after, be cycled to used in liquid hydrocarbon soda finishing process.
2. in accordance with the method for claim 1, it is characterized in that: when the pH of waste liquid value reached 3～4, stopping acidification was processed in the step (1).
3. it is characterized in that in accordance with the method for claim 1: step (1) N
2/ SO
2In the gas mixture, N
2/ SO
2Mol ratio be 50:1～100:1.
4. in accordance with the method for claim 1, it is characterized in that: the acidification process of step (1), the sulfide clearance in the alkaline residue waste liquid are more than 99% in mass.
5. in accordance with the method for claim 1, it is characterized in that: after the tail gas that step (2) obtains adopts the method organic sulfide removal compound of absorption, be re-used as the raw material of sulphur production installation.
6. in accordance with the method for claim 1, it is characterized in that: after separating the crude phenols operation in the step (3), the clearance of phenol is more than 80% in mass, and COD can clearance be more than 60%.
7. in accordance with the method for claim 1, it is characterized in that: the lime that uses in the step (4) is white lime or unslaked lime, and the material that works when regenerative response occurs is Ca (OH)
2
8. in accordance with the method for claim 1, it is characterized in that: step (4) is in regeneration alkali lye, and precipitation is removed inferior sulfate radical, and basicity can return to more than 40% of former alkaline residue waste liquid.
9. it is characterized in that in accordance with the method for claim 8: the throw out that precipitation is removed inferior sulfate radical carries out the SO that Roasting Decomposition obtains
2, and be cycled to used in the acidification step of step (1).
10. it is characterized in that in accordance with the method for claim 1: liquid hydrocarbon alkaline residue waste liquid is the alkaline residue waste liquid that liquid hydrocarbon soda finishing process produces.
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN104611003A (en) * | 2013-11-05 | 2015-05-13 | 中国石油化工股份有限公司 | Oil refining alkali dreg waste liquid processing method |
| CN104607435A (en) * | 2013-11-05 | 2015-05-13 | 中国石油化工股份有限公司 | Sulfur-containing alkaline residue comprehensive control method |
| CN104984652A (en) * | 2015-07-11 | 2015-10-21 | 河北新启元能源技术开发股份有限公司 | Treating device for tail gas in acidifying refinement of alkaline residues and treating process thereof |
| CN105712556A (en) * | 2014-12-05 | 2016-06-29 | 中国石油化工股份有限公司 | Processing method of oil refining alkaline residues |
| CN105712457A (en) * | 2014-12-05 | 2016-06-29 | 中国石油化工股份有限公司 | Oil refining alkaline residue acidification reactor with antifoaming function and antifoaming method |
| CN105712456A (en) * | 2014-12-05 | 2016-06-29 | 中国石油化工股份有限公司 | Processing method of alkaline residue waste liquid |
| CN113121033A (en) * | 2019-12-31 | 2021-07-16 | 中国石油化工股份有限公司 | Oil refining alkaline residue treatment method and device |
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Cited By (11)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104611003A (en) * | 2013-11-05 | 2015-05-13 | 中国石油化工股份有限公司 | Oil refining alkali dreg waste liquid processing method |
| CN104607435A (en) * | 2013-11-05 | 2015-05-13 | 中国石油化工股份有限公司 | Sulfur-containing alkaline residue comprehensive control method |
| CN104607435B (en) * | 2013-11-05 | 2017-01-04 | 中国石油化工股份有限公司 | A kind of comprehensive processing method of sulfur-bearing alkaline residue |
| CN104611003B (en) * | 2013-11-05 | 2017-01-04 | 中国石油化工股份有限公司 | The processing method of refinery alkaline residue |
| CN105712556A (en) * | 2014-12-05 | 2016-06-29 | 中国石油化工股份有限公司 | Processing method of oil refining alkaline residues |
| CN105712457A (en) * | 2014-12-05 | 2016-06-29 | 中国石油化工股份有限公司 | Oil refining alkaline residue acidification reactor with antifoaming function and antifoaming method |
| CN105712456A (en) * | 2014-12-05 | 2016-06-29 | 中国石油化工股份有限公司 | Processing method of alkaline residue waste liquid |
| CN105712456B (en) * | 2014-12-05 | 2018-04-10 | 中国石油化工股份有限公司 | A kind of processing method of alkali residue waste liquid |
| CN105712556B (en) * | 2014-12-05 | 2019-06-11 | 中国石油化工股份有限公司 | A kind of processing method of refinery basic sewage |
| CN104984652A (en) * | 2015-07-11 | 2015-10-21 | 河北新启元能源技术开发股份有限公司 | Treating device for tail gas in acidifying refinement of alkaline residues and treating process thereof |
| CN113121033A (en) * | 2019-12-31 | 2021-07-16 | 中国石油化工股份有限公司 | Oil refining alkaline residue treatment method and device |
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