CN102815811A - Short flow method for recycling sodium sulfate from ethylene waste alkali liquid - Google Patents
Short flow method for recycling sodium sulfate from ethylene waste alkali liquid Download PDFInfo
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Abstract
A short flow method for recycling sodium sulfate from ethylene waste alkali liquid includes the following process steps: (1) conducting wet oxidizing through air or oxygen under the wet oxidizing condition to obtain oxidizing liquid; (2) conducting neutralization operation on the oxidizing liquid to obtain neutralization liquid; (3) separating the neutralization liquid to obtain clear liquid or filtering liquid and (4) drying the clear liquid or the filtering liquid to obtain anhydrous sodium sulfate. The short flow method resolves the technical problem that ethylene waste alkali liquid is subjected to the wet oxidizing processing to be diluted and then subjected to biochemical treatment, and high salinity contained in the short flow method still impacts a biochemical treatment system. The short flow method simultaneously shortens the process flow, reduces equipment investment for recycling sodium sulfate, and can be applied to the fields of petrifaction, chemical engineering, environment protection, resource comprehensive utilization, light industry and the like.
Description
Technical field
The present invention is specifically related to a kind of method of comprehensive utilization of ethylene waste lye, particularly from wet oxidation handle, the method for separating anhydrous sodium sulfate the ethylene waste lye after the neutralization, belong to the recycling field of trade waste.
Background technology
Sour gas in the ethene cracking gas mainly comprises hydrogen sulfide, carbonic acid gas, organosulfur etc., for removing sour gas, takes the washing of alkaline solution and splitting gas counter current contact, and the waste liquid of generation is called ethylene waste lye.Remove in the waste lye and contain Na
2S, Na
2CO
3, NaOH and minor N a
2SO
3, Na
2S
2O
3Also contain organic sulfides such as mercaptan, thereby have unpleasant stink outward.
Methods such as biochemical treatment, comprehensive use were carried out in dilution after the method for improvement ethylene waste lye comprised direct facture, pre-treatment.Directly facture comprises deep-well injection, landfill, dilution discharge and burning, the use because environmental protection requirement has been under an embargo.The pre-treatment that ethylene waste lye is carried out comprises oxidation style or neutralisation, but pretreated ethylene waste lye contains a large amount of inorganic salt, directly enters composite wastewater treatment plant, will impact to biochemical treatment system, and causes the waste of inorganic salt.
The method forefathers of comprehensive utilization ethylene waste lye also have research.CN1789162 has proposed a kind of technique for reclaiming ethylene alkali-washing waste liquid, uses the transition metal oxide desulfurization behind the employing alkaline earth metal oxide causticization waste lye, and the sulfide that obtains is expected to become high value-added product, but does not have product to detect; It is the method for feedstock production S-WAT that CN1305954 has proposed with liquid hydrocarbon or waste alkali solution of gasoline, and the S-WAT of this method preparation still exists in solution, and contains more sodium sulfate impurity; CN101143293 has proposed a kind of method of deodorant waste lye absorbing treating smoke, and this method has produced the waste liquid that more contains high salt, and this method is used for the comprehensive utilization of the ethylene waste lye after the wet oxidation, is worth not as reclaim(ed) sulfuric acid sodium.
If the recovery of SODIUM SULPHATE ANHYDROUS 99PCT adopts oxidation-neutralization-crystallization-drying process to carry out in the ethylene waste lye, this process is used for such the recovery on a small scale of ethylene waste lye and has complex process on the SODIUM SULPHATE ANHYDROUS 99PCT, the problem that cost of investment is too high.
Summary of the invention
The technical problem that the present invention will solve:
After the invention provides a kind of wet oxidation; The neutralizing treatment ethylene waste lye; And the short flow path processing method of reclaim(ed) sulfuric acid sodium therefrom; Reduced salt amount, can reduce or avoid the impact of wet oxidation treat effluent and the follow-up biochemical treatment of contained high salt pair thereof, also helped ethylene production enterprise and carry out waste water recycling work to Waste Water Treatment and environmental emission; Shorten the technological process that reclaims SODIUM SULPHATE ANHYDROUS 99PCT, can have been met the SODIUM SULPHATE ANHYDROUS 99PCT of the specification of quality of " GB/T 6009-2003 industrial anhydrous sodium sulfate " without crystallization.
