CN102452674B - Processing method for recycling sodium sulfate from waste alkali liquor in ethylene unit - Google Patents
Processing method for recycling sodium sulfate from waste alkali liquor in ethylene unit Download PDFInfo
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Abstract
The invention discloses a processing method for recycling sodium sulfate from waste alkali liquor in an ethylene unit, wherein the method comprises the following steps: (1), performing wet oxidation on waste alkali liquor with air or oxygen under wet oxidation conditions to obtain oxidation liquid; (2), neutralizing the oxidation liquid to obtain neutralized liquid; (3), crystallizing out sodium sulfate decahydrate from the neutralized liquid by a freezing crystallization method; (4), performing biochemical treatment on frozen mother liquor; (5), performing vaccum evaporation to dry the sodium sulfate decahydrate to obtain anhydrous sodium sulfate products, and returning evaporation mother liquor to the neutralizing unit. The method solves the technical problem that waste alkali liquor of ethylene after being processed by deodorization, dilution and biochemical treatment still contains high-salt which can cause an impact to the biochemical treatment system. The method can be applied in fields like petrochemical, chemical engineering, environment protection, comprehensive utilization of the resources and light industries.
Description
Technical field
The present invention relates to the technology of reclaim(ed) sulfuric acid sodium from waste alkali liquor of ethylene unit, the technology of sodium sulfate, the i.e. oxidation of waste alkali liquor of ethylene unit, neutralization, crystallization reclaim(ed) sulfuric acid sodium are processed and are isolated in the wet oxidation that more particularly relates to waste lye from waste liquid.
Background technology
Sour gas in 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 waste lye and contain Na
2S, Na
2CO
3, NaOH and a small amount of Na
2SO
3, Na
2S
2O
3Also contain the organic sulfides such as mercaptan, thereby have unpleasant stink outward.
After the method for improvement ethylene waste lye comprises direct facture, pre-treatment, the methods such as biochemical treatment, comprehensive use are advanced in dilution.At the Ethylene Development initial stage, the processing of waste lye adopts direct facture, comprises deep-well injection, landfill, dilution discharge and burning, and front several method is due to the requirement of the environmental protection use that has been under an embargo; The burning method energy consumption is large, and running cost is high.
The deodorization technique that wet air oxidation is processed ethylene waste lye is proven technique.Carry out the important means that biochemical treatment has progressively become the ethylene waste lye processing after adopting the wet type air oxidation to carry out recycling other wastewater dilution after deodorization is processed.Ethylene waste lye after processing through wet oxidation contains a large amount of inorganic salt, and biodegradability is poor.Directly enter composite wastewater treatment plant, will impact biochemical treatment system, affect the sewage discharge compliance rate, after dilution, biochemical treatment is still more difficult.For making ethylene waste lye not enter biochemical treatment system, the comprehensive utilization of ethylene waste lye looks like up-and-coming method.
The method of comprehensive utilization ethylene waste lye comprises crystallization recovery sulfide method, precipitated sulfur compound regeneration NaOH method etc.Can obtain Na after secondary crystal
2The industrial goods of S content 28%～31% contain NaOH and Na
2CO
3If mother liquor be cycled to used in the sour gas that absorbs splitting gas, can cause Na
2CO
3Alkali lye in accumulation and affect device and operate.Cupric oxide, magnesium oxide precipitation method are regenerated as sodium hydroxide with sodium sulphite, sodium carbonate, make ethylene waste lye obtain holomorphosis, but this precipitation agent is expensive, and the precipitation poor quality who obtains is not high as the commodity selling price.
CN1789162 has proposed a kind of technique for reclaiming ethylene alkali-washing waste liquid, uses the transition metal oxide desulfurization after 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.