Technical scheme provided by the invention:
The short flow and method of reclaim(ed) sulfuric acid sodium in a kind of ethylene waste lye specifically comprises following process step:
(1) ethylene waste lye is carried out wet oxidation and handle, wherein sulfide mainly is oxidized to vitriol;
(2) in oxidation after ethylene waste lye, obtain neutralizer;
(3) neutralizer is separated obtain clear liquid or filtrating;
(4) clear liquid or filtrating drying are obtained SODIUM SULPHATE ANHYDROUS 99PCT.
Described ethylene waste lye is through the ethylene waste lye of water or water vapour dilution, without in the ethylene waste lye of water or water vapour dilution any one; For the ethylene waste lye without the dilution of water or water vapour, the neutralizer after oxidation, the neutralization can be selected through water or water vapour dilution or in without water or water vapour dilution.
In the step (1), sulfide mainly is oxidized to following method: the S of the main basis of judgement of vitriol
2-, S
2O
3 2-, SO
3 2-, SO
4 2-Can be by chemical analysis and ion-chromatographic determination, its measuring method is all with reference to GB; Can judge whether that through concentration ratio primary product is a vitriol.
Described molar content ratio for Sodium sulfhydrate and yellow soda ash directly carries out wet oxidation less than 1 ethylene waste lye.
Described molar content ratio for Sodium sulfhydrate and yellow soda ash is greater than 1 ethylene waste lye; Complete oxidation can make its pH value be reduced to acidity; Receive the restriction of wet oxidation reaction equipment matter, rooting is regulated earlier the pH value of waste lye according to Sodium sulfhydrate content or is divided two-stage oxidizing and control the pH value of intermediate oxidation liquid according to Sodium sulfhydrate content possibly.
Described pH value of regulating waste lye according to Sodium sulfhydrate content earlier; Using massfraction in the step (1) earlier is that 30～45% sodium hydroxide solution is regulated molar content ratio that ethylene waste lye makes Sodium sulfhydrate and yellow soda ash in 0.95 to 1 scope, carries out wet oxidation again.
Described minute two-stage oxidizing and according to the pH value of Sodium sulfhydrate content control intermediate oxidation liquid; Oxidation divides two sections in the step (1); Between the two-stage oxidizing reaction member, using massfraction is the pH value that 30～45% sodium hydroxide solution is regulated intermediate oxidation liquid; First section pH that is oxidizing to ethylene waste lye stopped wet oxidation at 4.3～7.5 o'clock, and the pH value of using sodium hydroxide to regulate intermediate oxidation liquid is 8.8～10.5; And then carry out second section wet oxidation.
Described wet oxidation is treated to any one in wet type air oxide treatment or the processing of wet type dioxygen oxidation.
Described wet oxidation treatment temperature is 160 ℃～250 ℃; Pressure is to be higher than the saturated vapor pressure 20% of waste lye at each temperature; The residence time of wet oxidation reaction is different and change according to treatment temp, when being specially 160 ℃ of treatment temps, and the residence time >=5h; When treatment temp was 180 ℃, the residence time was >=3h; When treatment temp is 210 ℃, the residence time >=2h; When treatment temp is 250 ℃, the residence time >=1h.The residence time can infinitely prolong, but the sulphate content of oxidation liquid only can increase slightly, considers only to limit the minimum time that stops from economy
In the step (2), described to adopt sulphuric acid soln or the massfraction of mass percent concentration 70～98% for the ethylene waste lye after the oxidation be that 30～45% sodium hydroxide solution carries out neutralization reaction.