CN1305954 has proposed to prepare the method for S-WAT as raw material take liquid hydrocarbon or waste alkali solution of gasoline, and it is mainly that the sulfurous gas gas mixture that sulfur burning produces is delivered to absorption tower I bottom, and waste lye neutralizes under the tower top spray.The tail gas of absorption tower I is delivered to absorption tower II bottom through the sulfur dioxide gas that contains that burning produces.3～10% sodium hydroxide solutions are under the tower top spray.Separately will deliver to stirred pot from absorption tower I liquid out, and add ferrous sulfate or zinc sulfate to stir.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, adopts the deodorant waste lye after the wet type air oxide treatment that the sulfurous gas in flue gas, flue dust and oxynitride are absorbed.Adopt two sections absorption patterns, leading portion adopts the absorption liquid of back segment discharging directly to contact with flue gas, to reduce flue-gas temperature, removes simultaneously wherein part pollutent; Back segment contacts take deodorant waste lye as absorption liquid with through the flue gas after the leading portion cooling, absorbs the pollutent that comprises oxysulfide or oxynitride, the fume emission after purification.This method has produced the waste liquid that more contains high salt, and the method is worth not as reclaim(ed) sulfuric acid sodium for the comprehensive utilization of the ethylene waste lye after wet oxidation.
Ethylene waste lye carries out carrying out biochemical treatment after deodorization is processed, diluted through wet oxidation again, and contained high salt still can produce biochemical treatment system and impact; And existing comprehensive utilization technique: or the alkali lye utilization is limited, or waste lye direct crystallization mother liquor still gets nowhere, or precipitation agent is expensive, the precipitation poor quality that obtains.
In view of sodium sulfate concentration in the extensive utilization of ethylene waste lye wet air oxidation deodorization, deodorization and in rear waste lye higher, the present invention is the sodium sulfate in the ethylene waste lye after the reclaim(ed) sulfuric acid neutralizing treatment on the basis that the wet oxidation deodorization is processed, reduced the saltiness of waste lye, can reduce or avoid the impact of the water outlet of wet type air oxide treatment and the follow-up biochemical treatment of contained high salt pair thereof, also be conducive to ethylene production enterprise and carry out waste water recycling work.
Term:
Wet type air oxidation (Wet Air Oxidation, WAO): be under high temperature, high top pressure operation condition, use air as oxygenant in liquid phase, be a kind for the treatment of process of organism or the reduction-state inorganics of solubilised state or suspended state in oxidizing water.
The wet type dioxygen oxidation: in the wet type air oxidation operation, it is also feasible replacing air with oxygen, can call the wet type dioxygen oxidation to this method.
Wet oxidation: comprise wet type air oxidation and wet type dioxygen oxidation.
Ethylene waste lye: the sour gas in ethene cracking gas is mainly hydrogen sulfide, carbonic acid gas, organosulfur etc., ethylene waste lye results from the counter current contact of alkaline solution and splitting gas, sour gas and sodium hydroxide reaction generate sodium salt, and the hydrocarbons component in cleaved gas of waste lye while is saturated.Can contain Na in waste lye
2S, Na
2CO
3, NaOH and a small amount of Na
2SO
3, Na
2S
2O
3, also may contain NaHCO
3, and contain the organic sulfides such as mercaptan, have unpleasant stink.
Oxidation solution: ethylene waste lye is carried out the wet oxidation operation, and the liquid that obtains is referred to herein as oxidation solution.
Intermediate oxidation liquid: when ethylene waste lye is carried out 2 grades of wet oxidations operation, go out the oxidized liquid that the 1st grade of wet oxidation advance the 2nd grade of wet oxidation and be called intermediate oxidation liquid.
Regulate the pH value: for the high ethylene waste lye of Sodium sulfhydrate content, complete oxidation can make its pH value be reduced to acidity, be subjected to the restriction of wet oxidation reaction equipment matter, rooting is first regulated the pH value of waste lye or/and minute two-stage oxidizing according to Sodium sulfhydrate content and is controlled the pH value of intermediate oxidation liquid according to Sodium sulfhydrate content possibly.The present invention requires to regulate with sodium hydroxide the pH value of intermediate oxidation liquid between waste lye pH value and two-stage oxidizing reaction member.
Neutralizer: oxidation solution is carried out neutralization operation, and the liquid that obtains is referred to herein as neutralizer.Neutralize with the vitriol oil or sodium hydroxide at this paper.
Single stage method, two step method: enterprise is during according to sodium sulfate-aqueous systems phase diagram theory processing saltcake, can be directly from solution crystallization go out thenardite, be called single stage method; Can adopt also that crystallization goes out saltcake from the aqueous solution, the method that saltcake dewaters again is called two step method.Single stage method generally adopts vacuum vapor deposition method; The method of saltcake dehydration is divided into again seasoning evaporation, widely different desiccating method, scorification, the vacuum-evaporation evaporation etc. of turning.
Sodium sulfate anhydrous.min(99): the trade(brand)name of industrial anhydrous sodium sulfate/be commonly called as.
Summary of the invention
The defects that the present invention exists separately in order to overcome existing ethylene waste lye treatment process provides after a kind of wet oxidation neutralizing treatment ethylene waste lye and the method for reclaim(ed) sulfuric acid sodium therefrom.This invention can reduce the saltiness of waste lye, and the impact that can reduce or avoid wet oxidation to process the follow-up biochemical treatment of high salt pair in water outlet reaches the disadvantageous effect to reusing sewage, simultaneously the sodium sulfate in the ethylene waste lye after the reclaim(ed) sulfuric acid neutralizing treatment.
The invention provides after a kind of wet oxidation neutralizing treatment ethylene waste lye and the method for reclaim(ed) sulfuric acid sodium therefrom.Particularly, the method comprises the steps: that (1) under the wet oxidation condition, carry out wet oxidation with air or oxygen to it, obtains oxidation solution; (2) oxidation solution is neutralized, obtain neutralizer; (3) adopt freeze crystallization crystallization from neutralizer to go out sal glauberi; (4) freezing mother liquor goes biochemical treatment; (5) sal glauberi is carried out the vacuum-evaporation drying, obtain the anhydrous sodium sulphate product, mother liquid evaporation returns neutralisation unit.
In step (1), the ethylene waste lye oxidizing temperature is the scope interior (pressure is on hold-up vapour pressure at each temperature) of 110～250 ℃.
In step (3), crystallization adopts freeze crystallization crystallization from neutralizer to go out sal glauberi.Obtain the anhydrous sodium sulphate product after the sal glauberi drying, i.e. Sodium sulfate anhydrous.min(99).Freezing mother liquor carries out biochemical treatment.
Gained Sodium sulfate anhydrous.min(99) quality can reach or higher than the requirement of II class salable product in industrial anhydrous sodium sulfate quality standard (GB/T 6009-2003), and the rate of recovery of whole process sodium is greater than 85%, and namely the quantity discharged of salt reduces approximately 85%.
The preferred embodiment of the present invention:
The condition of step (1) wet oxidation: the wet oxidation temperature requirement of ethylene waste lye is 115 ℃～250 ℃, reaction pressure is more than 20%, guarantee enough residence time and oxygen partial pressure so that sodium sulphite fully is converted into sodium sulfate greater than at each temperature saturated vapor pressure.Different wet type oxidizing temperatures require the minimum residence time:
For the high ethylene waste lye of Sodium sulfhydrate content, complete oxidation can make its pH value be reduced to acidity, be subjected to the restriction of wet oxidation reaction equipment matter, rooting is first regulated pH value or minute two-stage oxidizing of waste lye according to Sodium sulfhydrate content and is controlled the pH value of intermediate oxidation liquid according to Sodium sulfhydrate content possibly.The present invention requires to regulate with sodium hydroxide the pH value of intermediate oxidation liquid between waste lye pH value and two-stage oxidizing reaction member.