The churned mechanically neutralization reactor of the optional airtight normal pressure of described neutralization reactor (if any the mechanical stirring neutralization reactor of venting port) or blast in the neutralization reactor of pneumatic blending any one; For the churned mechanically neutralization reactor of airtight normal pressure (if any the mechanical stirring neutralization reactor of venting port), the neutralizer pH value that goes out reactor drum is controlled at 4.36～5.36; For the neutralization reactor that blasts pneumatic blending, the neutralizer pH value that goes out reactor drum is controlled at 5.36～6.36.
In the step (3), can select in sedimentation, filtration or the air supporting any one described neutralizer is separated; Sedimentation can be selected any one in gravity settling or the centrifugal settling; All can select not add flocculation agent or add flocculation agent to the separation of neutralizer;
Said neutralizer is during without the dilution of water or water vapour, adopts when not adding the gravity settling of flocculation agent, and the required settling time is 16h to 48h.
Said neutralizer is when the dilution of water or water vapour, adopts the centrifugal settling that does not add flocculation agent, and the required settling time can be lower than neutralizer and adopt the gravity settling time that does not add flocculation agent for without water or water vapour dilution the time.
Said neutralizer is after water or water vapour dilution; Employing adds the gravity settling or the centrifugal settling of flocculation agent; The required settling time can be lower than neutralizer adopts the gravity settling time that does not add flocculation agent for without the dilution of water or water vapour the time, releases degree, flocculation agent kind dimly and confirms through experiment.
Said neutralizer comprises the neutralizer that ethylene waste lye obtains earlier through the dilution of water or water vapour after water or water vapour dilution and then oxidation, neutralization, perhaps without the neutralizer that obtains after the ethylene waste lye oxidation of water or water vapour dilution, the neutralization any one in water or water vapour dilution again.
In the optional SEPIGEL 305 of said flocculation agent, the cationic-type polyacrylamide any one or multiple.
Said neutralizer does not add flocculation agent; Handle the product that can obtain meeting quality product requirement (specific targets " GB/T 6009-2003 industrial anhydrous sodium sulfate ") through air supporting, suitably use flocculation agent can make the quality product grade improve (such as bringing up to the II class) from the III class.
In the step (4), described drying means can select that atmospheric evaporation is dry, vacuum-evaporation is dry, in the spraying drying any one; Also can select to let the submerged combustion of flame contact saltcake liquid evaporate, obtain the SODIUM SULPHATE ANHYDROUS 99PCT product.
The invention has the beneficial effects as follows:
Ethylene waste lye to after the deodorization is further handled; Reclaim(ed) sulfuric acid sodium; Can reduce salt amount to Sewage treatment systems and environmental emission; Reduce or avoid the impact of the follow-up biochemical treatment of high salt pair in the wet oxidation treat effluent, also help ethylene production enterprise and carry out other waste water recycling work.Through the optimal conditions of embodiment of the present invention, reduce approximately more than 90% to the salt amount of wastewater biochemical treatment facility and environmental emission, wastewater discharge reduces about more than 90%; Methods such as the SODIUM SULPHATE ANHYDROUS 99PCT that reclaims need not burn can reach the specification of quality of " GB/T 6009-2003 industrial anhydrous sodium sulfate ".
Description of drawings
Fig. 1 is through the schematic flow sheet of the ethene alkali lye after 160 ℃～250 ℃ wet oxidations processing through neutralization, dried recovered SODIUM SULPHATE ANHYDROUS 99PCT.
Embodiment
Use the ethylene waste lye after certain enterprise's oil removing removes the gred to consist of (mass percent): NaOH 17.9%, Na among the embodiment 1-4
2S 3.8%, Na
2CO
31.7%, COD 25000mg/L, TOC 1300mg/L; Impurity metallic elements content is extremely low, Fe 0.6mg/L, Cr 1.2mg/L, Ni 1.8mg/L, Cu 0.8mg/L, Ca, Mg (in Mg) 0.6mg/L, Cl 73.8mg/L.