In step (2) and pH control: neutralization reaction is at strong stirring or pass into pressurized air and carry out under stirring, with the CO that guarantees that solution mixes, generates
2Fully discharge.The neutralizer pH that goes out reactor is controlled at 3.5～5.5, and for reaching higher anhydrous sodium sulphate product hierarchy, more excellent scope is 4.5～5.1.Neutralizer is processed through sedimentation and is removed impurity.
For the high ethylene waste lye of Sodium sulfhydrate content, complete oxidation can make its pH value be reduced to acidity.For the acidic oxidation liquid of acidity surplus, the present invention requires with in sodium hydroxide and unnecessary acidity, because the price of sodium carbonate is higher than sodium hydroxide, and uses sodium carbonate can increase sodium carbonate foreign matter content in sodium sulfate.Be subjected to the restriction of wet oxidation reaction equipment matter, may require minute two-stage oxidizing and control the pH value of intermediate oxidation liquid according to Sodium sulfhydrate content.The present invention requires to regulate the pH value with sodium hydroxide between the two-stage oxidizing reaction member.
Step (3) crystallization mode: the wet oxidation temperature is in the time of 110 ℃～250 ℃, adopt the sal glauberi in freezing and crystallizing recovery neutralizer, then sal glauberi is carried out the vacuum-evaporation drying, obtain the anhydrous sodium sulphate product, be Sodium sulfate anhydrous.min(99), mother liquid evaporation returns neutralisation unit.
The essential distinction of the present invention and prior art is,
For the treatment process of ethylene waste lye, reclaim sodium sulfate on existing wet oxidation basis, have new meaning.For reclaim(ed) sulfuric acid sodium, the report of the existing reclaim(ed) sulfuric acid sodium of other several industries, but have no report for reclaim(ed) sulfuric acid sodium from ethylene waste lye.
For reclaim(ed) sulfuric acid sodium, the wet oxidation that the present invention relates to the processing ethylene waste lye, neutralization, crystallization, crystalline mother solution are processed and have all been carried out preferably:
For wet oxidation operation, carried out preferably for the residence time under differing temps and pressure.The operational condition that the wet oxidation of existing different enterprises is processed is as follows:
Ethylene waste lye after deodorization goes biochemical will the neutralization before, but neutralization gets final product to pH 7～9.Due to Na in ethylene waste lye
2CO
3Content higher than Na in mirabilite ore, bittern
2CO
3Content, in it and the pH of the pH of terminal point saltcake solution when also various conventional sodium sulfate is produced.Remove the carbonate in waste lye, will be reduced to pH lower.The present invention will be preferably 3.5～5.5 with terminal point pH in oxidation solution, and more excellent is 4.5-5.1.
For the vacuum-evaporation mother liquor, be again gained crystallization nitre to be got back to the evaporative crystallization operation after freezing and crystallizing in general sodium sulfate production, the present invention gets back to the oxidation solution neutralisation unit with it and carries out neutralization operation.
The present invention does not carry out preferably acid and the concentration of neutralization because at present sewage work substantially all use in the vitriol oil with deodorization after ethylene waste lye.
The invention has the beneficial effects as follows:
Ethylene waste lye after deodorization is further processed, reclaim(ed) sulfuric acid sodium, can reduce the quantity discharged of waste lye, reduce or avoid wet oxidation to process the impact of the follow-up biochemical treatment of high salt pair in water outlet, also be conducive to ethylene production enterprise and carry out other waste water recycling work.The mother liquor amount of ethylene waste lye after reclaim(ed) sulfuric acid sodium is processed reduces, and the saltiness of freezing and crystallizing mother liquor reduces greatly, and the biochemical treatment difficulty is reduced greatly.By implementing optimal conditions of the present invention, can make the sodium sulfate good product quality of recovery, the method such as need not burn and can reach " GB-T 6009-2003 industrial anhydrous sodium sulfate " II class salable product and above index.
Description of drawings
Fig. 1 is that the ethene alkali lye after processing through 110 ℃～250 ℃ wet oxidations reclaims the schematic flow sheet of anhydrous sodium sulphate through two step method.
Embodiment
Use the ethylene waste lye after certain enterprise's oil removing removes the gred to consist of (mass percent): NaOH17.9%, Na in embodiment
2S 3.8%, Na
2CO
31.7%, COD 25000mg/L, TOC1300mg/L; Impurity metallic elements content is extremely low, Fe 0.6mg/L, Cr1.2mg/L, Ni1.8mg/L, Cu 0.8mg/L, Ca, Mg (in Mg) 0.6mg/L, Cl 73.8mg/L.
Below in conjunction with Fig. 1, by 5 specific embodiments, the present invention is further detailed.
Embodiment 1
This ethylene waste lye is not in the situation that dilute and pH regulator, through 120 ℃ of (6MPa) wet type air oxidation 8h, the gained oxidation solution is with the vitriol oil pH5.46 that neutralizes, neutralizer is through freezing and crystallizing, freezing mother liquor removes biochemistry, freezing and crystallizing is dried to Sodium sulfate anhydrous.min(99) after vacuum evaporating crystalization, mother liquid evaporation returns to neutralisation unit.Gained Sodium sulfate anhydrous.min(99) sodium sulphate content is 93.76%, meets " GB-T 6009-2003 industrial anhydrous sodium sulfate " III class salable product standard; During the freezing mother liquor amount of gained is reduced to approximately and liquid measure 1/3, COD 2900mg/L, total dissolved solidss 9%.
Embodiment 2
This ethylene waste lye is not in the situation that dilute and pH regulator, through 150 ℃ of (4.5MPa) wet type dioxygen oxidation 6h, the gained oxidation solution is with the vitriol oil pH5.03 that neutralizes, neutralizer is through freezing and crystallizing, freezing mother liquor removes biochemistry, freezing and crystallizing is dried to Sodium sulfate anhydrous.min(99) after vacuum evaporating crystalization, mother liquid evaporation returns to neutralisation unit.Gained Sodium sulfate anhydrous.min(99) sodium sulphate content is 97.24%, meets " GB-T 6009-2003 industrial anhydrous sodium sulfate " II class salable product standard; During the freezing mother liquor amount of gained is reduced to approximately and liquid measure 1/3, COD 900mg/L, total dissolved solidss 7%.
Embodiment 3
This ethylene waste lye is not in the situation that dilute and pH regulator, through 160 ℃ of (6MPa) wet type air oxidation 5h, the gained oxidation solution is with the vitriol oil pH4.64 that neutralizes, neutralizer is through freezing and crystallizing, freezing mother liquor removes biochemistry, freezing and crystallizing is dried to Sodium sulfate anhydrous.min(99) after vacuum evaporating crystalization, mother liquid evaporation returns to neutralisation unit.Gained Sodium sulfate anhydrous.min(99) sodium sulphate content is 99.05%, meets " GB-T 6009-2003 industrial anhydrous sodium sulfate " II class salable product standard (because color jaundice); During the freezing mother liquor amount of gained is reduced to approximately and liquid measure 1/3, COD 450mg/L, total dissolved solidss 6%.
Embodiment 4
This ethylene waste lye is not in the situation that dilute and pH regulator, through 180 ℃ of (6MPa) wet type air oxidation 5h, the gained oxidation solution is with the vitriol oil pH4.01 that neutralizes, neutralizer is through freezing and crystallizing, freezing mother liquor removes biochemistry, freezing and crystallizing is dried to Sodium sulfate anhydrous.min(99) after vacuum evaporating crystalization, mother liquid evaporation returns to neutralisation unit.Gained Sodium sulfate anhydrous.min(99) sodium sulphate content is 98.08%, meets " GB-T 6009-2003 industrial anhydrous sodium sulfate " II class acceptable end product standard; During the freezing mother liquor amount of gained is reduced to approximately and liquid measure 1/3, COD 300mg/L, total dissolved solidss 6%.