Below in conjunction with accompanying drawing, specify through embodiment.
Embodiment 1
This ethylene waste lye is under the situation of not diluting with pH regulator, through 160 ℃ of (6MPa) wet type air oxidation 5h; Gained oxidation liquid uses mass concentration in the neutralization reactor of drum pneumatic blending be that 98% the vitriol oil pH value that neutralizes is 5.64; The gained neutralizer add SEPIGEL 305 (PAM) flocculation agent to 1ppm after filter to remove impurity; The dry products therefrom sodium sulphate content of filtrating is 98.65%, meets " GB-T 6009-2003 industrial anhydrous sodium sulfate " II class standard.
Embodiment 2
This ethylene waste lye is under the situation of not diluting with pH regulator, through 180 ℃ of (6MPa) wet type air oxidation 3h; Gained oxidation liquid uses mass concentration in the neutralization reactor of drum pneumatic blending be that 98% the vitriol oil pH value that neutralizes is 6.23; The gained neutralizer is removed impurity through gravity settling 36h; The stillness of night, dry products therefrom sodium sulphate content was 98.08%, met " GB-T 6009-2003 industrial anhydrous sodium sulfate " II class standard.
Embodiment 3
This ethylene waste lye is under the situation of not diluting with pH regulator, through 210 ℃ of (6MPa) wet type dioxygen oxidation 2h; Gained oxidation liquid in mechanical stirring, have that to use mass concentration in the neutralization reactor of venting port be that 98% the vitriol oil pH value that neutralizes is 4.70; The gained neutralizer add cationic polyacrylamide (CPAM) to the 0.3ppm gas through the floating impurity of removing; The dry products therefrom sodium sulphate content of clear liquid is 99.13%, meets " GB-T 6009-2003 industrial anhydrous sodium sulfate " I class standard.
Embodiment 4
This ethylene waste lye is under the situation of not diluting with pH regulator, through 240 ℃ of (6MPa) wet type dioxygen oxidation 1h; Gained oxidation liquid in mechanical stirring, have that to use mass concentration in the neutralization reactor of venting port be that 70% the vitriol oil pH value that neutralizes is 5.26; The gained neutralizer adds cationic polyacrylamide (CPAM) and removes impurity through gravity settling 3h to 0.1ppm; The stillness of night, dry products therefrom sodium sulphate content was 98.51%, met " GB-T 6009-2003 industrial anhydrous sodium sulfate " II class standard.
Use the ethylene waste lye after certain enterprise's oil removing removes the gred to consist of (mass percent): NaOH 0% among the embodiment 5-8, NaHS 8.8%, Na
2CO
38.3%, COD 75000mg/L, TOC 2300mg/L; Impurity metallic elements content is extremely low, Fe 0.8mg/L, Cr 1.3mg/L, Ni 1.8mg/L, Cu 0.8mg/L, Ca, Mg (in Mg) 0.7mg/L, Cl 75.8mg/L.
Below in conjunction with accompanying drawing, specify through embodiment.
Embodiment 5
This ethylene waste lye is under the situation of not diluting with pH regulator; Through 160 ℃ of (6MPa) wet type air oxidation 2.5h; Gained intermediate oxidation liquid pH is 7.3, and using mass concentration is that the pH value that 30% sodium hydroxide is regulated intermediate oxidation liquid is 9.5, and continuation oxidation 2.5h gets oxidation liquid; Gained oxidation liquid uses mass concentration in the neutralization reactor of drum pneumatic blending be that 98% the vitriol oil pH value that neutralizes is 5.65; The gained neutralizer add SEPIGEL 305 (PAM) flocculation agent to 1ppm after filter to remove impurity; The dry products therefrom sodium sulphate content of filtrating is 98.63%, meets " GB-T 6009-2003 industrial anhydrous sodium sulfate " II class standard.