Embodiment 5
This ethylene waste lye is not in the situation that dilute and pH regulator, through 210 ℃ of (6MPa) wet type dioxygen oxidation 2h, the gained oxidation solution is with the vitriol oil pH4.70 that neutralizes, neutralizer is through freezing and crystallizing, freezing mother liquor removes biochemistry, freezing and crystallizing is dried to Sodium sulfate anhydrous.min(99) after vacuum evaporating crystalization, mother liquid evaporation returns to neutralisation unit.Gained Sodium sulfate anhydrous.min(99) sodium sulphate content is 99.13%, meets " GB-T 6009-2003 industrial anhydrous sodium sulfate " I class acceptable end product standard; During the freezing mother liquor amount of gained is reduced to approximately and liquid measure 1/3, COD 220mg/L, total dissolved solidss 6%.
Claims (6)
1. process ethylene waste lye and the method for reclaim(ed) sulfuric acid sodium therefrom for one kind, the method comprises the steps:
(1) under the wet oxidation condition, with air or oxygen, it is carried out wet oxidation, obtain oxidation solution;
Wherein, the condition of wet oxidation: the wet oxidation temperature requirement of ethylene waste lye is 115 ℃～250 ℃, and reaction pressure is greater than at each temperature saturated vapor pressure more than 20%, and different wet type oxidizing temperatures require the minimum residence time as follows
(2) oxidation solution is neutralized, obtain neutralizer; Neutralization reaction is at strong stirring or pass into pressurized air and carry out under stirring, and the neutralizer pH that goes out reactor is controlled at 3.5～5.5;
(3) adopt freeze crystallization crystallization from neutralizer to go out sal glauberi;
(4) freezing mother liquor goes biochemical treatment;
(5) sal glauberi is carried out the vacuum-evaporation drying, obtain the anhydrous sodium sulphate product, mother liquid evaporation returns neutralisation unit.
2. method according to claim 1, the neutralizer pH that goes out reactor in step (2) is controlled at 4.5～5.1.
3. method according to claim 2, adopt the vitriol oil to neutralize in step (2).
4. method according to claim 1, for the high ethylene waste lye of Sodium sulfhydrate content, neutralize with sodium hydroxide in step (2).
5. method according to claim 1, for the high ethylene waste lye of Sodium sulfhydrate content, first regulate ethylene waste lye pH value with sodium hydroxide and carry out again oxidation in step (1), adopt sodium hydroxide or the vitriol oil to neutralize in step (2).
6. method according to claim 1 or 5, for the high ethylene waste lye of Sodium sulfhydrate content, in step (1), oxidation divides two sections, regulate the pH value of intermediate oxidation liquid with sodium hydroxide between the two-stage oxidizing reaction member, adopt sodium hydroxide or the vitriol oil to neutralize in step (2).
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| CN105016551B (en) * | 2014-04-22 | 2017-08-22 | 中国石油化工股份有限公司 | The processing method of the spent lye containing organic nitrogen during refining liquid hydrocarbon |
| CN104140115A (en) * | 2014-08-25 | 2014-11-12 | 湖南江冶机电科技股份有限公司 | Method and device for recovering anhydrous sodium sulfate from filtrate after purification treatment of desulfurated lead plasters |
| CN105565567B (en) * | 2015-12-25 | 2018-08-31 | 石家庄杰克化工有限公司 | Method for processing organic wastewater with high salt in a kind of production of EDTA sodium cyanide methods |
| CN108892279A (en) * | 2018-08-06 | 2018-11-27 | 陈式好 | A kind of liquid waste treating apparatus |
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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 |
| CN1789162A (en) * | 2005-12-06 | 2006-06-21 | 河北工业大学 | Technique for reclaiming ethylene alkali-washing waste liquid |
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| CN1162571A (en) * | 1996-01-31 | 1997-10-22 | 日本石油化学株式会社 | Wet oxidizing process |
| 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 |
| CN1789162A (en) * | 2005-12-06 | 2006-06-21 | 河北工业大学 | Technique for reclaiming ethylene alkali-washing waste liquid |
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