Embodiment 6
This ethylene waste lye is under the situation of not diluting with pH regulator; Through 180 ℃ of (6MPa) wet type air oxidation 1.5h; Gained intermediate oxidation liquid pH is 6.3, and using mass concentration is that the pH value that 30% sodium hydroxide is regulated intermediate oxidation liquid is 10.5, and continuation oxidation 1.5h gets oxidation liquid; Oxidation liquid uses mass concentration in the neutralization reactor of drum pneumatic blending be that 98% the vitriol oil pH value that neutralizes is 6.25; The gained neutralizer is removed impurity through gravity settling 36h; The stillness of night, dry products therefrom sodium sulphate content was 98.05%, met " GB-T 6009-2003 industrial anhydrous sodium sulfate " II class standard.
Embodiment 7
This ethylene waste lye is 0.95: 1 with the molar content ratio that sodium hydroxide solution (massfraction is 30%) is adjusted to Sodium sulfhydrate and yellow soda ash; Employed mass concentration is that 30% sodium hydroxide solution quality is 11.0% of this ethylene waste lye quality, then through 210 ℃ of (6MPa) wet type dioxygen oxidation 2h; Gained oxidation liquid in mechanical stirring, have that to use mass concentration in the neutralization reactor of venting port be that 30% the sodium hydroxide pH value that neutralizes is 4.72; The gained neutralizer add cationic polyacrylamide (CPAM) to the 0.3ppm gas through the floating impurity of removing; The dry products therefrom sodium sulphate content of clear liquid is 99.15%, meets " GB-T 6009-2003 industrial anhydrous sodium sulfate " I class standard.
Embodiment 8
This ethylene waste lye is 0.97: 1 with the molar content ratio that sodium hydroxide solution (massfraction is 30%) is adjusted to Sodium sulfhydrate and yellow soda ash; Employed mass concentration is that 30% sodium hydroxide solution quality is 10.8% of this ethylene waste lye quality, then through 240 ℃ of (6MPa) wet type dioxygen oxidation 1h; Gained oxidation liquid in mechanical stirring, have that to use mass concentration in the neutralization reactor of venting port be that 98% the vitriol oil pH value that neutralizes is 5.26; The gained neutralizer adds cationic polyacrylamide (CPAM) and removes impurity through gravity settling 3h to 0.1ppm; The stillness of night, dry products therefrom sodium sulphate content was 98.50%, met " GB-T 6009-2003 industrial anhydrous sodium sulfate " II class standard.
Claims (12)
1. the short flow and method of reclaim(ed) sulfuric acid sodium in the ethylene waste lye is characterized in that comprising following process step:
(1) ethylene waste lye is carried out wet oxidation and handle, wherein sulfide mainly is oxidized to vitriol;
(2) in oxidation after ethylene waste lye, obtain neutralizer;
(3) neutralizer is separated obtain clear liquid or filtrating;
(4) stillness of night or filtrating drying are obtained SODIUM SULPHATE ANHYDROUS 99PCT.
2. method according to claim 1 is characterized in that step (1) ethylene waste lye is for through the ethylene waste lye of water or water vapour dilution, without in the ethylene waste lye of water or water vapour dilution any one.
3. method according to claim 2 is characterized in that for the ethylene waste lye without the dilution of water or water vapour, and the neutralizer after oxidation, the neutralization can be selected through water or water vapour dilution or without water or water vapour dilution.
4. method according to claim 1 is characterized in that for the molar content ratio of Sodium sulfhydrate and yellow soda ash directly carrying out wet oxidation less than 1 ethylene waste lye.
5. method according to claim 1; It is characterized in that for the molar content ratio of Sodium sulfhydrate and yellow soda ash greater than 1 ethylene waste lye; Using massfraction in the step (1) earlier is that 30～45% sodium hydroxide solution is regulated molar content ratio that ethylene waste lye makes Sodium sulfhydrate and yellow soda ash in 0.95 to 1 scope, carries out wet oxidation again.
6. method according to claim 1; It is characterized in that for the molar content ratio of Sodium sulfhydrate and yellow soda ash greater than 1 ethylene waste lye; Oxidation divides two sections in the step (1); Between the two-stage oxidizing reaction member, using massfraction is the pH value that 30～45% sodium hydroxide solution is regulated intermediate oxidation liquid, and first section pH that is oxidizing to ethylene waste lye stopped wet oxidation at 4.3～7.5 o'clock, and using the pH value of sodium hydroxide adjusting intermediate oxidation liquid is 8.8～10.5; And then carry out second section wet oxidation.
7. according to claim 1,4,5,6 described arbitrary methods, it is characterized in that wet oxidation is treated to any one in wet type air oxide treatment or the processing of wet type dioxygen oxidation.
8. according to claim 1,4,5,6 described arbitrary methods, it is characterized in that the wet oxidation treatment temperature is 160 ℃～250 ℃; Pressure is to be higher than the saturated vapor pressure 20% of waste lye at each temperature; The residence time of wet oxidation reaction is different and change according to treatment temp, when being specially 160 ℃ of treatment temps, and the residence time >=5h; When treatment temp was 180 ℃, the residence time was >=3h; When treatment temp is 210 ℃, the residence time >=2h; When treatment temp is 250 ℃, the residence time >=1h; The residence time can infinitely prolong, but the sulphate content of oxidation liquid only can increase slightly, considers only to limit the minimum time that stops from economy.
9. according to claim 1,4,5,6 described arbitrary methods, it is characterized in that adopting sulphuric acid soln or the massfraction of mass percent concentration 70～98% for the ethylene waste lye after the oxidation is that 30～45% sodium hydroxide solution carries out neutralization reaction.
10. method according to claim 1, it is characterized in that neutralization reactor is optional has the mechanical stirring neutralization reactor of venting port or blasts in the neutralization reactor of pneumatic blending any one; For the mechanical stirring neutralization reactor that venting port is arranged, the neutralizer pH value that goes out reactor drum is controlled at 4.36～5.36; For the neutralization reactor that blasts pneumatic blending, the neutralizer pH value that goes out reactor drum is controlled at 5.36～6.36.
11. method according to claim 1 is characterized in that step (3) is separated neutralizer can to select in sedimentation, filtration or the air supporting any one; Sedimentation can be selected any one in gravity settling or the centrifugal settling; All can select not add flocculation agent or add flocculation agent to the separation of neutralizer;
12. method according to claim 1 is characterized in that drying means in the step (4) can select that atmospheric evaporation is dry, vacuum-evaporation is dry, in the spraying drying any one; Also can select to let the submerged combustion of flame contact saltcake liquid evaporate, obtain the SODIUM SULPHATE ANHYDROUS 99PCT product.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103359880A (en) * | 2013-07-19 | 2013-10-23 | 中国石油大学(华东) | Biochemical treatment process for ethylene waste lye |
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| CN1257102A (en) * | 1998-12-16 | 2000-06-21 | 中国石油化工集团公司 | Process for treating waste lye of refining oil products in petroleum refining industry |
| WO2009035642A1 (en) * | 2007-09-11 | 2009-03-19 | Siemens Water Technologies Corp. | Treatment of spent caustic waste |
| US7850822B2 (en) * | 2003-10-29 | 2010-12-14 | Siemens Water Technologies Holding Corp. | System and method of wet oxidation of a viscose process stream |
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2011
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| CN1257102A (en) * | 1998-12-16 | 2000-06-21 | 中国石油化工集团公司 | Process for treating waste lye of refining oil products in petroleum refining industry |
| US7850822B2 (en) * | 2003-10-29 | 2010-12-14 | Siemens Water Technologies Holding Corp. | System and method of wet oxidation of a viscose process stream |
| WO2009035642A1 (en) * | 2007-09-11 | 2009-03-19 | Siemens Water Technologies Corp. | Treatment of spent caustic waste |
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| CN103359880A (en) * | 2013-07-19 | 2013-10-23 | 中国石油大学(华东) | Biochemical treatment process for ethylene waste lye |
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